#------------------------------------------------------------------------------ #$Date: 2024-12-25 04:29:43 +0200 (Wed, 25 Dec 2024) $ #$Revision: 296965 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/35/1573535.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1573535 loop_ _publ_author_name 'Ndiaye-Gueye, Mboss\'e' 'Traor\'e, Bocar' 'Thiam, Ibrahima Elhadji' 'Diouf, Ousmane' 'Wenger, Emmanuel' 'Sall, Abdou Salam' 'Lecomte, Claude' 'Gaye, Mohamed' _journal_coeditor_code PK2715 _journal_paper_doi 10.1107/S2056989024012349 _journal_year 2024 _chemical_formula_iupac '[La2 (C2 H3 O2)4 (C11 H10 N4) (H2 O1)4] (N1 O3)2, 0.5H2 O' _chemical_formula_moiety 'C30 H40 La2 N8 O12 2+, 2(N1 O3 -), 0.5(H2 O)' _chemical_formula_sum 'C30 H41 La2 N10 O18.5' _chemical_formula_weight 1115.55 _chemical_name_systematic ;Di-\m-acetato-\k^4^O:O'-bis{(acetato-\k^2^O,O')tetraaqua[1-(pyridin-2-ylmethylidene-\kN)-2-(pyridin-2-yl-\kN)hydrazine-\kN^1^]lanthanum(III)} dinitrate hemihydrate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 114.213(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.1170(11) _cell_length_b 17.8366(19) _cell_length_c 11.8094(12) _cell_measurement_reflns_used 21184 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.4120 _cell_measurement_theta_min 2.6650 _cell_volume 2135.7(4) _computing_cell_refinement ; APEX5 (Bruker, 2023) ; _computing_data_collection ; APEX5 (Bruker, 2023) ; _computing_data_reduction ; APEX5 (Bruker, 2023) ; _computing_molecular_graphics ; Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker X8' _diffrn_measurement_method ; Single crystals were positioned at 35, 40, 35, and 28 mm from the detector ; _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_unetI/netI 0.0671 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 72063 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.434 _diffrn_reflns_theta_min 2.209 _exptl_absorpt_coefficient_mu 2.057 _exptl_absorpt_correction_T_max 0.4235 _exptl_absorpt_correction_T_min 0.2151 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour 'metallic yellowish yellow' _exptl_crystal_density_diffrn 1.735 _exptl_crystal_description block _exptl_crystal_F_000 1106 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.262 _refine_diff_density_min -0.945 _refine_ls_extinction_coef 0.00071(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 10392 _refine_ls_number_restraints 781 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0387 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+1.5461P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.0638 _reflns_number_gt 7368 _reflns_number_total 10392 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file pk2715.cif _cod_data_source_block I _cod_original_formula_sum 'C30 H41 La2 N10 O18.50' _cod_database_code 1573535 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.684 _shelx_estimated_absorpt_t_max 0.821 _shelx_hkl_file ; 1 0 0 0.03 0.45 2 0 0 485.73 31.27 2 0 0 545.64 30.08 2 0 0 584.32 30.67 -2 0 0 539.11 29.08 -2 0 0 516.48 30.05 -2 0 0 498.21 30.44 -2 0 0 506.56 31.38 -2 0 0 517.80 28.82 2 0 0 560.46 29.15 3 0 0 3693.66 200.18 -3 0 0 4000.41 203.79 -3 0 0 3563.92 199.56 -3 0 0 3723.50 200.09 3 0 0 3838.54 201.59 3 0 0 3849.52 202.01 3 0 0 3668.57 203.58 -3 0 0 3391.47 201.85 -4 0 0 11.53 3.61 -4 0 0 5.37 4.98 -4 0 0 6.88 6.20 -4 0 0 8.54 1.32 4 0 0 12.72 2.48 4 0 0 1.97 3.30 4 0 0 18.97 5.59 4 0 0 8.60 5.69 -4 0 0 8.91 2.26 5 0 0 505.32 28.97 5 0 0 525.48 32.05 -5 0 0 495.71 35.11 5 0 0 465.73 31.05 -5 0 0 507.30 28.77 5 0 0 473.12 34.88 -5 0 0 532.73 31.32 6 0 0 1315.71 76.22 -6 0 0 1283.23 81.11 6 0 0 1280.80 73.62 6 0 0 1246.67 80.37 -6 0 0 1455.27 76.48 -6 0 0 1381.67 73.39 7 0 0 2492.46 140.30 -7 0 0 2803.14 143.33 7 0 0 2383.43 148.08 7 0 0 2491.91 143.18 -7 0 0 2656.50 148.69 -8 0 0 1082.82 72.35 8 0 0 1043.73 63.54 8 0 0 1077.23 64.25 -8 0 0 1157.04 65.65 8 0 0 1016.30 70.07 8 0 0 1051.39 60.88 9 0 0 273.69 31.31 9 0 0 259.71 24.61 -9 0 0 281.37 27.02 9 0 0 244.83 19.25 9 0 0 257.78 23.73 10 0 0 582.88 46.68 10 0 0 493.88 37.99 10 0 0 453.51 32.55 10 0 0 556.44 38.01 11 0 0 11.91 16.27 11 0 0 17.05 9.76 11 0 0 88.91 23.01 11 0 0 27.57 13.13 12 0 0 49.57 12.17 12 0 0 42.72 23.96 12 0 0 50.33 19.57 12 0 0 76.74 17.14 12 0 0 39.91 20.02 13 0 0 225.29 32.33 13 0 0 179.31 43.63 13 0 0 242.53 30.75 14 0 0 331.70 40.48 14 0 0 297.32 45.16 14 0 0 297.60 38.88 15 0 0 333.76 59.22 15 0 0 278.01 40.67 15 0 0 259.40 40.38 16 0 0 169.75 76.18 16 0 0 216.74 36.09 16 0 0 124.78 52.17 -2 -1 0 93.23 8.27 2 -1 0 80.93 6.24 2 -1 0 78.83 5.65 -2 -1 0 83.72 6.05 -2 -1 0 72.80 7.47 2 -1 0 72.70 6.47 2 -1 0 86.25 8.05 2 1 0 89.13 5.91 -2 1 0 89.61 8.33 2 1 0 74.40 7.39 -2 1 0 91.65 6.44 2 1 0 78.48 5.14 2 1 0 91.89 7.79 -2 1 0 80.16 5.49 -3 -1 0 178.77 14.05 3 -1 0 175.75 14.40 -3 -1 0 178.54 11.61 -3 -1 0 153.54 13.10 3 -1 0 186.29 11.95 3 -1 0 165.25 12.04 3 -1 0 162.67 10.80 3 1 0 163.61 11.92 3 1 0 175.18 14.08 -3 1 0 194.84 14.90 3 1 0 167.84 13.53 3 1 0 152.72 10.09 -3 1 0 192.77 12.20 -3 1 0 164.45 10.54 4 -1 0 389.17 24.26 4 -1 0 384.93 22.95 -4 -1 0 354.82 25.48 4 -1 0 395.00 24.58 -4 -1 0 419.44 24.19 4 -1 0 390.56 27.21 -4 -1 0 366.20 26.90 -4 -1 0 401.43 22.66 4 1 0 392.19 27.34 4 1 0 379.30 22.27 -4 1 0 410.93 28.07 -4 1 0 395.43 22.65 4 1 0 371.55 24.26 -4 1 0 423.93 24.85 4 1 0 385.80 25.69 5 -1 0 95.01 8.22 5 -1 0 110.95 15.83 -5 -1 0 112.68 14.74 -5 -1 0 80.56 11.57 -5 -1 0 70.15 10.17 -5 -1 0 99.42 7.18 5 -1 0 105.10 10.99 5 -1 0 98.68 10.48 -5 1 0 125.60 16.53 5 1 0 113.38 15.58 -5 1 0 83.54 10.92 -5 1 0 100.10 7.82 5 1 0 96.36 10.74 5 1 0 94.36 11.30 5 1 0 96.47 7.20 6 -1 0 842.33 48.94 6 -1 0 797.15 49.30 -6 -1 0 880.61 49.37 -6 -1 0 799.18 53.61 6 -1 0 810.76 54.10 6 -1 0 802.06 47.23 -6 -1 0 818.25 45.43 6 1 0 727.93 53.25 -6 1 0 863.61 46.75 6 1 0 834.32 50.43 6 1 0 828.63 49.60 -6 1 0 899.77 49.67 6 1 0 809.82 46.41 -6 1 0 839.02 54.83 7 -1 0 48.01 6.82 7 -1 0 49.40 8.93 7 -1 0 35.26 14.71 7 -1 0 41.92 9.32 -7 -1 0 52.81 10.70 -7 -1 0 47.56 15.01 7 1 0 51.41 14.64 -7 1 0 42.29 18.41 7 1 0 42.58 9.87 -7 1 0 47.90 6.56 -7 1 0 42.80 9.78 7 1 0 39.33 9.19 7 1 0 54.74 6.48 8 -1 0 7.39 9.14 -8 -1 0 7.18 11.47 8 -1 0 -0.06 5.88 -8 -1 0 16.09 17.02 8 -1 0 10.09 7.38 8 -1 0 2.96 16.28 8 1 0 -9.51 12.45 -8 1 0 -4.36 16.61 8 1 0 7.65 7.06 8 1 0 1.96 4.54 -8 1 0 -4.69 4.99 8 1 0 7.70 8.70 -8 1 0 9.37 10.07 9 -1 0 22.28 10.28 9 -1 0 26.91 7.21 9 -1 0 32.60 16.46 -9 -1 0 28.23 15.58 9 -1 0 5.11 10.62 9 1 0 13.50 9.35 9 1 0 23.12 10.84 9 1 0 19.63 6.65 9 1 0 43.22 20.52 -9 1 0 26.96 16.47 10 -1 0 153.18 17.77 10 -1 0 145.17 18.03 10 -1 0 140.75 17.34 10 -1 0 130.62 26.39 10 1 0 138.17 20.17 10 1 0 143.77 18.34 10 1 0 136.56 14.61 10 1 0 111.67 27.43 11 -1 0 7.92 10.63 11 -1 0 -17.14 19.82 11 -1 0 12.75 13.96 11 -1 0 0.92 11.59 11 -1 0 -5.46 14.73 11 1 0 -21.16 13.48 11 1 0 35.13 18.73 11 1 0 5.38 8.15 11 1 0 2.00 20.70 12 -1 0 12.32 14.23 12 -1 0 30.97 22.85 12 -1 0 33.10 22.27 12 1 0 -24.87 29.36 12 1 0 20.03 15.21 12 1 0 -5.62 20.19 12 1 0 2.62 9.70 13 -1 0 47.60 18.34 13 -1 0 -17.15 28.02 13 -1 0 69.89 24.70 13 1 0 38.03 29.36 13 1 0 14.51 17.42 13 1 0 26.98 21.20 14 -1 0 -9.42 41.39 14 -1 0 -65.81 24.52 14 -1 0 17.00 25.45 14 1 0 -16.17 25.30 14 1 0 -40.58 42.44 14 1 0 -13.18 24.64 15 -1 0 3.62 47.70 15 -1 0 -30.77 23.64 15 -1 0 -30.62 30.89 15 1 0 -24.82 24.43 15 1 0 -47.22 36.45 15 1 0 34.79 53.06 16 -1 0 -14.43 62.01 16 -1 0 -7.39 40.06 16 -1 0 15.00 36.50 16 1 0 -1.60 48.19 16 1 0 -20.93 65.58 16 1 0 11.20 30.79 0 -2 0 0.38 0.98 -1 -2 0 4944.69 261.79 1 -2 0 4742.03 262.23 -1 -2 0 5208.58 262.40 -1 -2 0 4730.93 260.98 1 -2 0 4720.31 262.04 1 -2 0 4241.56 261.55 1 -2 0 4965.28 261.23 1 2 0 5101.54 261.93 -1 2 0 4521.60 261.58 -1 2 0 4902.65 261.22 1 2 0 5503.64 262.36 -1 2 0 4696.87 262.33 -2 -2 0 1933.71 107.82 2 -2 0 1848.03 109.68 2 -2 0 1941.87 108.34 -2 -2 0 1918.71 109.22 -2 -2 0 2073.66 109.91 2 -2 0 1942.27 108.15 -2 2 0 2023.14 108.28 -2 2 0 2046.96 110.21 2 2 0 1930.24 109.42 2 2 0 2229.69 109.89 -2 2 0 2023.78 108.21 2 2 0 1972.62 107.79 3 -2 0 61.54 8.39 -3 -2 0 43.93 7.23 3 -2 0 56.57 6.08 3 -2 0 53.77 5.78 -3 -2 0 54.53 7.59 3 -2 0 51.61 5.35 -3 -2 0 42.94 5.63 -3 2 0 59.31 6.26 3 2 0 61.10 5.72 3 2 0 59.28 8.05 -3 2 0 53.98 5.40 3 2 0 56.05 7.55 -3 2 0 71.39 9.61 4 -2 0 6.03 3.55 -4 -2 0 0.73 2.82 4 -2 0 4.42 5.69 -4 -2 0 -4.38 5.28 4 -2 0 8.94 3.55 -4 -2 0 4.12 4.50 4 2 0 2.30 1.69 -4 2 0 11.08 3.05 -4 2 0 13.15 7.33 -4 2 0 4.40 4.06 4 2 0 9.59 5.67 4 2 0 -3.02 4.68 -5 -2 0 1718.97 109.33 -5 -2 0 2041.94 107.33 5 -2 0 2069.36 107.30 5 -2 0 1997.67 111.81 5 -2 0 1854.38 106.50 5 -2 0 1879.02 107.61 -5 -2 0 1956.82 110.78 -5 -2 0 1925.37 106.19 -5 2 0 2037.51 106.02 5 2 0 1930.49 111.56 5 2 0 1871.16 105.28 5 2 0 2111.59 109.42 -5 2 0 1993.00 108.03 -5 2 0 1719.77 111.14 5 2 0 1907.43 108.18 -6 -2 0 2920.19 159.18 -6 -2 0 2581.65 163.52 6 -2 0 2814.38 166.00 -6 -2 0 3202.77 161.57 6 -2 0 3103.73 161.04 6 -2 0 2851.77 161.67 -6 -2 0 2847.13 165.26 6 -2 0 2875.17 160.28 6 2 0 3029.84 163.00 6 2 0 2864.42 158.90 -6 2 0 3130.58 159.57 6 2 0 2883.14 162.11 -6 2 0 3002.77 167.11 -6 2 0 3005.29 162.40 6 2 0 2794.85 166.06 7 -2 0 725.82 44.51 -7 -2 0 740.40 52.51 -7 -2 0 752.58 42.53 -7 -2 0 835.02 47.20 7 -2 0 812.33 47.41 7 -2 0 716.90 51.83 7 -2 0 816.16 45.67 7 2 0 665.07 51.55 -7 2 0 779.84 43.61 7 2 0 770.69 47.66 7 2 0 724.87 46.82 -7 2 0 646.18 53.51 7 2 0 753.37 42.98 -7 2 0 808.82 48.35 -8 -2 0 705.75 52.71 -8 -2 0 702.55 44.54 8 -2 0 660.23 50.33 8 -2 0 685.80 41.88 -8 -2 0 694.86 38.55 8 -2 0 683.88 45.05 8 2 0 694.84 40.28 8 2 0 653.46 46.02 -8 2 0 686.33 54.77 -8 2 0 734.36 47.17 -8 2 0 741.79 40.78 8 2 0 696.93 51.05 8 2 0 676.37 44.67 9 -2 0 598.10 39.40 9 -2 0 602.08 48.33 9 -2 0 622.98 41.66 -9 -2 0 727.67 45.44 9 2 0 623.90 36.95 -9 2 0 652.97 44.70 9 2 0 525.78 48.40 9 2 0 631.59 42.23 -9 2 0 635.47 37.16 9 2 0 586.66 42.40 10 -2 0 367.83 30.00 -10 -2 0 471.07 39.81 10 -2 0 445.14 32.77 10 -2 0 379.56 30.07 10 -2 0 412.80 39.95 10 2 0 439.17 45.95 10 2 0 385.38 34.15 10 2 0 414.12 26.63 10 2 0 423.76 32.45 11 -2 0 17.16 12.84 11 -2 0 35.91 24.17 11 -2 0 4.69 11.58 11 -2 0 5.14 11.56 11 -2 0 -0.72 19.79 11 2 0 4.19 8.15 11 2 0 23.53 21.33 11 2 0 19.25 11.85 12 -2 0 90.07 27.12 12 -2 0 104.54 18.14 12 -2 0 96.56 22.70 12 2 0 88.97 18.29 12 2 0 74.82 12.25 12 2 0 127.54 30.10 13 -2 0 103.72 31.17 13 -2 0 106.76 21.84 13 -2 0 103.45 37.64 13 2 0 164.19 23.58 13 2 0 171.96 40.28 13 2 0 136.98 26.43 14 -2 0 200.14 39.06 14 -2 0 185.24 27.41 14 -2 0 183.17 34.63 14 2 0 185.84 35.28 14 2 0 206.36 30.02 14 2 0 167.61 48.41 15 -2 0 169.08 55.04 15 -2 0 238.00 33.04 15 -2 0 278.05 43.47 15 2 0 190.29 58.06 15 2 0 233.20 34.51 15 2 0 327.76 46.26 16 -2 0 33.78 41.22 16 -2 0 85.18 32.57 16 -2 0 87.89 62.63 16 2 0 123.59 70.60 16 2 0 6.01 50.32 16 2 0 149.58 32.63 0 -3 0 -0.91 1.40 0 -3 0 2.76 1.81 0 3 0 2.08 2.07 0 3 0 2.53 1.44 0 3 0 -0.83 1.38 -1 -3 0 42.21 5.50 1 -3 0 41.50 5.17 -1 -3 0 35.82 4.31 1 -3 0 35.60 4.56 1 -3 0 34.59 2.69 1 3 0 27.91 4.27 -1 3 0 43.04 5.20 1 3 0 33.79 3.06 -1 3 0 31.91 4.36 1 3 0 32.25 3.25 1 3 0 43.31 4.44 -1 3 0 36.01 3.58 -1 3 0 30.87 2.54 -1 3 0 39.46 5.74 -2 -3 0 2699.45 140.79 -2 -3 0 2750.59 143.23 2 -3 0 2355.88 142.39 2 -3 0 2280.89 141.53 -2 -3 0 2657.45 142.25 2 -3 0 2598.88 141.11 2 -3 0 2631.06 143.03 -2 3 0 2650.72 141.20 2 3 0 2903.81 143.05 2 3 0 2558.00 140.66 -2 3 0 2566.25 141.56 -2 3 0 2537.55 143.21 2 3 0 2633.90 142.53 3 -3 0 282.09 18.12 3 -3 0 288.23 19.61 3 -3 0 323.21 19.27 -3 -3 0 295.52 21.62 3 -3 0 307.39 21.87 -3 -3 0 307.19 18.80 -3 -3 0 333.83 21.23 3 3 0 310.68 21.47 -3 3 0 347.13 19.64 3 3 0 319.07 21.47 -3 3 0 306.96 19.10 3 3 0 311.56 18.63 -3 3 0 350.29 23.51 -4 -3 0 2938.46 162.28 4 -3 0 2807.71 159.08 -4 -3 0 2958.48 159.52 4 -3 0 2921.56 163.21 4 -3 0 2735.58 159.92 4 -3 0 2909.57 157.81 -4 -3 0 2715.22 162.45 4 -3 0 2900.45 160.05 4 3 0 3174.82 163.39 4 3 0 2915.35 159.35 -4 3 0 3003.98 160.31 -4 3 0 3067.53 164.05 4 3 0 2999.30 162.02 -4 3 0 2984.20 159.41 -5 -3 0 1955.69 101.83 -5 -3 0 1717.94 101.59 5 -3 0 1830.53 106.19 5 -3 0 1830.59 102.25 -5 -3 0 1685.47 104.91 5 -3 0 1808.76 101.82 5 -3 0 1884.57 101.19 -5 -3 0 1888.41 105.38 5 3 0 1801.80 105.96 -5 3 0 1935.72 101.06 5 3 0 1936.37 104.34 -5 3 0 1676.56 106.29 5 3 0 1754.12 99.93 -5 3 0 1957.78 102.84 -6 -3 0 382.28 31.74 6 -3 0 452.74 27.78 -6 -3 0 443.51 27.32 6 -3 0 425.23 33.76 -6 -3 0 481.19 29.04 6 -3 0 418.30 27.95 6 -3 0 443.81 29.01 -6 -3 0 432.87 33.87 6 3 0 419.22 25.65 -6 3 0 454.32 30.08 6 3 0 458.41 34.46 -6 3 0 427.73 36.14 6 3 0 432.28 29.65 -6 3 0 467.17 27.06 6 3 0 473.46 31.31 -7 -3 0 27.87 10.34 -7 -3 0 44.20 6.39 7 -3 0 42.29 7.90 7 -3 0 34.50 7.79 7 -3 0 52.73 13.98 -7 -3 0 46.68 9.07 7 -3 0 37.73 7.05 -7 -3 0 41.43 14.82 7 3 0 33.95 8.61 7 3 0 26.23 12.74 7 3 0 36.30 5.13 7 3 0 29.38 11.84 -7 3 0 29.38 16.06 -7 3 0 28.52 10.36 -7 3 0 36.45 6.63 8 -3 0 -4.25 8.15 8 -3 0 6.49 7.51 8 -3 0 -8.18 15.31 -8 -3 0 -1.59 15.61 8 -3 0 4.99 7.54 -8 -3 0 -0.67 4.11 -8 -3 0 5.75 10.61 8 3 0 5.96 10.46 8 3 0 -7.31 16.15 -8 3 0 16.46 10.64 -8 3 0 4.78 5.27 8 3 0 5.48 8.32 8 3 0 -2.71 4.07 -8 3 0 -23.28 17.75 9 -3 0 197.53 29.14 9 -3 0 237.04 22.47 -9 -3 0 237.27 15.19 -9 -3 0 264.27 25.42 9 -3 0 278.19 21.36 9 -3 0 213.84 22.13 9 3 0 251.83 17.29 9 3 0 257.95 29.20 9 3 0 181.42 27.63 9 3 0 228.84 23.16 -9 3 0 265.16 18.57 10 -3 0 269.65 22.28 -10 -3 0 312.92 34.76 10 -3 0 261.01 37.21 10 -3 0 249.44 23.59 10 -3 0 277.77 25.07 10 -3 0 225.20 31.58 -10 3 0 290.24 20.40 10 3 0 273.19 26.57 10 3 0 257.07 19.17 10 3 0 239.62 33.02 10 3 0 261.38 29.41 11 -3 0 365.63 38.49 11 -3 0 413.19 46.07 11 -3 0 416.60 34.55 11 -3 0 339.99 27.87 11 3 0 349.76 49.15 11 3 0 356.27 32.09 11 3 0 354.58 24.89 12 -3 0 331.28 44.52 12 -3 0 358.07 34.07 12 -3 0 318.38 41.55 12 3 0 333.95 47.29 12 3 0 422.91 34.77 13 -3 0 37.27 30.29 13 -3 0 108.70 37.04 13 -3 0 90.15 19.51 13 3 0 62.90 20.37 13 3 0 57.07 38.26 13 3 0 47.17 26.88 14 -3 0 62.26 29.87 14 -3 0 41.71 21.03 14 -3 0 62.11 40.89 14 3 0 40.12 31.06 14 3 0 12.46 21.59 14 3 0 -57.69 42.85 15 -3 0 18.20 25.82 15 -3 0 -9.25 33.05 15 -3 0 31.09 47.59 15 3 0 -25.91 30.04 15 3 0 1.52 25.57 15 3 0 65.25 55.51 16 -3 0 -68.51 74.24 16 -3 0 12.61 49.78 16 -3 0 15.09 30.83 16 3 0 34.46 54.32 16 3 0 -2.76 48.70 16 3 0 44.27 32.24 0 -4 0 2748.45 150.37 0 -4 0 2753.83 150.58 0 4 0 2681.22 150.14 0 4 0 2833.80 150.59 0 4 0 2843.23 150.43 -1 -4 0 42.07 5.93 -1 -4 0 42.57 5.13 1 -4 0 51.60 6.55 -1 -4 0 43.69 4.19 1 -4 0 48.18 4.00 1 -4 0 47.40 6.01 -1 4 0 27.50 5.01 -1 4 0 45.16 6.35 -1 4 0 38.76 3.53 1 4 0 50.91 4.59 -1 4 0 38.92 6.39 1 4 0 46.24 5.41 1 4 0 56.20 6.33 -2 -4 0 1966.62 105.54 2 -4 0 1824.36 104.51 2 -4 0 1909.13 107.98 -2 -4 0 1991.22 108.27 -2 -4 0 2024.80 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716.17 53.14 11 5 0 700.51 42.43 12 -5 0 595.11 46.84 12 -5 0 629.22 58.05 12 -5 0 563.33 53.00 12 5 0 531.05 60.07 12 5 0 520.53 45.09 13 -5 0 193.73 35.00 13 -5 0 239.12 27.69 13 -5 0 189.40 38.98 13 5 0 236.92 48.59 13 5 0 217.63 28.70 14 -5 0 45.94 37.18 14 -5 0 26.01 37.71 14 -5 0 28.09 25.61 14 5 0 -9.48 30.19 14 5 0 39.69 50.68 14 5 0 25.48 29.04 15 -5 0 -66.56 43.70 15 -5 0 39.43 26.24 15 -5 0 10.09 35.45 15 5 0 -28.67 36.41 15 5 0 -45.73 47.82 15 5 0 30.42 26.75 16 -5 0 6.45 53.70 16 -5 0 24.23 29.64 16 5 0 -10.92 72.92 16 5 0 60.24 32.61 0 -6 0 0.16 3.77 0 -6 0 8.56 3.55 0 6 0 1.37 3.23 0 6 0 3.81 3.54 0 6 0 -0.04 2.97 -1 -6 0 167.88 13.63 -1 -6 0 154.40 10.90 1 -6 0 162.48 12.90 1 -6 0 167.00 11.26 -1 -6 0 149.53 11.68 -1 6 0 123.62 12.78 -1 6 0 170.63 14.83 -1 6 0 167.22 10.29 1 6 0 162.10 12.88 1 6 0 155.16 11.97 1 6 0 154.87 11.21 -1 6 0 158.24 13.26 2 -6 0 1057.23 57.18 2 -6 0 1109.74 61.18 -2 -6 0 1089.02 59.64 2 -6 0 996.09 60.09 -2 -6 0 1061.11 61.18 2 6 0 977.85 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334.88 28.10 9 -7 0 308.66 34.19 9 -7 0 342.25 27.45 9 -7 0 323.13 34.39 -9 7 0 350.08 27.59 9 7 0 339.19 22.70 9 7 0 325.37 29.86 9 7 0 345.32 39.59 10 -7 0 614.60 51.08 -10 -7 0 676.62 52.19 10 -7 0 680.02 54.70 10 -7 0 684.33 45.09 -10 -7 0 623.42 41.48 10 7 0 640.28 56.65 -10 7 0 648.41 42.94 10 7 0 646.93 38.91 10 7 0 586.59 46.22 11 -7 0 630.67 57.88 11 -7 0 629.80 54.99 -11 -7 0 632.31 41.87 11 -7 0 694.58 47.41 11 7 0 687.07 49.75 -11 7 0 643.87 44.53 11 7 0 673.42 40.14 11 7 0 639.69 61.65 -12 -7 0 449.73 29.94 12 -7 0 463.64 48.78 12 -7 0 450.51 52.62 12 -7 0 417.43 37.83 12 7 0 451.58 42.25 12 7 0 499.70 64.24 13 -7 0 167.40 33.14 13 -7 0 158.27 24.18 13 -7 0 185.89 36.22 13 7 0 123.25 25.92 13 7 0 108.12 38.51 14 -7 0 -16.43 22.51 14 -7 0 78.03 34.23 14 -7 0 14.28 34.95 14 7 0 43.22 55.15 14 7 0 63.94 26.45 14 7 0 34.72 30.74 15 -7 0 -9.44 38.40 15 -7 0 1.30 50.92 15 7 0 56.36 29.24 15 7 0 -17.66 65.34 16 -7 0 55.62 57.56 16 -7 0 35.18 33.50 16 7 0 136.69 46.80 16 7 0 53.78 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9 0 713.95 46.03 -4 9 0 651.02 51.28 4 9 0 726.17 42.74 4 9 0 789.69 47.92 5 -9 0 1062.80 65.94 -5 -9 0 1030.64 64.41 5 -9 0 1127.85 66.04 5 -9 0 1040.83 62.35 -5 -9 0 968.58 66.93 -5 9 0 1039.02 70.08 5 9 0 1029.81 59.73 5 9 0 1095.22 60.03 -5 9 0 1070.48 63.20 -5 9 0 1036.93 62.15 5 9 0 1056.29 65.34 5 9 0 1053.39 66.00 -6 -9 0 293.88 23.52 6 -9 0 319.82 23.41 6 -9 0 358.39 31.21 6 -9 0 328.78 28.95 -6 -9 0 295.82 29.14 6 -9 0 316.10 24.38 -6 -9 0 234.97 28.92 -6 9 0 327.15 27.10 -6 9 0 277.38 26.14 -6 9 0 353.72 38.55 6 9 0 333.90 22.17 6 9 0 330.64 21.79 6 9 0 347.45 30.01 6 9 0 331.29 30.03 -7 -9 0 104.32 13.59 7 -9 0 68.05 9.66 -7 -9 0 97.91 16.22 7 -9 0 69.09 16.18 -7 -9 0 74.74 16.97 7 -9 0 68.21 15.66 7 -9 0 74.83 12.51 -7 9 0 95.08 25.74 -7 9 0 100.44 15.74 7 9 0 107.32 12.46 7 9 0 53.50 16.38 -7 9 0 83.65 15.60 7 9 0 40.38 17.68 8 -9 0 212.88 14.97 8 -9 0 206.66 30.44 -8 -9 0 218.71 28.77 8 -9 0 237.16 22.88 -8 -9 0 234.34 25.14 8 -9 0 209.52 28.66 -8 -9 0 189.33 22.63 8 9 0 195.09 27.70 8 9 0 235.79 17.08 -8 9 0 218.81 21.98 9 -9 0 484.67 44.24 9 -9 0 432.63 41.74 9 -9 0 436.38 33.69 -9 -9 0 389.55 40.89 -9 -9 0 444.83 35.65 -9 -9 0 491.68 38.79 9 9 0 412.29 44.56 -9 9 0 511.96 36.63 9 9 0 456.87 29.17 -10 -9 0 332.38 37.07 10 -9 0 302.26 37.71 -10 -9 0 324.69 29.62 10 -9 0 342.23 32.69 10 -9 0 334.86 40.84 -10 9 0 333.16 33.05 10 9 0 315.35 45.25 10 9 0 392.19 34.57 10 9 0 337.53 24.02 11 -9 0 380.49 43.84 -11 -9 0 397.20 31.73 11 -9 0 368.23 33.76 11 -9 0 343.30 46.46 11 9 0 370.36 27.17 11 9 0 338.57 48.68 11 9 0 395.90 37.76 -12 -9 0 181.93 20.35 12 -9 0 149.94 31.56 12 -9 0 183.30 25.33 12 -9 0 170.04 31.88 12 9 0 156.23 26.50 12 9 0 150.47 39.27 13 -9 0 20.58 19.76 13 -9 0 17.14 36.32 13 -9 0 51.75 31.59 13 9 0 9.34 49.53 13 9 0 91.91 25.81 14 -9 0 8.71 22.96 14 -9 0 -62.87 38.97 14 -9 0 -11.23 43.83 14 9 0 20.63 26.72 14 9 0 -8.32 51.63 15 -9 0 -27.53 26.47 15 -9 0 30.57 52.96 15 9 0 -121.99 57.31 15 9 0 -28.21 30.33 16 -9 0 33.53 40.73 16 -9 0 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0 13.20 10.69 4 10 0 7.64 10.09 -4 10 0 6.33 9.07 4 10 0 17.35 9.24 -4 10 0 18.33 9.40 4 10 0 12.70 4.85 -4 10 0 27.46 14.99 4 10 0 19.40 6.06 5 -10 0 111.51 14.70 5 -10 0 130.61 18.06 -5 -10 0 101.78 16.13 -5 -10 0 92.87 16.90 5 -10 0 107.20 16.04 -5 10 0 122.98 13.93 5 10 0 108.39 16.04 5 10 0 106.31 11.93 5 10 0 108.47 11.59 5 10 0 130.45 17.47 -5 10 0 118.85 15.49 -5 10 0 113.36 22.91 6 -10 0 396.83 34.01 -6 -10 0 375.35 34.18 -6 -10 0 370.48 35.78 6 -10 0 422.76 33.78 -6 10 0 369.78 44.02 6 10 0 423.72 27.48 6 10 0 449.35 35.18 -6 10 0 414.06 33.55 -6 10 0 444.48 31.38 6 10 0 428.27 27.27 6 10 0 419.51 34.55 7 -10 0 1121.73 69.34 7 -10 0 1000.55 60.33 -7 -10 0 952.08 69.53 7 -10 0 1053.89 62.67 -7 -10 0 928.49 65.10 7 -10 0 947.13 68.28 7 10 0 1067.87 70.23 -7 10 0 1091.96 64.29 -7 10 0 1017.15 65.22 7 10 0 1136.47 61.07 7 10 0 1097.50 60.90 8 -10 0 885.29 59.23 8 -10 0 899.04 54.48 -8 -10 0 733.83 61.95 -8 -10 0 827.17 53.26 -8 -10 0 861.81 57.23 8 -10 0 873.38 49.16 8 -10 0 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55.48 9.90 -10 -11 0 83.07 18.78 -10 -11 0 54.05 22.88 10 -11 0 50.74 23.42 10 -11 0 41.65 22.11 10 -11 0 66.95 18.10 10 11 0 41.55 18.49 10 11 0 91.98 27.81 10 11 0 79.72 11.94 11 -11 0 90.83 27.89 11 -11 0 131.75 33.98 11 -11 0 124.74 19.46 -11 -11 0 78.43 19.14 11 11 0 123.57 17.32 11 11 0 105.63 22.62 11 11 0 89.87 32.59 12 -11 0 36.38 27.79 -12 -11 0 71.79 19.10 12 -11 0 19.30 18.06 12 -11 0 8.25 33.85 12 11 0 20.67 22.58 12 11 0 14.03 38.10 12 11 0 -7.71 12.15 13 -11 0 -18.46 32.74 13 -11 0 20.04 30.98 13 -11 0 55.43 23.05 13 11 0 -20.34 53.49 13 11 0 -8.14 24.56 14 -11 0 70.96 25.99 14 -11 0 -23.82 36.29 14 11 0 34.38 37.00 14 11 0 3.34 67.10 15 -11 0 10.27 29.58 15 -11 0 -36.68 41.38 15 11 0 34.35 66.89 15 11 0 138.55 37.62 0 -12 0 2174.09 122.25 0 -12 0 2229.32 124.64 0 12 0 2188.74 123.19 0 12 0 2006.04 123.57 0 12 0 2276.66 129.30 0 12 0 2210.63 121.62 1 -12 0 2191.69 122.80 1 -12 0 2228.95 123.81 -1 -12 0 2106.47 121.05 -1 -12 0 2173.87 125.28 -1 12 0 1981.99 124.23 1 12 0 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55.35 -6 10 3 860.72 51.35 -6 10 3 808.03 66.26 6 10 -3 882.74 52.49 6 10 -3 896.01 57.24 6 10 -3 771.92 58.20 5 -10 -3 969.56 53.19 -5 -10 3 971.25 59.35 -5 -10 3 960.63 56.85 5 -10 -3 806.32 58.10 5 -10 -3 895.68 62.58 5 -10 -3 865.55 58.78 -5 10 3 956.29 53.92 -5 10 3 832.73 66.85 -5 10 3 938.23 57.55 5 10 -3 1019.95 56.34 5 10 -3 926.87 59.19 5 10 -3 911.87 60.99 4 -10 -3 433.85 34.61 4 -10 -3 543.16 29.67 -4 -10 3 441.09 31.22 4 -10 -3 451.26 37.30 4 -10 -3 421.87 33.40 -4 -10 3 523.84 36.00 -4 10 3 469.83 29.24 4 10 -3 475.22 32.02 -4 10 3 511.77 33.70 -4 10 3 468.45 46.61 4 10 -3 486.23 36.81 4 10 -3 448.97 33.32 4 10 -3 446.40 26.34 3 -10 -3 269.65 26.77 3 -10 -3 300.10 29.40 3 -10 -3 290.33 24.63 -3 -10 3 372.71 28.58 -3 -10 3 319.04 23.24 3 -10 -3 358.02 22.21 3 10 -3 319.17 24.61 -3 10 3 322.00 35.01 3 10 -3 321.89 24.57 3 10 -3 364.30 30.46 -3 10 3 366.69 26.24 2 -10 -3 34.85 7.84 2 -10 -3 32.11 11.19 -2 -10 3 46.48 10.98 2 -10 -3 41.84 7.16 -2 -10 3 46.41 7.84 -2 10 3 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35.73 12 -15 -5 24.46 22.81 -12 -15 5 7.83 23.04 12 15 -5 -36.66 37.89 12 15 -5 38.32 15.46 11 -15 -5 -19.35 29.32 11 -15 -5 -5.18 26.10 11 -15 -5 0.83 10.38 -11 -15 5 -26.59 19.92 11 15 -5 12.06 35.03 11 15 -5 -0.96 12.32 10 -15 -5 65.70 12.18 10 -15 -5 16.61 24.72 -10 -15 5 58.31 22.33 10 -15 -5 11.24 33.19 10 15 -5 55.15 30.85 9 -15 -5 145.73 27.54 9 -15 -5 151.64 30.85 9 -15 -5 132.37 37.20 9 -15 -5 184.26 18.54 -9 -15 5 135.41 22.32 -9 15 5 142.78 25.23 9 15 -5 171.54 32.20 8 -15 -5 480.53 50.45 8 -15 -5 408.82 46.70 8 -15 -5 341.06 42.25 8 -15 -5 474.15 31.89 -8 -15 5 458.37 39.68 8 15 -5 481.13 46.70 -8 15 5 445.26 39.32 7 -15 -5 745.49 61.40 7 -15 -5 699.03 54.29 7 -15 -5 706.89 45.17 -7 -15 5 726.52 54.42 -7 -15 5 650.86 51.21 -7 15 5 693.82 47.94 7 15 -5 709.69 58.52 6 -15 -5 347.99 25.34 6 -15 -5 362.40 41.87 -6 -15 5 260.43 33.84 6 -15 -5 275.46 35.56 -6 -15 5 355.64 34.34 -6 15 5 299.15 26.89 6 15 -5 344.41 35.11 5 -15 -5 249.73 32.61 5 -15 -5 191.57 24.79 -5 -15 5 245.80 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47.36 5 2 -19 47.01 32.67 -5 2 19 -9.69 41.43 -4 -2 19 33.88 41.06 4 -2 -19 21.32 35.23 -4 2 19 -12.89 45.31 4 2 -19 -34.93 40.79 11 -3 -19 -6.14 38.11 11 -3 -19 60.66 47.59 11 3 -19 -75.88 49.54 10 -3 -19 3.00 42.49 10 -3 -19 2.03 37.13 -10 3 19 -51.24 46.13 10 3 -19 24.79 39.55 9 -3 -19 -26.83 40.03 9 -3 -19 34.88 34.84 -9 3 19 30.01 44.26 9 3 -19 -44.95 31.20 9 3 -19 1.22 37.37 8 -3 -19 -26.74 40.48 8 -3 -19 -5.00 40.04 8 3 -19 72.77 34.70 -8 3 19 94.36 43.37 8 3 -19 8.45 37.74 -7 -3 19 50.38 69.53 7 -3 -19 117.96 42.43 7 -3 -19 98.37 37.58 7 3 -19 72.25 34.78 7 3 -19 113.11 47.68 -7 3 19 53.45 44.19 -6 -3 19 218.86 43.85 6 -3 -19 176.03 38.76 6 -3 -19 238.38 55.79 -6 3 19 138.52 44.73 6 3 -19 146.10 48.99 6 3 -19 207.63 40.07 5 -3 -19 219.44 40.27 -5 -3 19 187.98 44.72 5 3 -19 187.96 37.81 5 3 -19 106.77 50.64 -5 3 19 237.41 49.21 4 -3 -19 48.67 43.95 -4 3 19 39.91 38.52 4 3 -19 73.49 41.56 11 -4 -19 125.95 49.09 11 -4 -19 37.23 113.72 11 -4 -19 152.55 41.85 11 4 -19 154.93 55.06 -11 4 19 120.16 53.95 10 -4 -19 240.19 45.92 10 -4 -19 110.66 47.05 10 4 -19 229.15 46.80 -10 4 19 285.26 54.90 9 -4 -19 158.99 41.16 9 -4 -19 223.90 55.11 -9 4 19 166.69 49.56 9 4 -19 154.89 45.90 9 4 -19 207.66 43.04 8 -4 -19 90.72 53.99 8 -4 -19 169.92 39.45 8 4 -19 104.59 36.16 8 4 -19 116.42 41.02 -8 4 19 142.34 48.35 7 -4 -19 84.08 52.42 7 -4 -19 121.66 43.99 7 4 -19 91.77 36.29 -7 4 19 122.57 37.94 7 4 -19 105.00 47.88 6 -4 -19 98.68 54.22 6 -4 -19 4.86 34.86 -6 4 19 30.29 43.76 6 4 -19 25.42 32.24 6 4 -19 90.93 46.93 5 -4 -19 66.75 43.78 -5 4 19 -28.37 44.95 5 4 -19 -40.59 46.03 5 4 -19 29.57 33.47 4 -4 -19 158.55 41.04 4 4 -19 145.25 38.95 -4 4 19 56.40 49.97 10 -5 -19 -12.82 54.22 10 -5 -19 71.86 40.25 10 5 -19 86.16 42.23 -10 5 19 13.49 48.44 9 -5 -19 16.89 42.33 9 -5 -19 -19.48 38.51 9 5 -19 46.19 38.19 -9 5 19 89.97 50.11 8 -5 -19 -50.33 43.82 8 -5 -19 41.87 44.41 8 5 -19 -4.00 37.05 8 5 -19 -10.40 33.00 -8 5 19 -8.65 38.28 7 -5 -19 28.51 35.95 7 -5 -19 47.34 53.15 -7 5 19 90.95 46.50 7 5 -19 0.63 33.11 7 5 -19 -60.89 44.09 6 -5 -19 57.18 37.47 6 -5 -19 12.40 55.21 6 5 -19 28.53 46.08 -6 5 19 41.22 46.29 6 5 -19 13.95 32.57 5 -5 -19 50.43 36.93 5 5 -19 -34.15 31.69 5 5 -19 71.17 48.93 -5 5 19 -88.88 46.58 4 -5 -19 -15.74 37.90 4 5 -19 20.38 35.94 -4 5 19 42.08 41.68 10 -6 -19 273.10 55.54 10 -6 -19 272.07 131.06 10 6 -19 335.58 57.76 -10 6 19 213.60 55.45 9 -6 -19 244.22 59.88 9 -6 -19 57.86 40.26 9 6 -19 125.41 41.65 -9 6 19 139.40 51.23 8 -6 -19 160.94 42.59 8 -6 -19 131.97 58.39 8 6 -19 139.40 42.13 8 6 -19 188.19 38.05 -8 6 19 169.29 53.77 7 -6 -19 64.12 46.38 7 -6 -19 50.23 40.19 -7 6 19 64.81 51.03 7 6 -19 119.80 48.53 7 6 -19 178.41 37.19 6 -6 -19 1.89 48.08 6 -6 -19 47.92 37.59 6 6 -19 -44.63 40.44 -6 6 19 -45.52 47.42 6 6 -19 9.00 38.40 5 -6 -19 69.19 39.02 -5 6 19 13.27 51.05 5 6 -19 52.30 50.34 5 6 -19 -3.36 34.21 9 -7 -19 -22.97 41.60 9 -7 -19 -20.43 46.91 9 7 -19 61.44 50.25 -9 7 19 -20.22 53.35 8 -7 -19 16.32 39.42 8 -7 -19 28.70 46.26 8 7 -19 16.13 34.72 8 7 -19 21.79 49.87 -8 7 19 20.34 42.68 7 -7 -19 55.45 38.44 7 -7 -19 76.20 59.22 7 7 -19 -21.63 33.32 -7 7 19 -83.79 50.24 7 7 -19 -17.09 48.40 6 -7 -19 -23.04 61.66 6 -7 -19 -18.57 36.96 6 7 -19 -98.33 40.36 -6 7 19 59.00 42.96 6 7 -19 53.23 40.83 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_max 0.4235 _exptl_absorpt_correction_T_min 0.2151 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71072 11.133 17.846 11.809 90.032 114.266 89.977 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95808 _shelx_res_file ; TITL it4 in P 21/c pk2715.res created by SHELXL-2019/1 at 11:11:59 on 16-Dec-2024 REM The ZERR numbers (after Z) are all zero - this must be fixed. REM H atoms on O9 are added mainly to get the atom count right. The REM occuopancy refined to about 0.28, but was fixed at 0.25 for the REM sake of convenience. REM Instructions for potential hydrogen bonds REM OMIT -1 2 5 <--- There is no reason to OMIT this reflection. REM acetate REM ligand - disordered REM nitrate - slight disorder REM water (partial) CELL 0.71073 11.117 17.8366 11.8094 90 114.213 90 ZERR 2 0.0011 0.0019 0.0012 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H La N O UNIT 60 82 4 20 37 EQIV $1 1-X,2-Y,-Z EQIV $2 +X,1.5-Y,-0.5+Z EQIV $3 1-X,2-Y,1-Z EQIV $4 2-X,2-Y,1-Z EQIV $5 1-X,0.5+Y,0.5-Z EQIV $6 -1+X,+Y,-1+Z DFIX 31 0.01 O1 H1a O1 H1b O2 H2a O2 H2b O9 H9a O9 H9b DFIX 31.581 H1a H1b H2a H2b H9a H9b SIMU 0.02 0.04 2 N1 > N4' RIGU N1 > N4 RIGU N1' > N4' CHIV 0 N5 N5' EADP N5 N5' EADP O6 O6' EADP O7 O7' EADP O8 O8' L.S. 10 PLAN 1 SIZE 0.1 0.2 0.2 CONF HTAB O1 O6 HTAB O1 O7 HTAB O1 O6' HTAB O1 O8_$2 HTAB O1 O8'_$2 HTAB O2 O4_$1 HTAB O2 O7_$2 HTAB O2 N5'_$2 HTAB O2 O7'_$2 HTAB C13 O7_$5 HTAB C13 O7'_$5 HTAB C13 O7_$3 HTAB C15 O9 HTAB C2 O6_$4 HTAB N2 O5_$3 HTAB C11 O9 HTAB N2' O5_$3 HTAB C6' O5_$3 HTAB C10' O6'_$4 HTAB O9 O6_$6 HTAB O9 O8_$6 FREE La1 C12 FREE La1 C14_$1 LIST 4 BOND $H MORE -1 HTAB fmap 2 acta OMIT 0 2 0 OMIT 1 0 0 REM REM REM WGHT 0.011200 1.546100 EXTI 0.000708 FVAR 0.37244 0.54732 0.76139 0.82558 LA1 3 0.567370 0.959054 0.204674 11.00000 0.01924 0.01380 = 0.01228 0.00176 0.00618 0.00382 O1 5 0.713526 0.847459 0.316379 11.00000 0.02848 0.01839 = 0.01511 0.00302 0.00892 0.00715 H1A 2 0.736902 0.833499 0.383124 11.00000 -1.50000 H1B 2 0.753493 0.824910 0.289299 11.00000 -1.50000 O2 5 0.521812 0.849918 0.054634 11.00000 0.03750 0.01912 = 0.01361 0.00308 0.00641 0.00353 H2A 2 0.489548 0.857952 -0.014681 11.00000 -1.50000 H2B 2 0.574145 0.820539 0.062020 11.00000 -1.50000 O3 5 0.771809 0.960478 0.162510 11.00000 0.03040 0.04087 = 0.01963 0.00832 0.01272 0.00639 O4 5 0.575996 1.101808 0.182613 11.00000 0.03180 0.01864 = 0.01245 0.00111 0.00644 0.00455 O5 5 0.460891 1.064850 0.285441 11.00000 0.06255 0.03109 = 0.02734 0.01452 0.03174 0.02648 C12 1 0.502933 1.116552 0.238516 11.00000 0.04268 0.02442 = 0.01131 0.00248 0.01050 0.01509 C13 1 0.466444 1.196614 0.247458 11.00000 0.08253 0.02461 = 0.03452 0.00206 0.03106 0.02065 AFIX 137 H13A 2 0.431738 1.218889 0.166320 11.00000 -1.50000 H13B 2 0.543322 1.223772 0.300997 11.00000 -1.50000 H13C 2 0.400921 1.198418 0.280778 11.00000 -1.50000 AFIX 0 O10 5 0.374514 0.995212 0.012943 11.00000 0.02010 0.02577 = 0.02380 0.00103 0.00430 0.00594 C14 1 0.263270 1.023835 -0.050236 11.00000 0.01898 0.02575 = 0.01927 0.00305 0.00983 0.00096 C15 1 0.171237 1.040944 0.009281 11.00000 0.03150 0.07770 = 0.03467 0.01649 0.02200 0.01808 AFIX 137 H15A 2 0.104232 1.002998 -0.012831 11.00000 -1.50000 H15B 2 0.130825 1.088904 -0.018859 11.00000 -1.50000 H15C 2 0.219407 1.041944 0.097847 11.00000 -1.50000 AFIX 0 SAME 0.02 0.04 N1' > N4' PART 1 N1 4 0.738861 1.012696 0.416531 21.00000 0.01457 0.01873 = 0.01528 -0.00069 0.00854 -0.00163 C1 1 0.835129 1.059387 0.419435 21.00000 0.02460 0.02701 = 0.01808 0.00132 0.01228 -0.00435 AFIX 43 H1 2 0.837759 1.072530 0.344276 21.00000 -1.20000 AFIX 0 C2 1 0.930547 1.089133 0.527111 21.00000 0.02216 0.02307 = 0.02612 -0.00203 0.01101 -0.00315 AFIX 43 H2 2 0.993945 1.122342 0.524696 21.00000 -1.20000 AFIX 0 C3 1 0.927649 1.067219 0.639419 21.00000 0.01844 0.02626 = 0.01961 -0.00418 0.00378 -0.00201 AFIX 43 H3 2 0.990764 1.085119 0.714130 21.00000 -1.20000 AFIX 0 C4 1 0.831688 1.019385 0.638963 21.00000 0.01864 0.02532 = 0.01443 -0.00224 0.00289 -0.00037 AFIX 43 H4 2 0.828457 1.004507 0.713141 21.00000 -1.20000 AFIX 0 C5 1 0.738792 0.993189 0.526063 21.00000 0.01134 0.01481 = 0.00984 -0.00051 0.00353 0.00229 N2 4 0.640144 0.946034 0.524592 21.00000 0.01700 0.01915 = 0.01199 0.00220 0.00737 -0.00264 AFIX 43 H2C 2 0.637201 0.932701 0.593393 21.00000 -1.20000 AFIX 0 N3 4 0.548235 0.920616 0.416339 21.00000 0.01571 0.01391 = 0.01456 -0.00139 0.00410 0.00187 C6 1 0.457087 0.877528 0.420666 21.00000 0.01955 0.01828 = 0.01729 0.00258 0.01014 -0.00203 AFIX 43 H6 2 0.455719 0.865341 0.496698 21.00000 -1.20000 AFIX 0 C7 1 0.357200 0.848284 0.307077 21.00000 0.01684 0.01854 = 0.02225 -0.00422 0.00808 -0.00214 C8 1 0.263922 0.797400 0.312825 21.00000 0.02664 0.02632 = 0.03292 -0.00297 0.01427 -0.01138 AFIX 43 H8 2 0.266593 0.781473 0.388808 21.00000 -1.20000 AFIX 0 C9 1 0.167521 0.771416 0.202230 21.00000 0.02478 0.03505 = 0.04252 -0.00597 0.01290 -0.01339 AFIX 43 H9 2 0.104301 0.737475 0.202871 21.00000 -1.20000 AFIX 0 C10 1 0.166254 0.796551 0.090479 21.00000 0.02459 0.03433 = 0.03912 -0.00637 0.00776 -0.00907 AFIX 43 H10 2 0.101955 0.780214 0.015203 21.00000 -1.20000 AFIX 0 C11 1 0.263201 0.846640 0.093714 21.00000 0.02119 0.02958 = 0.02340 -0.00307 0.00123 -0.00693 AFIX 43 H11 2 0.262204 0.863073 0.018597 21.00000 -1.20000 AFIX 0 N4 4 0.358080 0.872661 0.198773 21.00000 0.01911 0.01913 = 0.01748 -0.00016 0.00710 -0.00186 PART 2 N1' 4 0.377968 0.878548 0.238845 -21.00000 0.02712 0.02411 = 0.01912 -0.00329 0.00803 0.00278 C1' 1 0.278080 0.850181 0.138732 -21.00000 0.03091 0.03891 = 0.02519 -0.00213 0.00915 -0.00265 AFIX 43 H1' 2 0.271747 0.863508 0.060346 -21.00000 -1.20000 AFIX 0 C2' 1 0.183947 0.801897 0.147021 -21.00000 0.03522 0.04631 = 0.03764 -0.00646 0.00871 -0.00968 AFIX 43 H2' 2 0.113781 0.784576 0.076477 -21.00000 -1.20000 AFIX 0 C3' 1 0.199270 0.780631 0.265366 -21.00000 0.03517 0.04149 = 0.04627 -0.00337 0.01534 -0.01339 AFIX 43 H3' 2 0.140352 0.746774 0.274681 -21.00000 -1.20000 AFIX 0 C4' 1 0.299141 0.808687 0.367385 -21.00000 0.02965 0.03202 = 0.03803 -0.00060 0.01508 -0.00608 AFIX 43 H4' 2 0.308199 0.795176 0.446545 -21.00000 -1.20000 AFIX 0 C5' 1 0.387993 0.858154 0.351444 -21.00000 0.02058 0.01986 = 0.02223 0.00000 0.01085 0.00145 N2' 4 0.488742 0.887738 0.452698 -21.00000 0.02000 0.02469 = 0.01584 -0.00044 0.00735 -0.00245 AFIX 43 H2'A 2 0.493246 0.878841 0.525905 -21.00000 -1.20000 AFIX 0 N3' 4 0.580655 0.930580 0.438521 -21.00000 0.01543 0.01567 = 0.01199 0.00035 0.00522 0.00105 C6' 1 0.676532 0.955197 0.538227 -21.00000 0.01755 0.02318 = 0.00601 -0.00324 -0.00058 0.00208 AFIX 43 H6' 2 0.680870 0.941845 0.615935 -21.00000 -1.20000 AFIX 0 C7' 1 0.776220 1.003176 0.528642 -21.00000 0.01320 0.01745 = 0.01962 -0.00218 0.00352 0.00154 C8' 1 0.874539 1.033362 0.636356 -21.00000 0.01811 0.02952 = 0.01483 -0.00456 -0.00172 -0.00542 AFIX 43 H8' 2 0.879996 1.020580 0.714666 -21.00000 -1.20000 AFIX 0 C9' 1 0.961933 1.082109 0.622454 -21.00000 0.02165 0.02550 = 0.03001 -0.00650 0.00181 -0.00372 AFIX 43 H9' 2 1.027339 1.103938 0.691992 -21.00000 -1.20000 AFIX 0 C10' 1 0.953657 1.099161 0.505559 -21.00000 0.02599 0.02275 = 0.03318 -0.00208 0.00700 -0.00223 AFIX 43 H10' 2 1.013469 1.131946 0.495294 -21.00000 -1.20000 AFIX 0 C11' 1 0.854169 1.066324 0.403730 -21.00000 0.02101 0.02123 = 0.02612 -0.00113 0.00968 -0.00307 AFIX 43 H11' 2 0.848158 1.078181 0.324895 -21.00000 -1.20000 AFIX 0 N4' 4 0.767631 1.019053 0.413402 -21.00000 0.01423 0.01785 = 0.01501 -0.00023 0.00459 0.00425 SAME 0.02 0.04 N5' > O8' PART 1 N5 4 0.811987 0.771693 0.622690 41.00000 0.03043 0.02185 = 0.03429 0.00977 0.01651 0.00661 O6 5 0.875704 0.814037 0.584722 41.00000 0.04399 0.06409 = 0.09000 0.05050 0.03693 0.00824 O7 5 0.694050 0.763575 0.554828 41.00000 0.04071 0.02546 = 0.03468 0.00357 -0.00538 -0.01309 O8 5 0.862337 0.741499 0.727065 41.00000 0.02822 0.05914 = 0.03627 0.02328 0.00310 -0.01002 PART 2 N5' 4 0.800013 0.750105 0.599302 -41.00000 0.03043 0.02185 = 0.03429 0.00977 0.01651 0.00661 O6' 5 0.868778 0.771709 0.548039 -41.00000 0.04399 0.06409 = 0.09000 0.05050 0.03693 0.00824 O7' 5 0.681568 0.748353 0.543177 -41.00000 0.04071 0.02546 = 0.03468 0.00357 -0.00538 -0.01309 O8' 5 0.853553 0.719134 0.700952 -41.00000 0.02822 0.05914 = 0.03627 0.02328 0.00310 -0.01002 PART 0 O9 5 0.042108 0.889791 -0.167332 10.25000 0.04749 0.06870 = 0.04694 -0.01678 -0.00373 0.00746 H9A 2 0.015926 0.906612 -0.232187 10.25000 -1.50000 H9B 2 -0.009861 0.861042 -0.170436 10.25000 -1.50000 HKLF 4 REM it4 in P 21/c REM wR2 = 0.0638, GooF = S = 1.041, Restrained GooF = 1.008 for all data REM R1 = 0.0387 for 7368 Fo > 4sig(Fo) and 0.0774 for all 10392 data REM 451 parameters refined using 781 restraints END WGHT 0.0112 1.5461 REM Instructions for potential hydrogen bonds HTAB O1 O6 HTAB O1 O7 HTAB O1 O6' HTAB O1 O8_$2 HTAB O1 O8'_$2 HTAB O2 O4_$1 HTAB O2 O7_$2 HTAB O2 N5'_$2 HTAB O2 O7'_$2 HTAB C13 O7_$5 HTAB C13 O7'_$5 HTAB C13 O7_$3 HTAB C15 O9 HTAB C2 O6_$4 HTAB N2 O5_$3 HTAB C6 O5_$3 HTAB C11 O9 HTAB N2' O5_$3 HTAB C6' O5_$3 HTAB C10' O6'_$4 HTAB O9 O6_$6 HTAB O9 O8_$6 REM Highest difference peak 1.262, deepest hole -0.945, 1-sigma level 0.141 Q1 1 0.5452 0.9394 0.2339 11.00000 0.05 1.26 ; _shelx_res_checksum 54180 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group La La1 0.56737(2) 0.95905(2) 0.20467(2) 0.01520(3) Uani d 1 . . O O1 0.71353(15) 0.84746(8) 0.31638(13) 0.0207(3) Uani d 1 . . H H1A 0.737(2) 0.8335(14) 0.3831(15) 0.031 Uiso d 1 . . H H1B 0.753(2) 0.8249(13) 0.289(2) 0.031 Uiso d 1 . . O O2 0.52181(16) 0.84992(8) 0.05463(13) 0.0247(3) Uani d 1 . . H H2A 0.490(2) 0.8580(14) -0.0147(14) 0.037 Uiso d 1 . . H H2B 0.574(2) 0.8205(13) 0.062(2) 0.037 Uiso d 1 . . O O3 0.77181(16) 0.96048(9) 0.16251(13) 0.0295(3) Uani d 1 . . O O4 0.57600(14) 1.10181(8) 0.18261(12) 0.0218(3) Uani d 1 . . O O5 0.46089(19) 1.06485(10) 0.28544(14) 0.0360(4) Uani d 1 . . C C12 0.5029(2) 1.11655(12) 0.23852(17) 0.0263(5) Uani d 1 . . C C13 0.4664(3) 1.19661(14) 0.2475(2) 0.0449(7) Uani d 1 . . H H13A 0.431738 1.218889 0.166320 0.067 Uiso calc 1 . . H H13B 0.543322 1.223772 0.300997 0.067 Uiso calc 1 . . H H13C 0.400921 1.198418 0.280778 0.067 Uiso calc 1 . . O O10 0.37451(14) 0.99521(9) 0.01294(13) 0.0248(3) Uani d 1 . . C C14 0.2633(2) 1.02384(12) -0.05024(18) 0.0207(4) Uani d 1 . . C C15 0.1712(3) 1.04094(18) 0.0093(2) 0.0452(7) Uani d 1 . . H H15A 0.104232 1.002998 -0.012831 0.068 Uiso calc 1 . . H H15B 0.130825 1.088904 -0.018859 0.068 Uiso calc 1 . . H H15C 0.219407 1.041944 0.097847 0.068 Uiso calc 1 . . N N1 0.7389(8) 1.0127(6) 0.4165(8) 0.0154(11) Uani d 0.547(8) A 1 C C1 0.8351(10) 1.0594(7) 0.4194(8) 0.0221(14) Uani d 0.547(8) A 1 H H1 0.837759 1.072530 0.344276 0.026 Uiso calc 0.547(8) A 1 C C2 0.9305(7) 1.0891(5) 0.5271(6) 0.0234(12) Uani d 0.547(8) A 1 H H2 0.993945 1.122342 0.524696 0.028 Uiso calc 0.547(8) A 1 C C3 0.9276(6) 1.0672(4) 0.6394(5) 0.0228(10) Uani d 0.547(8) A 1 H H3 0.990764 1.085119 0.714130 0.027 Uiso calc 0.547(8) A 1 C C4 0.8317(6) 1.0194(3) 0.6390(5) 0.0207(10) Uani d 0.547(8) A 1 H H4 0.828457 1.004507 0.713141 0.025 Uiso calc 0.547(8) A 1 C C5 0.7388(6) 0.9932(4) 0.5261(5) 0.0123(9) Uani d 0.547(8) A 1 N N2 0.6401(5) 0.9460(4) 0.5246(6) 0.0156(10) Uani d 0.547(8) A 1 H H2C 0.637201 0.932701 0.593393 0.019 Uiso calc 0.547(8) A 1 N N3 0.5482(6) 0.9206(4) 0.4163(6) 0.0154(10) Uani d 0.547(8) A 1 C C6 0.4571(7) 0.8775(4) 0.4207(6) 0.0175(10) Uani d 0.547(8) A 1 H H6 0.455719 0.865341 0.496698 0.021 Uiso calc 0.547(8) A 1 C C7 0.3572(5) 0.8483(3) 0.3071(5) 0.0192(9) Uani d 0.547(8) A 1 C C8 0.2639(6) 0.7974(3) 0.3128(6) 0.0279(11) Uani d 0.547(8) A 1 H H8 0.266593 0.781473 0.388808 0.034 Uiso calc 0.547(8) A 1 C C9 0.1675(5) 0.7714(3) 0.2022(7) 0.0344(13) Uani d 0.547(8) A 1 H H9 0.104301 0.737475 0.202871 0.041 Uiso calc 0.547(8) A 1 C C10 0.1663(5) 0.7966(3) 0.0905(6) 0.0344(12) Uani d 0.547(8) A 1 H H10 0.101955 0.780214 0.015203 0.041 Uiso calc 0.547(8) A 1 C C11 0.2632(6) 0.8466(4) 0.0937(6) 0.0273(12) Uani d 0.547(8) A 1 H H11 0.262204 0.863073 0.018597 0.033 Uiso calc 0.547(8) A 1 N N4 0.3581(6) 0.8727(3) 0.1988(5) 0.0187(9) Uani d 0.547(8) A 1 N N1' 0.3780(8) 0.8785(5) 0.2388(6) 0.0239(13) Uani d 0.453(8) A 2 C C1' 0.2781(9) 0.8502(5) 0.1387(7) 0.0324(15) Uani d 0.453(8) A 2 H H1' 0.271747 0.863508 0.060346 0.039 Uiso calc 0.453(8) A 2 C C2' 0.1839(8) 0.8019(5) 0.1470(8) 0.0418(16) Uani d 0.453(8) A 2 H H2' 0.113781 0.784576 0.076477 0.050 Uiso calc 0.453(8) A 2 C C3' 0.1993(8) 0.7806(4) 0.2654(9) 0.0414(16) Uani d 0.453(8) A 2 H H3' 0.140352 0.746774 0.274681 0.050 Uiso calc 0.453(8) A 2 C C4' 0.2991(7) 0.8087(4) 0.3674(8) 0.0328(14) Uani d 0.453(8) A 2 H H4' 0.308199 0.795176 0.446545 0.039 Uiso calc 0.453(8) A 2 C C5' 0.3880(7) 0.8582(4) 0.3514(7) 0.0202(11) Uani d 0.453(8) A 2 N N2' 0.4887(7) 0.8877(4) 0.4527(6) 0.0202(12) Uani d 0.453(8) A 2 H H2'A 0.493246 0.878841 0.525905 0.024 Uiso calc 0.453(8) A 2 N N3' 0.5807(7) 0.9306(5) 0.4385(7) 0.0145(12) Uani d 0.453(8) A 2 C C6' 0.6765(8) 0.9552(6) 0.5382(8) 0.0174(13) Uani d 0.453(8) A 2 H H6' 0.680870 0.941845 0.615935 0.021 Uiso calc 0.453(8) A 2 C C7' 0.7762(7) 1.0032(5) 0.5286(7) 0.0178(13) Uani d 0.453(8) A 2 C C8' 0.8745(7) 1.0334(4) 0.6364(6) 0.0236(13) Uani d 0.453(8) A 2 H H8' 0.879996 1.020580 0.714666 0.028 Uiso calc 0.453(8) A 2 C C9' 0.9619(8) 1.0821(4) 0.6225(7) 0.0286(14) Uani d 0.453(8) A 2 H H9' 1.027339 1.103938 0.691992 0.034 Uiso calc 0.453(8) A 2 C C10' 0.9537(9) 1.0992(6) 0.5056(8) 0.0290(16) Uani d 0.453(8) A 2 H H10' 1.013469 1.131946 0.495294 0.035 Uiso calc 0.453(8) A 2 C C11' 0.8542(12) 1.0663(8) 0.4037(10) 0.0228(17) Uani d 0.453(8) A 2 H H11' 0.848158 1.078181 0.324895 0.027 Uiso calc 0.453(8) A 2 N N4' 0.7676(9) 1.0191(7) 0.4134(9) 0.0162(14) Uani d 0.453(8) A 2 N N5 0.8120(3) 0.7717(2) 0.6227(3) 0.0278(7) Uani d 0.826(9) B 1 O O6 0.8757(3) 0.8140(3) 0.5847(4) 0.0629(13) Uani d 0.826(9) B 1 O O7 0.6941(4) 0.7636(2) 0.5548(5) 0.0405(8) Uani d 0.826(9) B 1 O O8 0.8623(4) 0.7415(2) 0.7271(3) 0.0445(10) Uani d 0.826(9) B 1 N N5' 0.8000(16) 0.7501(9) 0.5993(15) 0.0278(7) Uani d 0.174(9) B 2 O O6' 0.8688(15) 0.7717(12) 0.5480(17) 0.0629(13) Uani d 0.174(9) B 2 O O7' 0.6816(18) 0.7484(13) 0.543(3) 0.0405(8) Uani d 0.174(9) B 2 O O8' 0.854(2) 0.7191(12) 0.7010(16) 0.0445(10) Uani d 0.174(9) B 2 O O9 0.0421(9) 0.8898(6) -0.1673(8) 0.062(3) Uani d 0.25 . . H H9A 0.016(14) 0.907(8) -0.232(6) 0.093 Uiso d 0.25 . . H H9B -0.010(11) 0.861(7) -0.170(13) 0.093 Uiso d 0.25 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 La1 0.01924(6) 0.01380(5) 0.01228(5) 0.00382(5) 0.00618(4) 0.00176(4) O1 0.0285(8) 0.0184(7) 0.0151(6) 0.0072(6) 0.0089(6) 0.0030(5) O2 0.0375(9) 0.0191(7) 0.0136(6) 0.0035(6) 0.0064(6) 0.0031(5) O3 0.0304(8) 0.0409(9) 0.0196(7) 0.0064(7) 0.0127(6) 0.0083(7) O4 0.0318(8) 0.0186(7) 0.0125(6) 0.0045(6) 0.0064(6) 0.0011(5) O5 0.0626(12) 0.0311(9) 0.0273(8) 0.0265(8) 0.0317(8) 0.0145(7) C12 0.0427(13) 0.0244(11) 0.0113(8) 0.0151(10) 0.0105(8) 0.0025(7) C13 0.083(2) 0.0246(13) 0.0345(13) 0.0207(13) 0.0311(14) 0.0021(10) O10 0.0201(7) 0.0258(8) 0.0238(7) 0.0059(6) 0.0043(6) 0.0010(6) C14 0.0190(9) 0.0258(11) 0.0193(9) 0.0010(8) 0.0098(8) 0.0030(7) C15 0.0315(13) 0.078(2) 0.0347(13) 0.0181(14) 0.0220(11) 0.0165(14) N1 0.015(3) 0.019(2) 0.0153(16) -0.002(2) 0.0085(18) -0.0007(13) C1 0.025(3) 0.027(3) 0.018(2) -0.004(2) 0.0123(18) 0.0013(18) C2 0.022(3) 0.023(3) 0.026(2) -0.0031(18) 0.0110(18) -0.0020(18) C3 0.018(3) 0.026(3) 0.0196(19) -0.0020(19) 0.0038(17) -0.0042(18) C4 0.019(2) 0.025(2) 0.0144(16) -0.0004(18) 0.0029(17) -0.0022(15) C5 0.011(2) 0.015(2) 0.0098(14) 0.0023(17) 0.0035(17) -0.0005(13) N2 0.017(2) 0.019(2) 0.012(2) -0.0026(18) 0.0074(19) 0.0022(15) N3 0.016(3) 0.014(2) 0.015(2) 0.0019(17) 0.0041(18) -0.0014(15) C6 0.020(3) 0.018(2) 0.017(3) -0.0020(19) 0.010(2) 0.0026(19) C7 0.017(2) 0.0185(19) 0.022(2) -0.0021(15) 0.0081(18) -0.0042(17) C8 0.027(3) 0.026(2) 0.033(3) -0.0114(19) 0.014(2) -0.003(2) C9 0.025(2) 0.035(3) 0.043(3) -0.0134(19) 0.013(2) -0.006(2) C10 0.025(2) 0.034(2) 0.039(3) -0.0091(18) 0.008(2) -0.006(2) C11 0.021(2) 0.030(2) 0.023(2) -0.0069(17) 0.001(2) -0.003(2) N4 0.019(2) 0.0191(19) 0.017(2) -0.0019(15) 0.0071(19) -0.0002(19) N1' 0.027(3) 0.024(2) 0.019(3) 0.003(2) 0.008(2) -0.003(2) C1' 0.031(3) 0.039(3) 0.025(3) -0.003(2) 0.009(3) -0.002(3) C2' 0.035(3) 0.046(4) 0.038(3) -0.010(3) 0.009(3) -0.006(3) C3' 0.035(4) 0.041(4) 0.046(4) -0.013(3) 0.015(3) -0.003(3) C4' 0.030(3) 0.032(3) 0.038(3) -0.006(2) 0.015(3) -0.001(3) C5' 0.021(3) 0.020(2) 0.022(3) 0.0015(19) 0.011(2) 0.000(2) N2' 0.020(3) 0.025(3) 0.016(3) -0.002(2) 0.007(2) 0.000(2) N3' 0.015(3) 0.016(3) 0.012(3) 0.001(2) 0.005(2) 0.0004(19) C6' 0.018(3) 0.023(3) 0.0060(19) 0.002(2) -0.001(2) -0.0032(19) C7' 0.013(3) 0.017(3) 0.020(2) 0.002(2) 0.004(2) -0.0022(17) C8' 0.018(3) 0.030(3) 0.0148(19) -0.005(2) -0.002(2) -0.005(2) C9' 0.022(3) 0.025(3) 0.030(3) -0.004(2) 0.002(2) -0.006(2) C10' 0.026(3) 0.023(3) 0.033(3) -0.002(2) 0.007(2) -0.002(2) C11' 0.021(3) 0.021(3) 0.026(3) -0.003(2) 0.010(2) -0.001(2) N4' 0.014(3) 0.018(3) 0.015(2) 0.004(2) 0.005(2) -0.0002(17) N5 0.0304(12) 0.0219(16) 0.0343(15) 0.0066(12) 0.0165(12) 0.0098(12) O6 0.0440(13) 0.064(3) 0.090(2) 0.0082(16) 0.0369(15) 0.050(2) O7 0.0407(14) 0.025(2) 0.0347(14) -0.0131(11) -0.0054(11) 0.0036(14) O8 0.0282(11) 0.059(3) 0.0363(16) -0.0100(16) 0.0031(13) 0.0233(15) N5' 0.0304(12) 0.0219(16) 0.0343(15) 0.0066(12) 0.0165(12) 0.0098(12) O6' 0.0440(13) 0.064(3) 0.090(2) 0.0082(16) 0.0369(15) 0.050(2) O7' 0.0407(14) 0.025(2) 0.0347(14) -0.0131(11) -0.0054(11) 0.0036(14) O8' 0.0282(11) 0.059(3) 0.0363(16) -0.0100(16) 0.0031(13) 0.0233(15) O9 0.047(5) 0.069(7) 0.047(5) 0.007(5) -0.004(4) -0.017(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 La1 O5 . . 131.31(5) ? O1 La1 N1 . . 74.6(2) ? O1 La1 N3 . . 66.31(17) ? O1 La1 N4 . . 85.96(14) ? O1 La1 N1' . . 83.07(18) ? O1 La1 N3' . . 65.1(2) ? O1 La1 N4' . . 74.6(3) ? O2 La1 O1 . . 70.56(5) ? O2 La1 O4 . . 134.03(4) ? O2 La1 O5 . . 145.03(6) ? O2 La1 N1 . . 143.4(2) ? O2 La1 N3 . . 112.63(15) ? O2 La1 N4 . . 68.32(13) ? O2 La1 N1' . . 75.71(16) ? O2 La1 N3' . . 118.17(18) ? O2 La1 N4' . . 140.7(3) ? O3 La1 O1 . . 71.15(5) ? O3 La1 O2 . . 78.91(6) ? O3 La1 O4 . . 84.00(5) ? O3 La1 O5 . . 130.31(6) ? O3 La1 N1 . . 79.82(16) ? O3 La1 N3 . . 127.56(15) ? O3 La1 N4 . . 144.90(14) ? O3 La1 N1' . . 148.59(18) ? O3 La1 N3' . . 121.26(17) ? O3 La1 N4' . . 73.2(2) ? O4 La1 O1 . . 141.26(5) ? O4 La1 O5 . . 50.23(5) ? O4 La1 N1 . . 72.1(2) ? O4 La1 N3 . . 111.64(16) ? O4 La1 N4 . . 128.03(14) ? O4 La1 N1' . . 127.18(18) ? O4 La1 N3' . . 107.23(19) ? O4 La1 N4' . . 69.9(2) ? O5 La1 N1 . . 69.4(2) ? O5 La1 N3 . . 67.84(17) ? O5 La1 N4 . . 84.78(14) ? O5 La1 N1' . . 80.33(18) ? O5 La1 N3' . . 67.2(2) ? O5 La1 N4' . . 73.4(2) ? O10 La1 O1 . . 143.00(5) ? O10 La1 O2 . . 73.27(5) ? O10 La1 O3 . . 109.21(5) ? O10 La1 O4 . . 72.76(5) ? O10 La1 O5 . . 78.09(5) ? O10 La1 N1 . . 142.4(2) ? O10 La1 N3 . . 123.20(15) ? O10 La1 N4 . . 73.67(12) ? O10 La1 N1' . . 80.82(16) ? O10 La1 N3' . . 129.37(18) ? O10 La1 N4' . . 142.2(3) ? N1 La1 N3 . . 60.63(17) ? N1 La1 N4 . . 120.08(16) ? N3 La1 N4 . . 59.61(13) ? N1' La1 N3' . . 58.56(16) ? N1' La1 N4' . . 117.50(19) ? N3' La1 N4' . . 59.0(2) ? La1 O1 H1A . . 131.3(18) ? La1 O1 H1B . . 123.4(18) ? H1A O1 H1B . . 105(2) ? La1 O2 H2A . . 118.5(19) ? La1 O2 H2B . . 122(2) ? H2A O2 H2B . . 105(2) ? C14 O3 La1 3_675 . 107.31(13) ? C12 O4 La1 . . 95.42(13) ? C12 O5 La1 . . 93.60(13) ? O4 C12 C13 . . 118.9(2) ? O5 C12 O4 . . 120.66(19) ? O5 C12 C13 . . 120.4(2) ? C12 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? C12 C13 H13C . . 109.5 ? H13A C13 H13B . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? La1 O10 La1 . 3_675 116.24(6) ? C14 O10 La1 . 3_675 83.51(11) ? C14 O10 La1 . . 156.33(14) ? O3 C14 La1 3_675 3_675 50.25(10) ? O3 C14 O10 3_675 . 121.44(19) ? O3 C14 C15 3_675 . 118.55(19) ? O10 C14 La1 . 3_675 72.88(11) ? O10 C14 C15 . . 120.00(19) ? C15 C14 La1 . 3_675 161.51(17) ? C14 C15 H15A . . 109.5 ? C14 C15 H15B . . 109.5 ? C14 C15 H15C . . 109.5 ? H15A C15 H15B . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? C1 N1 La1 . . 120.6(5) ? C5 N1 La1 . . 122.5(4) ? C5 N1 C1 . . 116.8(6) ? N1 C1 H1 . . 117.9 ? N1 C1 C2 . . 124.2(6) ? C2 C1 H1 . . 117.9 ? C1 C2 H2 . . 121.4 ? C1 C2 C3 . . 117.2(5) ? C3 C2 H2 . . 121.4 ? C2 C3 H3 . . 120.2 ? C4 C3 C2 . . 119.6(5) ? C4 C3 H3 . . 120.2 ? C3 C4 H4 . . 120.5 ? C3 C4 C5 . . 119.1(5) ? C5 C4 H4 . . 120.5 ? N1 C5 C4 . . 123.0(5) ? N1 C5 N2 . . 117.5(5) ? N2 C5 C4 . . 119.5(5) ? C5 N2 H2C . . 119.7 ? N3 N2 C5 . . 120.5(5) ? N3 N2 H2C . . 119.7 ? N2 N3 La1 . . 118.6(4) ? C6 N3 La1 . . 123.6(4) ? C6 N3 N2 . . 117.8(6) ? N3 C6 H6 . . 120.1 ? N3 C6 C7 . . 119.8(5) ? C7 C6 H6 . . 120.1 ? C8 C7 C6 . . 119.5(5) ? N4 C7 C6 . . 117.4(4) ? N4 C7 C8 . . 123.1(4) ? C7 C8 H8 . . 120.9 ? C9 C8 C7 . . 118.2(5) ? C9 C8 H8 . . 120.9 ? C8 C9 H9 . . 120.3 ? C8 C9 C10 . . 119.4(5) ? C10 C9 H9 . . 120.3 ? C9 C10 H10 . . 120.8 ? C9 C10 C11 . . 118.5(5) ? C11 C10 H10 . . 120.8 ? C10 C11 H11 . . 118.1 ? N4 C11 C10 . . 123.8(5) ? N4 C11 H11 . . 118.1 ? C7 N4 La1 . . 119.1(3) ? C11 N4 La1 . . 123.4(4) ? C11 N4 C7 . . 117.1(5) ? C1' N1' La1 . . 118.7(5) ? C5' N1' La1 . . 122.6(4) ? C5' N1' C1' . . 118.2(7) ? N1' C1' H1' . . 118.5 ? N1' C1' C2' . . 123.0(7) ? C2' C1' H1' . . 118.5 ? C1' C2' H2' . . 121.5 ? C1' C2' C3' . . 117.1(6) ? C3' C2' H2' . . 121.5 ? C2' C3' H3' . . 119.6 ? C4' C3' C2' . . 120.7(6) ? C4' C3' H3' . . 119.6 ? C3' C4' H4' . . 120.6 ? C3' C4' C5' . . 118.8(6) ? C5' C4' H4' . . 120.6 ? N1' C5' C4' . . 122.1(6) ? N1' C5' N2' . . 118.0(6) ? N2' C5' C4' . . 119.9(6) ? C5' N2' H2'A . . 119.8 ? N3' N2' C5' . . 120.3(6) ? N3' N2' H2'A . . 119.8 ? N2' N3' La1 . . 120.0(4) ? C6' N3' La1 . . 122.3(6) ? C6' N3' N2' . . 117.6(7) ? N3' C6' H6' . . 120.0 ? N3' C6' C7' . . 120.1(7) ? C7' C6' H6' . . 120.0 ? C8' C7' C6' . . 119.7(6) ? N4' C7' C6' . . 117.6(6) ? N4' C7' C8' . . 122.6(6) ? C7' C8' H8' . . 121.1 ? C9' C8' C7' . . 117.7(6) ? C9' C8' H8' . . 121.1 ? C8' C9' H9' . . 119.9 ? C8' C9' C10' . . 120.2(6) ? C10' C9' H9' . . 119.9 ? C9' C10' H10' . . 120.8 ? C9' C10' C11' . . 118.5(7) ? C11' C10' H10' . . 120.8 ? C10' C11' H11' . . 118.5 ? N4' C11' C10' . . 123.1(8) ? N4' C11' H11' . . 118.5 ? C7' N4' La1 . . 120.9(5) ? C11' N4' La1 . . 121.2(6) ? C11' N4' C7' . . 117.9(8) ? O6 N5 O8 . . 122.0(3) ? O7 N5 O6 . . 116.7(3) ? O7 N5 O8 . . 121.2(4) ? O6' N5' O8' . . 118.5(17) ? O7' N5' O6' . . 120.1(19) ? O7' N5' O8' . . 120.4(19) ? H9A O9 H9B . . 104(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag La1 O1 . 2.5659(14) ? La1 O2 . 2.5395(15) ? La1 O3 . 2.5184(16) ? La1 O4 . 2.5653(15) ? La1 O5 . 2.6073(16) ? La1 O10 . 2.4814(14) ? La1 N1 . 2.626(8) ? La1 N3 . 2.683(7) ? La1 N4 . 2.768(6) ? La1 N1' . 2.712(8) ? La1 N3' . 2.752(8) ? La1 N4' . 2.771(9) ? O1 H1A . 0.763(14) ? O1 H1B . 0.760(14) ? O2 H2A . 0.761(14) ? O2 H2B . 0.761(14) ? O3 C14 3_675 1.251(2) ? O4 C12 . 1.267(3) ? O5 C12 . 1.260(3) ? C12 C13 . 1.500(3) ? C13 H13A . 0.9600 ? C13 H13B . 0.9600 ? C13 H13C . 0.9600 ? O10 C14 . 1.261(2) ? C14 C15 . 1.491(3) ? C15 H15A . 0.9600 ? C15 H15B . 0.9600 ? C15 H15C . 0.9600 ? N1 C1 . 1.345(7) ? N1 C5 . 1.340(8) ? C1 H1 . 0.9300 ? C1 C2 . 1.385(9) ? C2 H2 . 0.9300 ? C2 C3 . 1.396(7) ? C3 H3 . 0.9300 ? C3 C4 . 1.364(6) ? C4 H4 . 0.9300 ? C4 C5 . 1.390(6) ? C5 N2 . 1.377(6) ? N2 H2C . 0.8600 ? N2 N3 . 1.346(6) ? N3 C6 . 1.289(7) ? C6 H6 . 0.9300 ? C6 C7 . 1.443(6) ? C7 C8 . 1.400(7) ? C7 N4 . 1.355(6) ? C8 H8 . 0.9300 ? C8 C9 . 1.386(6) ? C9 H9 . 0.9300 ? C9 C10 . 1.388(7) ? C10 H10 . 0.9300 ? C10 C11 . 1.388(7) ? C11 H11 . 0.9300 ? C11 N4 . 1.339(6) ? N1' C1' . 1.345(8) ? N1' C5' . 1.338(7) ? C1' H1' . 0.9300 ? C1' C2' . 1.389(10) ? C2' H2' . 0.9300 ? C2' C3' . 1.390(9) ? C3' H3' . 0.9300 ? C3' C4' . 1.356(8) ? C4' H4' . 0.9300 ? C4' C5' . 1.394(8) ? C5' N2' . 1.365(6) ? N2' H2'A . 0.8600 ? N2' N3' . 1.340(8) ? N3' C6' . 1.298(7) ? C6' H6' . 0.9300 ? C6' C7' . 1.441(8) ? C7' C8' . 1.401(8) ? C7' N4' . 1.355(10) ? C8' H8' . 0.9300 ? C8' C9' . 1.363(8) ? C9' H9' . 0.9300 ? C9' C10' . 1.379(9) ? C10' H10' . 0.9300 ? C10' C11' . 1.386(11) ? C11' H11' . 0.9300 ? C11' N4' . 1.319(9) ? N5 O6 . 1.238(3) ? N5 O7 . 1.233(4) ? N5 O8 . 1.248(3) ? N5' O6' . 1.216(14) ? N5' O7' . 1.208(15) ? N5' O8' . 1.231(15) ? O9 H9A . 0.761(16) ? O9 H9B . 0.762(16) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1A O6 . 0.763(14) 2.271(17) 2.994(3) 158(3) yes O1 H1A O7 . 0.763(14) 2.586(19) 3.273(6) 151(2) yes O1 H1A O6' . 0.763(14) 2.19(2) 2.901(14) 154(2) yes O1 H1B O8 4_575 0.760(14) 2.034(15) 2.793(4) 176(3) yes O1 H1B O8' 4_575 0.760(14) 1.97(3) 2.73(2) 171(3) yes O2 H2A O4 3_675 0.761(14) 1.948(15) 2.6971(19) 168(3) yes O2 H2B O7 4_575 0.761(14) 2.032(16) 2.786(4) 171(3) yes O2 H2B N5' 4_575 0.761(14) 2.68(2) 3.419(16) 164(3) yes O2 H2B O7' 4_575 0.761(14) 1.79(3) 2.54(2) 167(3) yes C13 H13A O7 2_655 0.96 2.53 3.483(5) 170.2 yes C13 H13A O7' 2_655 0.96 2.33 3.27(3) 167.0 yes C13 H13C O7 3_676 0.96 2.65 3.544(6) 155.0 yes C15 H15A O9 . 0.96 2.62 3.350(10) 133.4 yes C2 H2 O6 3_776 0.93 2.57 3.420(6) 152.6 yes N2 H2C O5 3_676 0.86 2.13 2.898(7) 149.2 yes C11 H11 O9 . 0.93 2.57 3.150(10) 120.5 yes N2' H2'A O5 3_676 0.86 2.30 3.028(7) 142.3 yes C6' H6' O5 3_676 0.93 2.32 3.067(9) 137.7 yes C10' H10' O6' 3_776 0.93 2.34 3.260(18) 169.8 yes O9 H9A O6 1_454 0.761(16) 2.66(14) 3.062(9) 115(13) yes O9 H9B O8 1_454 0.762(16) 2.57(10) 3.241(11) 147(16) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag La1 O4 C12 O5 . . . . 3.1(2) ? La1 O4 C12 C13 . . . . -176.59(19) ? La1 O5 C12 O4 . . . . -3.0(2) ? La1 O5 C12 C13 . . . . 176.64(19) ? La1 O10 C14 La1 . . . 3_675 148.0(3) ? La1 O10 C14 O3 3_675 . . 3_675 13.4(2) ? La1 O10 C14 O3 . . . 3_675 161.5(2) ? La1 O10 C14 C15 3_675 . . . -165.5(2) ? La1 O10 C14 C15 . . . . -17.4(5) ? La1 N1 C1 C2 . . . . -178.9(9) ? La1 N1 C5 C4 . . . . 177.9(5) ? La1 N1 C5 N2 . . . . -3.2(10) ? La1 N3 C6 C7 . . . . -1.0(9) ? La1 N1' C1' C2' . . . . 173.1(7) ? La1 N1' C5' C4' . . . . -171.4(5) ? La1 N1' C5' N2' . . . . 9.0(9) ? La1 N3' C6' C7' . . . . 4.1(12) ? N1 C1 C2 C3 . . . . 1.8(15) ? N1 C5 N2 N3 . . . . 0.3(10) ? C1 N1 C5 C4 . . . . 0.5(12) ? C1 N1 C5 N2 . . . . 179.4(8) ? C1 C2 C3 C4 . . . . -1.1(11) ? C2 C3 C4 C5 . . . . 0.3(9) ? C3 C4 C5 N1 . . . . 0.1(10) ? C3 C4 C5 N2 . . . . -178.8(6) ? C4 C5 N2 N3 . . . . 179.3(6) ? C5 N1 C1 C2 . . . . -1.5(15) ? C5 N2 N3 La1 . . . . 2.5(8) ? C5 N2 N3 C6 . . . . -179.0(7) ? N2 N3 C6 C7 . . . . -179.4(6) ? N3 C6 C7 C8 . . . . 175.6(6) ? N3 C6 C7 N4 . . . . -5.1(9) ? C6 C7 C8 C9 . . . . 178.7(5) ? C6 C7 N4 La1 . . . . 8.3(7) ? C6 C7 N4 C11 . . . . -178.5(6) ? C7 C8 C9 C10 . . . . -0.2(8) ? C8 C7 N4 La1 . . . . -172.4(4) ? C8 C7 N4 C11 . . . . 0.8(9) ? C8 C9 C10 C11 . . . . 0.6(9) ? C9 C10 C11 N4 . . . . -0.4(10) ? C10 C11 N4 La1 . . . . 172.5(5) ? C10 C11 N4 C7 . . . . -0.3(10) ? N4 C7 C8 C9 . . . . -0.6(8) ? N1' C1' C2' C3' . . . . -2.6(13) ? N1' C5' N2' N3' . . . . -5.7(11) ? C1' N1' C5' C4' . . . . 0.3(11) ? C1' N1' C5' N2' . . . . -179.3(7) ? C1' C2' C3' C4' . . . . 2.6(12) ? C2' C3' C4' C5' . . . . -1.3(11) ? C3' C4' C5' N1' . . . . -0.2(11) ? C3' C4' C5' N2' . . . . 179.4(7) ? C4' C5' N2' N3' . . . . 174.7(8) ? C5' N1' C1' C2' . . . . 1.2(13) ? C5' N2' N3' La1 . . . . -0.2(10) ? C5' N2' N3' C6' . . . . -177.8(8) ? N2' N3' C6' C7' . . . . -178.3(8) ? N3' C6' C7' C8' . . . . 175.9(9) ? N3' C6' C7' N4' . . . . -2.0(13) ? C6' C7' C8' C9' . . . . -176.0(7) ? C6' C7' N4' La1 . . . . -1.0(12) ? C6' C7' N4' C11' . . . . 176.2(10) ? C7' C8' C9' C10' . . . . -1.3(11) ? C8' C7' N4' La1 . . . . -178.9(6) ? C8' C7' N4' C11' . . . . -1.7(15) ? C8' C9' C10' C11' . . . . 0.7(14) ? C9' C10' C11' N4' . . . . -0.6(18) ? C10' C11' N4' La1 . . . . 178.2(10) ? C10' C11' N4' C7' . . . . 1.0(18) ? N4' C7' C8' C9' . . . . 1.8(12) ?