#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/86/2018637.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # 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_2018637 loop_ _publ_author_name 'Babaryk, Artem A.' 'Kozachkova, Alexandra N.' 'Tsaryk, Natalia V.' 'Dudko, Anatolij V.' 'Pekhnyo, Vasily I.' _publ_section_title ; Binary salt of a palladium(II) complex with (phosphonomethyl)phosphonic (medronic) acid comprising `handbell-like' [Pd{\m-CH~2~(PO~3~)~2~}]~3~ units ; _journal_coeditor_code KU3068 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m242 _journal_page_last m245 _journal_volume 68 _journal_year 2012 _chemical_formula_iupac 'K2 [Ni (H2 O)6]2 [Pd3 (C H2 O6 P2)3] , 6H2 O' _chemical_formula_moiety 'C3 H33 K2 Ni2 O30 P6 Pd3, 6(H2 O)' _chemical_formula_sum 'C3 H42 K2 Ni2 O36 P6 Pd3' _chemical_formula_weight 1354.02 _chemical_name_systematic ; dipotassium bis[hexaaquanickel(II)] tris(\m~2~-methylenediphosphonato)tripalladium(II) hexahydrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 128.934(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 23.6234(11) _cell_length_b 12.5467(6) _cell_length_c 16.0458(7) _cell_measurement_reflns_used 8292 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 4.43 _cell_measurement_theta_min 2.22 _cell_volume 3699.5(3) _computing_cell_refinement 'SAINT-Plus (Bruker, 2007)' _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_data_reduction ; SAINT-Plus (Bruker, 2007) and XPREP (Bruker, 2001) ; _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'DIRDIF (Beurskens et al., 1999)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEXII CCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3231 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 1.97 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.028 _exptl_absorpt_correction_T_max 0.513808 _exptl_absorpt_correction_T_min 0.401868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(TWINABS; Bruker, 2001)' _exptl_crystal_colour 'translucent brown' _exptl_crystal_density_diffrn 2.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2636 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.637 _refine_diff_density_min -0.725 _refine_ls_extinction_coef 0.00016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 2008)' _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 302 _refine_ls_number_reflns 3231 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0218 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0215P)^2^+12.6038P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.0521 _reflns_number_gt 3019 _reflns_number_total 3231 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL twin4 CELL 0.71073 23.6234 12.5467 16.0458 90.000 128.934 90.000 ZERR 4.00 0.0011 0.0006 0.0007 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.680 12.010 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.624 0.350 1.000 SFAC K 8.21861 12.79491 7.43981 0.77480 1.05190 213.18719 = 0.86590 41.68416 1.42280 0.201 0.249 1050.000 1.330 39.100 SFAC NI 12.83761 3.87850 7.29201 0.25650 4.44380 12.17631 = 2.38000 66.34216 1.03410 0.339 1.112 4570.000 1.500 58.690 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 = 0.86700 32.90894 0.25080 0.011 0.006 32.500 0.680 16.000 SFAC P 6.43451 1.90670 4.17910 27.15704 1.78000 0.52600 = 1.49080 68.16457 1.11490 0.102 0.094 410.000 1.050 30.970 SFAC PD 19.33192 0.69866 15.50172 7.98930 5.29537 25.20523 = 0.60584 76.89868 5.26593 -0.999 1.007 4360.000 1.500 106.400 UNIT 12 124 8 8 144 24 12 MERG 0 SADI 0.02 P1 O15 P1 O16 SADI 0.02 H5 H6 H7 H8 H9 H10 H11 H12 H13 H14 H15 H16 H181 H182 SADI 0.02 O9 H5 O9 H6 SADI 0.02 O10 H7 O10 H8 SADI 0.02 O11 H9 O11 H10 SADI 0.02 O12 H11 O12 H12 SADI 0.02 O13 H13 O13 H14 SADI 0.02 O14 H15 O14 H16 SADI 0.02 O21 H181 O21 H182 SADI 0.02 O17 H171 O18 H172 O20 H192 EADP O15 O16 EADP O17 O18 EADP O19 O20 EADP O21 O22 EQIV $1 X, -Y, Z-1/2 EQIV $2 -X+1/2, -Y+1/2, -Z EQIV $3 -X+1/2, -Y+1/2, -Z+1 EQIV $4 -X+1/2, Y-1/2, -Z+1/2 EQIV $5 -X+1/2, Y+1/2, -Z+1/2 EQIV $6 -X, -Y, -Z EQIV $7 X-1/2, Y-1/2, Z-1 EQIV $8 1-X, -Y, 2-Z BIND PD1 H1_$8 HTAB O21 O8_$1 HTAB O21 O14_$2 HTAB O17 O3_$3 HTAB O9 O6_$1 HTAB O9 O4_$1 HTAB O9 O15 HTAB O9 O16 HTAB O10 O16_$4 HTAB O10 O15_$4 HTAB O10 O5_$1 HTAB O11 O4_$1 HTAB O12 O8_$5 HTAB O11 O17_$1 HTAB O11 O18_$1 HTAB O12 O8_$1 HTAB O13 O5_$3 HTAB O13 O21_$4 HTAB O13 O22_$4 HTAB O13 O18 HTAB O14 O20_$6 HTAB O14 O19_$6 HTAB O14 O2_$7 RTAB PD1 H1_$8 RTAB PD1 H1_$8 C1_$8 ACTA FMAP 2 PLAN -10 SIZE 0.20 0.20 0.40 BOND $H CONF LIST 7 L.S. 50 TEMP -173.00 WGHT 0.021500 12.603806 EXTI 0.000157 BASF 0.10142 FVAR 0.16184 0.51798 0.74430 0.72281 0.72276 PD2 7 0.500000 0.284300 0.750000 10.50000 0.00899 0.00923 = 0.00764 0.00000 0.00528 0.00000 PD1 7 0.508025 -0.014356 0.851937 11.00000 0.00893 0.00943 = 0.00761 -0.00151 0.00400 -0.00204 NI1 4 0.227707 0.030177 0.125245 11.00000 0.00977 0.00942 = 0.01213 -0.00160 0.00480 -0.00125 K1 3 0.302531 -0.063387 0.407200 11.00000 0.01444 0.03415 = 0.01244 0.00348 0.00612 -0.00202 P3 6 0.419629 -0.192208 0.682604 11.00000 0.00849 0.00985 = 0.00989 -0.00235 0.00430 -0.00087 P2 6 0.425875 0.197951 0.836980 11.00000 0.01868 0.01025 = 0.01761 -0.00370 0.01448 -0.00352 P1 6 0.589072 0.199647 0.980783 11.00000 0.01882 0.01257 = 0.00880 -0.00062 0.00315 -0.00730 O6 5 0.428513 -0.122425 0.769312 11.00000 0.00889 0.01248 = 0.01287 -0.00484 0.00605 -0.00339 O2 5 0.582578 0.287508 0.907969 11.00000 0.01372 0.01240 = 0.00771 0.00038 0.00371 -0.00385 O7 5 0.415631 -0.126357 0.598235 11.00000 0.01250 0.01092 = 0.01037 -0.00070 0.00522 -0.00051 O4 5 0.426498 0.089373 0.793757 11.00000 0.01227 0.01069 = 0.01376 -0.00257 0.00622 -0.00016 O1 5 0.590514 0.087425 0.945551 11.00000 0.01246 0.01136 = 0.01806 0.00109 -0.00036 -0.00324 O11 5 0.290788 -0.020996 0.084150 11.00000 0.01187 0.01930 = 0.02030 -0.00890 0.00681 -0.00284 H9 2 0.329701 -0.038741 0.129097 11.00000 -1.50000 H10 2 0.271338 -0.064713 0.042024 11.00000 -1.50000 O8 5 0.353014 -0.261425 0.630544 11.00000 0.01027 0.01197 = 0.01273 -0.00289 0.00513 -0.00054 O3 5 0.425567 0.290221 0.772462 11.00000 0.01905 0.01307 = 0.02289 0.00077 0.01717 0.00017 O5 5 0.361056 0.209304 0.833713 11.00000 0.02799 0.01351 = 0.03727 -0.00707 0.02851 -0.00551 O9 5 0.320238 0.066657 0.275356 11.00000 0.01287 0.01332 = 0.01635 -0.00379 0.01007 -0.00143 H5 2 0.351697 0.075114 0.275895 11.00000 -1.50000 H6 2 0.315699 0.113743 0.299329 11.00000 -1.50000 O13 5 0.162631 0.082568 0.158248 11.00000 0.02654 0.01240 = 0.02885 0.00115 0.02176 -0.00090 H13 2 0.157049 0.140371 0.156811 11.00000 -1.50000 H14 2 0.161205 0.053090 0.195946 11.00000 -1.50000 O12 5 0.225664 0.183053 0.076993 11.00000 0.00833 0.01617 = 0.01174 0.00071 0.00374 0.00065 H11 2 0.198861 0.191023 0.018013 11.00000 -1.50000 H12 2 0.263500 0.198023 0.097151 11.00000 -1.50000 O14 5 0.135783 -0.012021 -0.027800 11.00000 0.01160 0.01096 = 0.01900 -0.00139 0.00746 -0.00382 H15 2 0.099246 0.007070 -0.038521 11.00000 -1.50000 H16 2 0.127673 -0.074393 -0.040139 11.00000 -1.50000 O10 5 0.234562 -0.112804 0.190984 11.00000 0.01643 0.01411 = 0.02765 0.00068 0.00018 -0.00656 H7 2 0.206419 -0.155290 0.155192 11.00000 -1.50000 H8 2 0.272167 -0.139478 0.224956 11.00000 -1.50000 C1 1 0.509476 0.209631 0.972242 11.00000 0.03445 0.01559 = 0.01660 -0.00557 0.02017 -0.00914 AFIX 23 H1 2 0.511185 0.152811 1.016589 11.00000 -1.20000 H2 2 0.510118 0.279128 1.002046 11.00000 -1.20000 AFIX 0 C2 1 0.500000 -0.273809 0.750000 10.50000 0.00853 0.01069 = 0.01086 0.00000 0.00655 0.00000 AFIX 23 H3 2 0.503288 -0.320150 0.802837 10.50000 -1.20000 H4 2 0.496713 -0.320142 0.697159 10.50000 -1.20000 AFIX 0 PART 1 O15 5 0.661997 0.214867 1.092703 51.00000 0.00751 0.01021 = 0.01045 -0.00272 0.00514 -0.00061 PART 2 O16 5 0.642284 0.234707 1.098467 -51.00000 0.00751 0.01021 = 0.01045 -0.00272 0.00514 -0.00061 PART 1 O17 5 0.225592 0.167330 0.420572 41.00000 0.01739 0.02999 = 0.02429 0.01486 0.01176 0.00686 H171 2 0.196913 0.177973 0.386726 41.00000 -1.50000 PART -1 O18 5 0.222200 0.117659 0.393111 -41.00000 0.01739 0.02999 = 0.02429 0.01486 0.01176 0.00686 PART 1 O19 5 0.009391 0.007722 0.101655 21.00000 0.01454 0.02613 = 0.01658 -0.00301 0.00760 -0.00350 PART -1 O20 5 -0.006801 -0.045886 0.076722 -21.00000 0.01454 0.02613 = 0.01658 -0.00301 0.00760 -0.00350 H192 2 0.018340 -0.020844 0.104874 -21.00000 -1.50000 PART 1 O21 5 0.356058 0.459096 0.206933 31.00000 0.03319 0.01233 = 0.02276 0.00106 0.02050 0.00030 H181 2 0.359101 0.398339 0.199098 31.00000 -1.50000 H182 2 0.360565 0.487540 0.168340 31.00000 -1.50000 PART 2 O22 5 0.362662 0.385944 0.269679 -31.00000 0.03319 0.01233 = 0.02276 0.00106 0.02050 0.00030 PART 0 HKLF 5 REM twin4 REM R1 = 0.0218 for 3019 Fo > 4sig(Fo) and 0.0243 for all 3231 data REM 302 parameters refined using 30 restraints END WGHT 0.0209 12.3354 REM Highest difference peak 0.637, deepest hole -0.725, 1-sigma level 0.093 Q1 1 0.5484 0.2056 0.9675 11.00000 0.05 0.64 Q2 1 0.2481 0.1792 0.3906 11.00000 0.05 0.50 Q3 1 0.0470 -0.0325 0.1512 11.00000 0.05 0.47 Q4 1 0.2447 -0.1260 0.1475 11.00000 0.05 0.47 Q5 1 0.3250 0.2146 0.7776 11.00000 0.05 0.46 Q6 1 0.4588 0.0035 0.7889 11.00000 0.05 0.45 Q7 1 0.2928 -0.0027 0.3996 11.00000 0.05 0.44 Q8 1 0.4509 -0.0158 0.8341 11.00000 0.05 0.43 Q9 1 0.4668 -0.2373 0.7366 11.00000 0.05 0.42 Q10 1 0.4533 0.2741 0.7060 11.00000 0.05 0.40 ; _[local]_cod_data_source_file ku3068.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2018637 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd2 0.5000 0.28430(3) 0.7500 0.00858(10) Uani d S 1 2 . . Pd Pd1 0.508025(13) -0.014356(19) 0.85194(2) 0.00949(8) Uani d . 1 1 . . Ni Ni1 0.22771(2) 0.03018(3) 0.12525(3) 0.01188(11) Uani d . 1 1 . . K K1 0.30253(4) -0.06339(7) 0.40720(6) 0.02195(19) Uani d . 1 1 . . P P3 0.41963(4) -0.19221(7) 0.68260(7) 0.01043(18) Uani d . 1 1 . . P P2 0.42588(5) 0.19795(7) 0.83698(7) 0.01338(19) Uani d . 1 1 . . P P1 0.58907(5) 0.19965(7) 0.98078(7) 0.0172(2) Uani d D 1 1 . . O O6 0.42851(11) -0.12243(17) 0.76931(17) 0.0120(5) Uani d . 1 1 . . O O2 0.58258(12) 0.28751(17) 0.90797(17) 0.0134(5) Uani d . 1 1 A . O O7 0.41563(12) -0.12636(17) 0.59824(17) 0.0126(5) Uani d . 1 1 . . O O4 0.42650(12) 0.08937(18) 0.79376(18) 0.0136(5) Uani d . 1 1 . . O O1 0.59051(12) 0.08742(18) 0.94555(19) 0.0209(6) Uani d . 1 1 A . O O11 0.29079(13) -0.02100(19) 0.0841(2) 0.0194(6) Uani d D 1 1 . . H H9 0.3297(13) -0.039(3) 0.129(2) 0.029 Uiso d D 1 1 . . H H10 0.2713(18) -0.065(3) 0.042(2) 0.029 Uiso d D 1 1 . . O O8 0.35301(11) -0.26142(18) 0.63054(17) 0.0131(5) Uani d . 1 1 . . O O3 0.42557(12) 0.29022(18) 0.77246(19) 0.0156(5) Uani d . 1 1 . . O O5 0.36106(14) 0.20930(18) 0.8337(2) 0.0207(6) Uani d . 1 1 . . O O9 0.32024(12) 0.06666(19) 0.27536(19) 0.0136(5) Uani d D 1 1 . . H H5 0.3517(17) 0.075(3) 0.276(3) 0.020 Uiso d D 1 1 . . H H6 0.316(2) 0.114(3) 0.299(3) 0.020 Uiso d D 1 1 . . O O13 0.16263(15) 0.0826(2) 0.1582(2) 0.0196(6) Uani d D 1 1 . . H H13 0.157(2) 0.1404(17) 0.157(3) 0.029 Uiso d D 1 1 . . H H14 0.161(2) 0.053(3) 0.196(3) 0.029 Uiso d D 1 1 . . O O12 0.22566(13) 0.18305(19) 0.07699(19) 0.0139(5) Uani d D 1 1 . . H H11 0.1989(15) 0.191(3) 0.0180(18) 0.021 Uiso d D 1 1 . . H H12 0.2635(11) 0.198(3) 0.097(3) 0.021 Uiso d D 1 1 . . O O14 0.13578(13) -0.01202(19) -0.0278(2) 0.0153(5) Uani d D 1 1 . . H H15 0.0992(18) 0.007(3) -0.039(3) 0.023 Uiso d D 1 1 . . H H16 0.128(2) -0.0744(18) -0.040(3) 0.023 Uiso d D 1 1 . . O O10 0.23456(14) -0.1128(2) 0.1910(2) 0.0289(7) Uani d D 1 1 . . H H7 0.2064(16) -0.155(3) 0.155(3) 0.043 Uiso d D 1 1 . . H H8 0.2722(13) -0.139(4) 0.225(3) 0.043 Uiso d D 1 1 . . C C1 0.5095(2) 0.2096(3) 0.9722(3) 0.0194(8) Uani d . 1 1 A . H H1 0.5112 0.1528 1.0166 0.023 Uiso calc R 1 1 . . H H2 0.5101 0.2791 1.0020 0.023 Uiso calc R 1 1 . . C C2 0.5000 -0.2738(3) 0.7500 0.0097(9) Uani d S 1 2 . . H H3 0.5033 -0.3202 0.8028 0.012 Uiso calc PR 0.50 1 . . H H4 0.4967 -0.3201 0.6972 0.012 Uiso calc PR 0.50 1 . . O O15 0.6620(3) 0.2149(4) 1.0927(3) 0.0097(10) Uani d PD 0.723(12) 1 A 1 O O16 0.6423(7) 0.2347(10) 1.0985(8) 0.0097(10) Uani d PD 0.277(12) 1 A 2 O O17 0.2256(2) 0.1673(5) 0.4206(4) 0.0248(13) Uani d PD 0.723(10) 1 B 1 H H171 0.197(4) 0.178(6) 0.387(6) 0.037 Uiso d PD 0.723(10) 1 B 1 O O18 0.2222(7) 0.1177(13) 0.3931(11) 0.0248(13) Uani d P 0.277(10) 1 B -1 O O19 0.0094(3) 0.0077(5) 0.1017(6) 0.0206(11) Uani d P 0.518(7) 1 C 1 O O20 -0.0068(4) -0.0459(6) 0.0767(5) 0.0206(11) Uani d PD 0.482(7) 1 C -1 H H192 0.018(5) -0.021(10) 0.105(10) 0.031 Uiso d PD 0.482(7) 1 C -1 O O21 0.3561(2) 0.4591(3) 0.2069(3) 0.0207(8) Uani d PD 0.744(4) 1 D 1 H H181 0.359(3) 0.398(2) 0.199(5) 0.031 Uiso d PD 0.744(4) 1 D 1 H H182 0.361(3) 0.488(4) 0.168(4) 0.031 Uiso d PD 0.744(4) 1 D 1 O O22 0.3627(5) 0.3859(7) 0.2697(8) 0.0207(8) Uani d P 0.256(4) 1 D 2 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 Pd2 0.00899(18) 0.00923(19) 0.00764(18) 0.000 0.00528(16) 0.000 Pd1 0.00893(14) 0.00943(14) 0.00761(14) -0.00204(10) 0.00400(12) -0.00151(10) Ni1 0.0098(2) 0.0094(2) 0.0121(2) -0.00125(17) 0.0048(2) -0.00160(17) K1 0.0144(4) 0.0341(5) 0.0124(4) -0.0020(3) 0.0061(3) 0.0035(4) P3 0.0085(4) 0.0098(4) 0.0099(4) -0.0009(3) 0.0043(4) -0.0024(3) P2 0.0187(5) 0.0103(4) 0.0176(5) -0.0035(4) 0.0145(4) -0.0037(4) P1 0.0188(5) 0.0126(5) 0.0088(4) -0.0073(4) 0.0032(4) -0.0006(4) O6 0.0089(11) 0.0125(12) 0.0129(12) -0.0034(9) 0.0061(10) -0.0048(10) O2 0.0137(12) 0.0124(12) 0.0077(12) -0.0039(9) 0.0037(10) 0.0004(9) O7 0.0125(12) 0.0109(12) 0.0104(11) -0.0005(9) 0.0052(10) -0.0007(9) O4 0.0123(12) 0.0107(12) 0.0138(12) -0.0002(9) 0.0062(10) -0.0026(10) O1 0.0125(12) 0.0114(13) 0.0181(13) -0.0032(10) -0.0004(11) 0.0011(10) O11 0.0119(13) 0.0193(14) 0.0203(15) -0.0028(11) 0.0068(12) -0.0089(11) O8 0.0103(12) 0.0120(12) 0.0127(12) -0.0005(9) 0.0051(10) -0.0029(10) O3 0.0190(13) 0.0131(12) 0.0229(13) 0.0002(10) 0.0172(12) 0.0008(10) O5 0.0280(14) 0.0135(13) 0.0373(16) -0.0055(11) 0.0285(14) -0.0071(11) O9 0.0129(13) 0.0133(13) 0.0163(13) -0.0014(10) 0.0101(12) -0.0038(10) O13 0.0265(14) 0.0124(13) 0.0289(16) -0.0009(12) 0.0218(13) 0.0011(12) O12 0.0083(12) 0.0162(13) 0.0117(12) 0.0007(10) 0.0037(11) 0.0007(11) O14 0.0116(13) 0.0110(12) 0.0190(14) -0.0038(10) 0.0075(12) -0.0014(11) O10 0.0164(14) 0.0141(15) 0.0277(16) -0.0066(11) 0.0002(13) 0.0007(12) C1 0.034(2) 0.0156(18) 0.0166(19) -0.0091(16) 0.0202(18) -0.0056(15) C2 0.009(2) 0.011(2) 0.011(2) 0.000 0.007(2) 0.000 O15 0.008(2) 0.0102(19) 0.0105(14) -0.0006(16) 0.0051(15) -0.0027(12) O16 0.008(2) 0.0102(19) 0.0105(14) -0.0006(16) 0.0051(15) -0.0027(12) O17 0.0174(18) 0.030(3) 0.024(3) 0.007(2) 0.012(2) 0.015(2) O18 0.0174(18) 0.030(3) 0.024(3) 0.007(2) 0.012(2) 0.015(2) O19 0.015(3) 0.026(3) 0.017(3) -0.004(2) 0.008(2) -0.003(2) O20 0.015(3) 0.026(3) 0.017(3) -0.004(2) 0.008(2) -0.003(2) O21 0.0332(19) 0.0123(16) 0.0228(19) 0.0003(15) 0.0205(17) 0.0011(14) O22 0.0332(19) 0.0123(16) 0.0228(19) 0.0003(15) 0.0205(17) 0.0011(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9990 1.0070 '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 O2 Pd2 O2 2_656 . 177.70(13) n O2 Pd2 O3 2_656 2_656 92.21(9) n O2 Pd2 O3 . 2_656 87.71(9) n O2 Pd2 O3 2_656 . 87.71(9) n O2 Pd2 O3 . . 92.20(9) n O3 Pd2 O3 2_656 . 175.75(13) n O2 Pd2 P2 2_656 2_656 79.08(7) y O2 Pd2 P2 . 2_656 101.77(7) y O3 Pd2 P2 2_656 2_656 26.97(7) y O3 Pd2 P2 . 2_656 156.59(7) y O2 Pd2 P2 2_656 . 101.76(7) y O2 Pd2 P2 . . 79.07(7) y O3 Pd2 P2 2_656 . 156.59(7) y O3 Pd2 P2 . . 26.96(7) y P2 Pd2 P2 2_656 . 138.29(3) y O6 Pd1 O1 . . 175.32(9) n O6 Pd1 O4 . . 84.50(9) n O1 Pd1 O4 . . 97.63(9) n O6 Pd1 O7 . 2_656 91.36(9) n O1 Pd1 O7 . 2_656 86.60(9) n O4 Pd1 O7 . 2_656 175.67(9) n O6 Pd1 H1 . 5_657 64.9 n O1 Pd1 H1 . 5_657 110.5 n O4 Pd1 H1 . 5_657 100.3 n O7 Pd1 H1 2_656 5_657 79.0 n O6 Pd1 Pd1 . 2_656 81.77(6) n O1 Pd1 Pd1 . 2_656 102.20(7) n O4 Pd1 Pd1 . 2_656 93.73(6) n O7 Pd1 Pd1 2_656 2_656 84.40(6) n H1 Pd1 Pd1 5_657 2_656 142.0 n O13 Ni1 O10 . . 88.67(11) n O13 Ni1 O9 . . 92.56(10) n O10 Ni1 O9 . . 84.76(10) n O13 Ni1 O12 . . 87.34(10) n O10 Ni1 O12 . . 172.78(11) n O9 Ni1 O12 . . 89.40(10) n O13 Ni1 O11 . . 177.32(11) n O10 Ni1 O11 . . 93.03(12) n O9 Ni1 O11 . . 89.66(10) n O12 Ni1 O11 . . 91.18(10) n O13 Ni1 O14 . . 89.45(10) n O10 Ni1 O14 . . 94.10(10) n O9 Ni1 O14 . . 177.67(10) n O12 Ni1 O14 . . 91.88(9) n O11 Ni1 O14 . . 88.36(10) n O8 P3 O7 . . 110.87(13) y O8 P3 O6 . . 109.24(12) y O7 P3 O6 . . 112.80(13) y O8 P3 C2 . . 110.15(15) y O7 P3 C2 . . 107.01(11) y O6 P3 C2 . . 106.65(11) y O5 P2 O4 . . 111.53(13) y O5 P2 O3 . . 109.16(14) y O4 P2 O3 . . 111.03(13) y O5 P2 C1 . . 110.81(16) y O4 P2 C1 . . 107.60(15) y O3 P2 C1 . . 106.58(15) y O5 P2 Pd2 . . 144.70(11) n O4 P2 Pd2 . . 86.39(9) n C1 P2 Pd2 . . 90.71(11) n O1 P1 O15 . . 106.2(2) y O1 P1 O16 . . 121.9(5) y O1 P1 O2 . . 113.19(14) y O15 P1 O2 . . 107.61(18) y O16 P1 O2 . . 110.0(5) y O1 P1 C1 . . 107.53(15) y O15 P1 C1 . . 115.6(3) y O16 P1 C1 . . 94.7(5) y O2 P1 C1 . . 106.89(15) y P3 O6 Pd1 . . 121.46(13) y P1 O2 Pd2 . . 119.87(13) y P3 O7 Pd1 . 2_656 118.77(13) y P2 O4 Pd1 . . 130.25(13) y P1 O1 Pd1 . . 128.98(14) y Ni1 O11 H9 . . 118(3) n Ni1 O11 H10 . . 111(3) n H9 O11 H10 . . 109(4) n P2 O3 Pd2 . . 117.10(13) y Ni1 O9 H5 . . 111(3) n Ni1 O9 H6 . . 113(3) n H5 O9 H6 . . 110(4) n Ni1 O13 H13 . . 118(3) n Ni1 O13 H14 . . 119(3) n H13 O13 H14 . . 115(4) n Ni1 O12 H11 . . 114(3) n Ni1 O12 H12 . . 109(3) n H11 O12 H12 . . 110(4) n Ni1 O14 H15 . . 111(3) n Ni1 O14 H16 . . 117(3) n H15 O14 H16 . . 100(3) n Ni1 O10 H7 . . 119(4) n Ni1 O10 H8 . . 116(4) n H7 O10 H8 . . 108(4) n P2 C1 P1 . . 112.80(18) y P2 C1 H1 . . 109.0 n P1 C1 H1 . . 109.0 n P2 C1 H2 . . 109.0 n P1 C1 H2 . . 109.0 n H1 C1 H2 . . 107.8 n P3 C2 P3 2_656 . 110.7(2) y P3 C2 H3 2_656 . 109.5 n P3 C2 H3 . . 109.5 n P3 C2 H4 2_656 . 109.5 n P3 C2 H4 . . 109.5 n H3 C2 H4 . . 108.1 n O18 O17 H171 . . 91(9) n O20 O19 H192 . . 47(10) n H181 O21 H182 . . 104(5) n 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 Pd2 O2 2_656 2.004(2) n Pd2 O2 . 2.004(2) y Pd2 O3 2_656 2.006(2) n Pd2 O3 . 2.006(2) y Pd2 P2 2_656 3.0429(9) n Pd2 P2 . 3.0429(9) n Pd1 O6 . 1.999(2) y Pd1 O1 . 2.001(2) y Pd1 O4 . 2.004(2) y Pd1 O7 2_656 2.013(2) y Pd1 H1 5_657 2.9795 ? Pd1 Pd1 2_656 3.0473(5) y Ni1 O13 . 2.025(2) n Ni1 O10 . 2.035(3) n Ni1 O9 . 2.043(2) n Ni1 O12 . 2.058(2) n Ni1 O11 . 2.074(3) n Ni1 O14 . 2.079(2) n P3 O8 . 1.509(2) y P3 O7 . 1.537(2) y P3 O6 . 1.543(2) y P3 C2 . 1.801(3) y P2 O5 . 1.506(2) y P2 O4 . 1.533(2) y P2 O3 . 1.550(2) y P2 C1 . 1.801(4) y P1 O1 . 1.526(3) y P1 O15 . 1.530(4) y P1 O16 . 1.535(10) n P1 O2 . 1.542(2) y P1 C1 . 1.802(4) y O7 Pd1 2_656 2.013(2) n O11 H9 . 0.76(2) n O11 H10 . 0.76(2) n O9 H5 . 0.75(2) n O9 H6 . 0.75(2) n O13 H13 . 0.73(2) n O13 H14 . 0.73(2) n O12 H11 . 0.74(2) n O12 H12 . 0.76(2) n O14 H15 . 0.80(2) n O14 H16 . 0.80(2) n O10 H7 . 0.76(2) n O10 H8 . 0.77(2) n C1 H1 . 0.9900 n C1 H2 . 0.9900 n C2 P3 2_656 1.800(3) n C2 H3 . 0.9900 n C2 H4 . 0.9900 n O17 O18 . 0.738(13) n O17 H171 . 0.56(6) n O18 H171 . 0.93(7) n O19 O20 . 0.753(6) n O19 H192 . 0.40(14) n O20 H192 . 0.56(7) n O21 H181 . 0.78(3) n O21 H182 . 0.78(3) n O22 H181 . 1.09(5) n 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 O21 H181 O8 6 0.78(3) 2.00(4) 2.747(4) 161(6) O21 H182 O14 7 0.78(3) 2.33(4) 3.072(4) 160(5) O17 H171 O3 7_556 0.56(6) 2.40(6) 2.954(5) 173(10) O9 H5 O6 6 0.75(2) 1.97(2) 2.712(3) 170(4) O9 H5 O4 6 0.75(2) 2.61(3) 3.048(3) 119(4) O10 H8 O5 6 0.77(2) 1.90(3) 2.653(4) 166(5) O11 H9 O4 6 0.76(2) 2.24(2) 2.962(3) 158(4) O12 H11 O8 4 0.74(2) 1.97(3) 2.693(3) 165(4) O11 H10 O17 6 0.76(2) 1.99(2) 2.748(5) 171(5) O11 H10 O18 6 0.76(2) 2.00(3) 2.693(12) 151(4) O12 H12 O8 6 0.76(2) 1.99(2) 2.740(3) 169(4) O13 H13 O5 7_556 0.73(2) 1.96(2) 2.691(3) 172(4) O13 H14 O21 4_545 0.73(2) 2.19(2) 2.911(4) 173(5) O13 H14 O22 4_545 0.73(2) 2.33(3) 2.941(10) 143(4) O13 H14 O18 . 0.73(2) 2.65(4) 3.116(15) 124(4) O14 H15 O20 5 0.80(2) 1.92(2) 2.724(7) 175(4) O14 H15 O19 5 0.80(2) 2.09(3) 2.839(7) 155(4) O14 H16 O2 3_444 0.80(2) 1.93(3) 2.709(3) 165(4) 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_4 _geom_torsion _geom_torsion_publ_flag O2 Pd2 P2 O5 2_656 . -48.79(19) n O2 Pd2 P2 O5 . . 129.02(19) n O3 Pd2 P2 O5 2_656 . -174.2(2) n O3 Pd2 P2 O5 . . 11.2(2) n P2 Pd2 P2 O5 2_656 . -135.51(18) n O2 Pd2 P2 O4 2_656 . 74.38(11) n O2 Pd2 P2 O4 . . -107.80(11) n O3 Pd2 P2 O4 2_656 . -51.1(2) n O3 Pd2 P2 O4 . . 134.43(18) n P2 Pd2 P2 O4 2_656 . -12.33(9) n O2 Pd2 P2 O3 2_656 . -60.04(17) n O2 Pd2 P2 O3 . . 117.77(17) n O3 Pd2 P2 O3 2_656 . 174.52(17) n P2 Pd2 P2 O3 2_656 . -146.75(15) n O2 Pd2 P2 C1 2_656 . -178.02(13) n O2 Pd2 P2 C1 . . -0.21(13) n O3 Pd2 P2 C1 2_656 . 56.5(2) n O3 Pd2 P2 C1 . . -117.98(19) n P2 Pd2 P2 C1 2_656 . 95.27(12) n O8 P3 O6 Pd1 . . -177.02(13) n O7 P3 O6 Pd1 . . -53.24(18) n C2 P3 O6 Pd1 . . 63.95(18) n O4 Pd1 O6 P3 . . 122.19(16) n O7 Pd1 O6 P3 2_656 . -56.54(15) n H1 Pd1 O6 P3 5_657 . -133.7 n Pd1 Pd1 O6 P3 2_656 . 27.60(13) n O1 P1 O2 Pd2 . . 55.40(19) n O15 P1 O2 Pd2 . . 172.4(3) n O16 P1 O2 Pd2 . . -164.5(6) n C1 P1 O2 Pd2 . . -62.80(19) n O3 Pd2 O2 P1 2_656 . -125.36(16) n O3 Pd2 O2 P1 . . 58.89(16) n P2 Pd2 O2 P1 2_656 . -102.21(14) n P2 Pd2 O2 P1 . . 35.22(14) n O8 P3 O7 Pd1 . 2_656 172.72(12) n O6 P3 O7 Pd1 . 2_656 49.85(17) n C2 P3 O7 Pd1 . 2_656 -67.13(17) n O5 P2 O4 Pd1 . . -134.69(18) n O3 P2 O4 Pd1 . . 103.32(18) n C1 P2 O4 Pd1 . . -13.0(2) n Pd2 P2 O4 Pd1 . . 76.64(16) n O6 Pd1 O4 P2 . . 155.77(18) n O1 Pd1 O4 P2 . . -20.04(19) n H1 Pd1 O4 P2 5_657 . 92.5 n Pd1 Pd1 O4 P2 2_656 . -122.89(17) n O15 P1 O1 Pd1 . . 147.8(3) n O16 P1 O1 Pd1 . . 130.9(6) n O2 P1 O1 Pd1 . . -94.3(2) n C1 P1 O1 Pd1 . . 23.5(2) n O4 Pd1 O1 P1 . . 13.5(2) n O7 Pd1 O1 P1 2_656 . -167.4(2) n H1 Pd1 O1 P1 5_657 . -90.5 n Pd1 Pd1 O1 P1 2_656 . 109.06(18) n O5 P2 O3 Pd2 . . -173.15(14) n O4 P2 O3 Pd2 . . -49.78(18) n C1 P2 O3 Pd2 . . 67.13(18) n O2 Pd2 O3 P2 2_656 . 121.91(15) n O2 Pd2 O3 P2 . . -60.39(15) n P2 Pd2 O3 P2 2_656 . 66.6(3) n O5 P2 C1 P1 . . -178.70(17) n O4 P2 C1 P1 . . 59.1(2) n O3 P2 C1 P1 . . -60.0(2) n Pd2 P2 C1 P1 . . -27.31(18) n O1 P1 C1 P2 . . -64.7(2) n O15 P1 C1 P2 . . 176.9(2) n O16 P1 C1 P2 . . 169.7(5) n O2 P1 C1 P2 . . 57.1(2) n O8 P3 C2 P3 . 2_656 -177.54(11) n O7 P3 C2 P3 . 2_656 61.86(10) n O6 P3 C2 P3 . 2_656 -59.10(10) n _cod_database_fobs_code 2018637