#------------------------------------------------------------------------------ #$Date: 2016-03-26 13:02:54 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180220 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/06/7110619.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided the Crystal Eye server at # http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the # Peter Murray-Rust laboratory. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_7110619 loop_ _publ_author_name 'Albert Cotton, F.' 'Murillo, Carlos A.' 'Timmons, Daren J.' 'Murillo, Carlos A.' _publ_section_title ; First paddlewheel complex with a doubly-bonded Ir26+ core ; _journal_issue 15 _journal_name_full 'Chemical Communications' _journal_page_first 1427 _journal_paper_doi 10.1039/a904698d _journal_year 1999 _chemical_compound_source synthesis _chemical_formula_sum 'C28 H48 Cl2 Ir2 N12' _chemical_formula_weight 1008.08 _space_group_IT_number 85 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4a' _symmetry_space_group_name_H-M 'P 4/n :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.966(3) _cell_length_b 9.966(3) _cell_length_c 15.907(6) _cell_measurement_reflns_used 149 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 20.8 _cell_measurement_theta_min 6.75 _cell_volume 1579.9(9) _computing_cell_refinement MADNES _computing_data_collection MADNES _computing_data_reduction PROCOR _computing_molecular_graphics 'XP (Siemens, 1996)' _computing_publication_material 'CIFTAB (SHELDRICK, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 213(2) _diffrn_measurement_device 'Nonius FAST' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5971 _diffrn_reflns_theta_max 22.50 _diffrn_reflns_theta_min 2.41 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 'None (area detector data)' _exptl_absorpt_coefficient_mu 8.627 _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour purple _exptl_crystal_density_diffrn 2.119 _exptl_crystal_density_meas ? _exptl_crystal_description plate _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.781 _refine_diff_density_min -1.535 _refine_diff_density_rms 0.167 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.150 _refine_ls_goodness_of_fit_obs 1.156 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 103 _refine_ls_number_reflns 1036 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.190 _refine_ls_restrained_S_obs 1.156 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_obs 0.0384 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+19.3866P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0931 _refine_ls_wR_factor_obs 0.0803 _reflns_number_observed 843 _reflns_number_total 1041 _reflns_observed_criterion >2sigma(I) _cod_data_source_file 904698dsup1.cif _cod_data_source_block 04698D _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (5 times). '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (9 times). Automatic conversion script Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+19.3866P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+19.3866P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1579.8(9) _cod_original_sg_symbol_H-M P4/n _cod_database_code 7110619 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0171(4) 0.0171(4) 0.0163(4) 0.000 0.000 0.000 Cl1 0.027(2) 0.027(2) 0.017(2) 0.000 0.000 0.000 Ir2 0.0178(4) 0.0178(4) 0.0153(4) 0.000 0.000 0.000 Cl2 0.026(2) 0.026(2) 0.023(2) 0.000 0.000 0.000 N11 0.036(6) 0.018(5) 0.022(4) -0.004(3) -0.005(4) 0.008(4) N12 0.035(6) 0.021(5) 0.024(5) 0.011(4) 0.006(4) 0.014(4) N13 0.033(5) 0.018(5) 0.030(5) 0.001(4) -0.002(4) 0.013(4) C11 0.049(8) 0.042(8) 0.028(6) -0.015(5) -0.010(5) 0.013(6) C12 0.065(10) 0.038(8) 0.031(6) -0.009(5) 0.005(6) 0.031(7) C13 0.041(8) 0.038(8) 0.041(7) -0.008(5) 0.003(5) 0.016(6) C14 0.055(9) 0.020(7) 0.035(6) 0.001(4) -0.007(5) 0.015(6) C15 0.049(8) 0.032(7) 0.029(5) 0.009(5) -0.004(5) 0.008(6) C16 0.048(8) 0.037(8) 0.025(5) 0.009(5) -0.010(5) -0.001(6) C17 0.019(5) 0.014(5) 0.021(5) 0.001(4) -0.004(4) -0.004(4) loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags Ir1 Ir 0.2500 0.2500 0.17586(4) 0.0168(3) Uani 1 d S Cl1 Cl 0.2500 0.2500 0.0114(3) 0.0239(11) Uani 1 d S Ir2 Ir 0.2500 0.2500 0.33271(4) 0.0169(3) Uani 1 d S Cl2 Cl 0.2500 0.2500 0.5005(3) 0.0248(11) Uani 1 d S N11 N 0.3191(9) 0.0611(9) 0.1836(4) 0.025(2) Uani 1 d . N12 N 0.3548(9) 0.0773(9) 0.3270(4) 0.027(2) Uani 1 d . N13 N 0.4329(9) -0.1122(8) 0.2525(5) 0.027(2) Uani 1 d . C11 C 0.3157(12) -0.0320(13) 0.1120(6) 0.040(3) Uani 1 d . H11A H 0.2895(12) 0.0166(13) 0.0610(6) 0.048 Uiso 1 calc R H11B H 0.2489(12) -0.1022(13) 0.1223(6) 0.048 Uiso 1 calc R C12 C 0.4498(14) -0.0940(13) 0.0996(7) 0.045(3) Uani 1 d . H12A H 0.5180(14) -0.0242(13) 0.0918(7) 0.053 Uiso 1 calc R H12B H 0.4492(14) -0.1516(13) 0.0497(7) 0.053 Uiso 1 calc R C13 C 0.4809(14) -0.1751(13) 0.1761(6) 0.040(3) Uani 1 d . H13A H 0.4395(14) -0.2638(13) 0.1705(6) 0.048 Uiso 1 calc R H13B H 0.5782(14) -0.1877(13) 0.1801(6) 0.048 Uiso 1 calc R C14 C 0.4568(14) -0.1925(12) 0.3280(6) 0.037(3) Uani 1 d . H14A H 0.5535(14) -0.2048(12) 0.3358(6) 0.044 Uiso 1 calc R H14B H 0.4160(14) -0.2813(12) 0.3209(6) 0.044 Uiso 1 calc R C15 C 0.3984(13) -0.1256(12) 0.4048(6) 0.037(3) Uani 1 d . H15A H 0.3013(13) -0.1406(12) 0.4071(6) 0.044 Uiso 1 calc R H15B H 0.4388(13) -0.1631(12) 0.4558(6) 0.044 Uiso 1 calc R C16 C 0.4273(13) 0.0193(12) 0.3991(6) 0.037(3) Uani 1 d . H16A H 0.3992(13) 0.0640(12) 0.4510(6) 0.044 Uiso 1 calc R H16B H 0.5240(13) 0.0333(12) 0.3920(6) 0.044 Uiso 1 calc R C17 C 0.3686(9) 0.0094(9) 0.2542(5) 0.018(2) Uani 1 d . 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ir1 N11 89.78(2) 4 . y N11 Ir1 N11 89.78(3) 4 2 ? N11 Ir1 N11 173.0(4) . 2 y N11 Ir1 N11 173.0(4) 4 3 ? N11 Ir1 N11 89.78(3) . 3 ? N11 Ir1 N11 89.78(3) 2 3 ? N11 Ir1 Ir2 86.5(2) 4 . y N11 Ir1 Ir2 86.5(2) . . ? N11 Ir1 Ir2 86.5(2) 2 . ? N11 Ir1 Ir2 86.5(2) 3 . ? N11 Ir1 Cl1 93.5(2) 4 . y N11 Ir1 Cl1 93.5(2) . . ? N11 Ir1 Cl1 93.5(2) 2 . ? N11 Ir1 Cl1 93.5(2) 3 . ? Ir2 Ir1 Cl1 180.0 . . ? N12 Ir2 N12 89.89(2) 2 3 y N12 Ir2 N12 89.89(2) 2 4 ? N12 Ir2 N12 174.9(4) 3 4 y N12 Ir2 N12 174.9(4) 2 . ? N12 Ir2 N12 89.89(2) 3 . ? N12 Ir2 N12 89.88(2) 4 . ? N12 Ir2 Ir1 87.4(2) 2 . y N12 Ir2 Ir1 87.4(2) 3 . ? N12 Ir2 Ir1 87.4(2) 4 . ? N12 Ir2 Ir1 87.4(2) . . ? N12 Ir2 Cl2 92.6(2) 2 . y N12 Ir2 Cl2 92.6(2) 3 . ? N12 Ir2 Cl2 92.6(2) 4 . ? N12 Ir2 Cl2 92.6(2) . . ? Ir1 Ir2 Cl2 180.0 . . ? C17 N11 C11 114.7(9) . . ? C17 N11 Ir1 122.8(6) . . ? C11 N11 Ir1 122.4(6) . . ? C17 N12 C16 114.9(9) . . ? C17 N12 Ir2 121.3(6) . . ? C16 N12 Ir2 123.7(7) . . ? C17 N13 C13 123.6(8) . . ? C17 N13 C14 122.9(8) . . ? C13 N13 C14 113.5(8) . . ? N11 C11 C12 110.2(9) . . ? C11 C12 C13 107.7(10) . . ? N13 C13 C12 112.4(10) . . ? N13 C14 C15 111.1(10) . . ? C16 C15 C14 107.9(10) . . ? N12 C16 C15 109.6(10) . . ? N11 C17 N12 119.5(9) . . y N11 C17 N13 119.9(8) . . ? N12 C17 N13 120.5(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 Ir2 2.4950(13) . y Ir1 Cl1 2.617(4) . y Ir1 N11 2.008(9) 4 y Ir1 N11 2.008(9) . ? Ir1 N11 2.008(9) 2 ? Ir1 N11 2.008(9) 3 ? Ir2 N12 2.016(9) 2 ? Ir2 N12 2.016(9) 3 ? Ir2 N12 2.016(9) 4 ? Ir2 Cl2 2.670(5) . y Ir2 N12 2.016(9) . y N11 C17 1.331(11) . ? N11 C11 1.470(12) . ? N12 C17 1.348(11) . ? N12 C16 1.473(12) . ? N13 C17 1.370(13) . ? N13 C13 1.450(12) . ? N13 C14 1.463(12) . ? C11 C12 1.49(2) . ? C12 C13 1.49(2) . ? C14 C15 1.508(15) . ? C15 C16 1.48(2) . ?