# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Jobic, Stephane' 'Brec, R.' 'Bujoli, M.' 'Coste, S.' 'Evain, M.' 'Massiot, D.' _publ_contact_author_name 'Dr Stephane Jobic' _publ_contact_author_address ; Dr stephane Jobic chimie des solides IMN 2 rue de la houssiniere, BP 32229 NANTES 44322 FRANCE ; _publ_contact_author_email 'JOBIC@CNRS-IMN.FR' _publ_section_title ; Synthesis and Structure of Phases Containing [Ni3P3S12]3- Crown-Shaped Trimers ; data_KNiPS4-cryp #(I).cif _database_code_CSD 185895 # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C18 H36 K1 N2 Ni1 O6 P1 S4' _chemical_formula_weight 633.5 _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 16.4431(10) _cell_length_b 22.1019(11) _cell_length_c 24.1758(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8786.1(9) _cell_formula_units_Z 12 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature ? _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 1.178 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type None _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 1.000 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'IPDS Stoe' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '??integration method??' _diffrn_reflns_number 29734 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 20.74 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.1435 _diffrn_reflns_av_sigmaI/netI 0.2593 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 9004 _reflns_number_gt 3650 _reflns_threshold_expression 'I>2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_gt 0.1467 _refine_ls_R_factor_all 0.1837 _refine_ls_wR_factor_ref 0.1658 _refine_ls_goodness_of_fit_ref 0.97 _refine_ls_goodness_of_fit_gt 1.38 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 9004 _refine_ls_number_parameters 368 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.001024I^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0199 _refine_ls_shift/su_mean 0.0016 _refine_diff_density_max 2.48 _refine_diff_density_min -1.72 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_versus_stol_list K 0.201 0.249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 19.000 18.204 16.733 15.243 13.728 12.268 10.977 9.908 9.061 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 8.403 7.889 7.474 7.125 6.814 6.523 6.241 5.961 5.684 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 5.406 5.130 4.859 4.594 4.337 4.090 3.855 3.632 3.423 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 3.227 3.045 2.877 2.722 2.580 2.033 1.951 1.876 1.809 ; Ni 0.339 1.112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 28.000 27.356 25.807 23.973 22.150 20.390 18.696 17.084 15.576 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 14.196 12.956 11.862 10.909 10.090 9.392 8.802 8.301 7.879 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 7.519 7.212 6.944 6.708 6.495 6.301 6.118 5.944 5.776 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 5.612 5.451 5.292 5.133 4.975 4.211 4.065 3.922 3.783 ; P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 15.000 14.458 13.138 11.629 10.327 9.335 8.600 8.029 7.547 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 7.103 6.674 6.250 5.829 5.418 5.020 4.640 4.284 3.953 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 3.649 3.372 3.122 2.898 2.698 2.521 2.364 2.226 2.104 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.997 1.903 1.820 1.747 1.683 1.453 1.420 1.389 1.360 ; S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 16.000 15.484 14.177 12.583 11.109 9.927 9.039 8.376 7.856 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 7.417 7.017 6.633 6.254 5.877 5.505 5.141 4.790 4.454 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 4.138 3.842 3.570 3.320 3.092 2.885 2.699 2.533 2.384 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 2.251 2.133 2.028 1.935 1.853 1.557 1.515 1.477 1.442 ; C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 6.000 5.749 5.107 4.311 3.560 2.949 2.494 2.171 1.948 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 1.794 1.685 1.603 1.537 1.479 1.426 1.374 1.322 1.271 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.219 1.166 1.114 1.063 1.012 0.962 0.914 0.867 0.822 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.778 0.736 0.697 0.659 0.622 0.468 0.442 0.418 0.395 ; O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 8.000 7.798 7.245 6.472 5.623 4.808 4.089 3.489 3.006 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 2.629 2.338 2.115 1.946 1.816 1.714 1.635 1.568 1.512 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.463 1.419 1.377 1.337 1.298 1.259 1.221 1.183 1.145 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.107 1.070 1.033 0.997 0.961 0.792 0.761 0.731 0.702 ; N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 7.000 6.776 6.180 5.385 4.563 3.825 3.219 2.747 2.393 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 2.132 1.942 1.802 1.697 1.616 1.551 1.496 1.445 1.398 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.353 1.309 1.265 1.221 1.177 1.133 1.090 1.047 1.004 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.962 0.921 0.882 0.843 0.805 0.636 0.606 0.578 0.551 ; H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 1.000 0.960 0.854 0.713 0.568 0.438 0.331 0.248 0.184 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 0.138 0.103 0.078 0.060 0.046 0.036 0.028 0.022 0.018 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 0.014 0.011 0.009 0.007 0.006 0.005 0.004 0.004 0.003 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.003 0.002 0.002 0.002 0.002 0.002 0.001 0.001 0.000 ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_adp_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni2 Ni Uani 0.58170(17) 0.51819(14) 0.95929(11) 0.0544(12) 4 1 d . . . Ni3 Ni Uani 0.57660(17) 0.50058(16) 0.82335(10) 0.0601(13) 4 1 d . . . Ni1 Ni Uani 0.40830(15) 0.49941(15) 0.89895(10) 0.0537(11) 4 1 d . . . P1 P Uani 0.4229(4) 0.5052(3) 1.0239(2) 0.056(2) 4 1 d . . . P2 P Uani 0.7308(3) 0.5078(3) 0.8874(3) 0.067(3) 4 1 d . . . P3 P Uani 0.4115(4) 0.4728(3) 0.7767(2) 0.065(3) 4 1 d . . . S1 S Uani 0.4621(4) 0.5651(3) 0.9570(3) 0.076(3) 4 1 d . . . S6 S Uani 0.7008(3) 0.4710(3) 0.9627(2) 0.058(2) 4 1 d . . . S5 S Uani 0.5383(3) 0.4717(3) 1.0348(2) 0.068(3) 4 1 d . . . S2 S Uani 0.6289(3) 0.5648(3) 0.8851(3) 0.068(3) 4 1 d . . . S12 S Uani 0.3425(4) 0.4891(4) 0.7138(2) 0.088(3) 4 1 d . . . S11 S Uani 0.8396(3) 0.5419(4) 0.8836(3) 0.093(3) 4 1 d . . . S7 S Uani 0.6979(4) 0.4557(3) 0.8212(3) 0.072(3) 4 1 d . . . S10 S Uani 0.3714(4) 0.5304(4) 1.0897(2) 0.091(3) 4 1 d . . . S9 S Uani 0.3553(4) 0.4317(3) 0.8429(2) 0.063(3) 4 1 d . . . S8 S Uani 0.5247(4) 0.4392(3) 0.7602(2) 0.068(3) 4 1 d . . . S4 S Uani 0.3525(3) 0.4547(3) 0.9711(2) 0.056(3) 4 1 d . . . S3 S Uani 0.4569(3) 0.5460(3) 0.8253(2) 0.062(3) 4 1 d . . . K1a K Uani 0.1923(2) 0.7430(2) 0.89097(19) 0.0526(19) 4 1 d . . . N1a N Uani 0.2263(11) 0.8748(9) 0.8960(9) 0.085(9) 4 1 d . . . N2a N Uani 0.1544(13) 0.6102(11) 0.8789(12) 0.146(14) 4 1 d . . . K1c K Uani 0.4770(3) 0.6705(3) 0.5742(2) 0.077(3) 4 1 d . . . N1c N Uani 0.5098(15) 0.5381(10) 0.5555(8) 0.110(11) 4 1 d . . . N2c N Uani 0.4466(10) 0.7990(9) 0.5865(6) 0.066(8) 4 1 d . . . K1b K Uani 0.8797(3) 0.7484(3) 0.69531(17) 0.056(2) 4 1 d . . . N1b N Uani 0.8372(9) 0.6175(9) 0.6810(8) 0.072(9) 4 1 d . . . N2b N Uani 0.9233(12) 0.8757(9) 0.7082(8) 0.086(9) 4 1 d . . . O1a O Uani 0.0620(12) 0.8251(7) 0.8705(12) 0.082(3) 4 1 d . . . O2a O Uani 0.0290(17) 0.7029(9) 0.8849(15) 0.081(3) 4 1 d . . . C1a C Uani 0.1565(17) 0.9075(10) 0.8673(17) 0.116(6) 4 1 d . . . C2a C Uani 0.0788(16) 0.8828(9) 0.8907(14) 0.123(6) 4 1 d . . . C3a C Uani -0.0113(14) 0.8025(11) 0.8891(15) 0.122(7) 4 1 d . . . C4a C Uani -0.0293(16) 0.7441(11) 0.8668(16) 0.108(6) 4 1 d . . . C5a C Uani 0.010(2) 0.6454(11) 0.8661(18) 0.118(6) 4 1 d . . . C6a C Uani 0.072(3) 0.6027(10) 0.886(2) 0.124(6) 4 1 d . . . H1c1a H Uiso 0.1589(12) 0.9534(7) 0.8723(12) 0.122(9) 4 1 d . . . H2c1a H Uiso 0.1586(12) 0.8984(7) 0.8271(12) 0.122(9) 4 1 d . . . H1c2a H Uiso 0.0872(12) 0.8804(7) 0.9335(12) 0.122(9) 4 1 d . . . H2c2a H Uiso 0.0341(12) 0.9117(7) 0.8842(12) 0.122(9) 4 1 d . . . H1c3a H Uiso -0.0117(12) 0.7939(7) 0.9307(12) 0.122(9) 4 1 d . . . H2c3a H Uiso -0.0595(12) 0.8283(7) 0.8805(12) 0.122(9) 4 1 d . . . H1c4a H Uiso -0.0255(12) 0.7501(7) 0.8236(12) 0.122(9) 4 1 d . . . H2c4a H Uiso -0.0852(12) 0.7314(7) 0.8748(12) 0.122(9) 4 1 d . . . H1c5a H Uiso 0.0179(12) 0.6445(7) 0.8201(12) 0.122(9) 4 1 d . . . H2c5a H Uiso -0.0437(12) 0.6313(7) 0.8717(12) 0.122(9) 4 1 d . . . H1c6a H Uiso 0.0700(12) 0.6014(7) 0.9268(12) 0.122(9) 4 1 d . . . H2c6a H Uiso 0.0587(12) 0.5572(7) 0.8732(12) 0.122(9) 4 1 d . . . O1b O Uani 0.2541(18) 0.7884(6) 0.9891(9) 0.082(3) 4 1 d . . . O2b O Uani 0.247(2) 0.6646(8) 0.9709(12) 0.081(3) 4 1 d . . . C1b C Uani 0.245(2) 0.8903(9) 0.9557(13) 0.116(6) 4 1 d . . . C2b C Uani 0.294(2) 0.8441(8) 0.9870(12) 0.123(7) 4 1 d . . . C3b C Uani 0.296(2) 0.7460(10) 1.0201(11) 0.122(7) 4 1 d . . . C4b C Uani 0.253(2) 0.6896(10) 1.0236(12) 0.108(6) 4 1 d . . . C5b C Uani 0.210(3) 0.6083(11) 0.9739(15) 0.118(6) 4 1 d . . . C6b C Uani 0.205(3) 0.5824(11) 0.9180(18) 0.124(7) 4 1 d . . . H1c1b H Uiso 0.2649(18) 0.9330(6) 0.9647(9) 0.122(9) 4 1 d . . . H2c1b H Uiso 0.1872(18) 0.8870(6) 0.9670(9) 0.122(9) 4 1 d . . . H1c2b H Uiso 0.3484(18) 0.8391(6) 0.9655(9) 0.122(9) 4 1 d . . . H2c2b H Uiso 0.3076(18) 0.8600(6) 1.0240(9) 0.122(9) 4 1 d . . . H1c3b H Uiso 0.3494(18) 0.7331(6) 1.0026(9) 0.122(9) 4 1 d . . . H2c3b H Uiso 0.3068(18) 0.7583(6) 1.0591(9) 0.122(9) 4 1 d . . . H1c4b H Uiso 0.1953(18) 0.7012(6) 1.0389(9) 0.122(9) 4 1 d . . . H2c4b H Uiso 0.2778(18) 0.6621(6) 1.0507(9) 0.122(9) 4 1 d . . . H1c5b H Uiso 0.1449(18) 0.6149(6) 0.9859(9) 0.122(9) 4 1 d . . . H2c5b H Uiso 0.2302(18) 0.5804(6) 1.0002(9) 0.122(9) 4 1 d . . . H1c6b H Uiso 0.2602(18) 0.5761(6) 0.9036(9) 0.122(9) 4 1 d . . . H2c6b H Uiso 0.1778(18) 0.5383(6) 0.9184(9) 0.122(9) 4 1 d . . . O1c O Uani 0.3101(16) 0.7938(7) 0.8217(11) 0.082(3) 4 1 d . . . O2c O Uani 0.2567(19) 0.6776(9) 0.7980(13) 0.081(3) 4 1 d . . . C1c C Uani 0.292(2) 0.8894(10) 0.8667(14) 0.116(6) 4 1 d . . . C2c C Uani 0.3093(19) 0.8562(9) 0.8139(13) 0.123(7) 4 1 d . . . C3c C Uani 0.3303(19) 0.7622(11) 0.7744(13) 0.122(7) 4 1 d . . . C4c C Uani 0.334(2) 0.6983(11) 0.7834(14) 0.108(6) 4 1 d . . . C5c C Uani 0.258(2) 0.6152(12) 0.8038(16) 0.118(6) 4 1 d . . . C6c C Uani 0.176(3) 0.5943(12) 0.8182(19) 0.124(7) 4 1 d . . . H1c1c H Uiso 0.3088(16) 0.9337(7) 0.8634(11) 0.122(9) 4 1 d . . . H2c1c H Uiso 0.3234(16) 0.8706(7) 0.8971(11) 0.122(9) 4 1 d . . . H1c2c H Uiso 0.2623(16) 0.8674(7) 0.7866(11) 0.122(9) 4 1 d . . . H2c2c H Uiso 0.3602(16) 0.8717(7) 0.7973(11) 0.122(9) 4 1 d . . . H1c3c H Uiso 0.2873(16) 0.7654(7) 0.7441(11) 0.122(9) 4 1 d . . . H2c3c H Uiso 0.3839(16) 0.7735(7) 0.7579(11) 0.122(9) 4 1 d . . . H1c4c H Uiso 0.3747(16) 0.6930(7) 0.8165(11) 0.122(9) 4 1 d . . . H2c4c H Uiso 0.3572(16) 0.6767(7) 0.7517(11) 0.122(9) 4 1 d . . . H1c5c H Uiso 0.2951(16) 0.6036(7) 0.8410(11) 0.122(9) 4 1 d . . . H2c5c H Uiso 0.2814(16) 0.5922(7) 0.7750(11) 0.122(9) 4 1 d . . . H1c6c H Uiso 0.1382(16) 0.6037(7) 0.7882(11) 0.122(9) 4 1 d . . . H2c6c H Uiso 0.1736(16) 0.5459(7) 0.8227(11) 0.122(9) 4 1 d . . . O1d O Uani 0.7596(16) 0.6982(7) 0.7626(11) 0.082(3) 4 1 d . . . O2d O Uani 0.8203(19) 0.8121(9) 0.7878(13) 0.081(3) 4 1 d . . . C1d C Uani 0.771(2) 0.6033(11) 0.7154(14) 0.116(6) 4 1 d . . . C2d C Uani 0.7573(19) 0.6357(10) 0.7691(13) 0.123(7) 4 1 d . . . C3d C Uani 0.7430(19) 0.7292(11) 0.8109(13) 0.122(7) 4 1 d . . . C4d C Uani 0.743(2) 0.7933(12) 0.8034(14) 0.108(6) 4 1 d . . . C5d C Uani 0.822(2) 0.8746(12) 0.7833(16) 0.118(7) 4 1 d . . . C6d C Uani 0.905(3) 0.8934(12) 0.7678(19) 0.124(7) 4 1 d . . . H1c1d H Uiso 0.7517(16) 0.5595(7) 0.7181(11) 0.122(9) 4 1 d . . . H2c1d H Uiso 0.7393(16) 0.6238(7) 0.6860(11) 0.122(9) 4 1 d . . . H1c2d H Uiso 0.8047(16) 0.6224(7) 0.7953(11) 0.122(9) 4 1 d . . . H2c2d H Uiso 0.7063(16) 0.6213(7) 0.7863(11) 0.122(9) 4 1 d . . . H1c3d H Uiso 0.7869(16) 0.7239(7) 0.8404(11) 0.122(9) 4 1 d . . . H2c3d H Uiso 0.6895(16) 0.7191(7) 0.8282(11) 0.122(9) 4 1 d . . . H1c4d H Uiso 0.7008(16) 0.8007(7) 0.7711(11) 0.122(9) 4 1 d . . . H2c4d H Uiso 0.7217(16) 0.8147(7) 0.8359(11) 0.122(9) 4 1 d . . . H1c5d H Uiso 0.7843(16) 0.8883(7) 0.7470(11) 0.122(9) 4 1 d . . . H2c5d H Uiso 0.8011(16) 0.8976(7) 0.8130(11) 0.122(9) 4 1 d . . . H1c6d H Uiso 0.9430(16) 0.8821(7) 0.7969(11) 0.122(9) 4 1 d . . . H2c6d H Uiso 0.9095(16) 0.9418(7) 0.7643(11) 0.122(9) 4 1 d . . . O1e O Uani 0.8070(17) 0.7088(6) 0.5951(10) 0.082(3) 4 1 d . . . O2e O Uani 0.822(2) 0.8313(8) 0.6183(13) 0.081(3) 4 1 d . . . C1e C Uani 0.824(2) 0.6050(9) 0.6213(13) 0.116(6) 4 1 d . . . C2e C Uani 0.768(2) 0.6532(9) 0.5997(12) 0.123(7) 4 1 d . . . C3e C Uani 0.758(2) 0.7533(10) 0.5727(12) 0.122(7) 4 1 d . . . C4e C Uani 0.800(2) 0.8096(10) 0.5663(13) 0.108(6) 4 1 d . . . C5e C Uani 0.858(2) 0.8876(11) 0.6131(15) 0.118(6) 4 1 d . . . C6e C Uani 0.880(3) 0.9099(11) 0.6685(18) 0.124(7) 4 1 d . . . H1c1e H Uiso 0.8006(17) 0.5630(6) 0.6131(10) 0.122(9) 4 1 d . . . H2c1e H Uiso 0.8770(17) 0.6088(6) 0.6025(10) 0.122(9) 4 1 d . . . H1c2e H Uiso 0.7206(17) 0.6570(6) 0.6286(10) 0.122(9) 4 1 d . . . H2c2e H Uiso 0.7428(17) 0.6397(6) 0.5647(10) 0.122(9) 4 1 d . . . H1c3e H Uiso 0.7108(17) 0.7652(6) 0.5978(10) 0.122(9) 4 1 d . . . H2c3e H Uiso 0.7353(17) 0.7435(6) 0.5354(10) 0.122(9) 4 1 d . . . H1c4e H Uiso 0.8516(17) 0.7989(6) 0.5428(10) 0.122(9) 4 1 d . . . H2c4e H Uiso 0.7682(17) 0.8389(6) 0.5446(10) 0.122(9) 4 1 d . . . H1c5e H Uiso 0.9185(17) 0.8816(6) 0.5921(10) 0.122(9) 4 1 d . . . H2c5e H Uiso 0.8314(17) 0.9171(6) 0.5916(10) 0.122(9) 4 1 d . . . H1c6e H Uiso 0.8307(17) 0.9154(6) 0.6904(10) 0.122(9) 4 1 d . . . H2c6e H Uiso 0.9078(17) 0.9539(6) 0.6665(10) 0.122(9) 4 1 d . . . O1f O Uani 1.0049(12) 0.6605(7) 0.7095(12) 0.082(3) 4 1 d . . . O2f O Uani 1.0475(17) 0.7814(9) 0.6981(15) 0.081(3) 4 1 d . . . C1f C Uani 0.9057(17) 0.5813(10) 0.7047(17) 0.116(6) 4 1 d . . . C2f C Uani 0.9884(16) 0.6034(9) 0.6881(14) 0.123(6) 4 1 d . . . C3f C Uani 1.0823(14) 0.6806(11) 0.6971(16) 0.122(7) 4 1 d . . . C4f C Uani 1.0996(16) 0.7384(12) 0.7209(16) 0.108(6) 4 1 d . . . C5f C Uani 1.066(2) 0.8383(11) 0.7184(18) 0.118(6) 4 1 d . . . C6f C Uani 1.012(3) 0.8829(10) 0.693(2) 0.124(6) 4 1 d . . . H1c1f H Uiso 0.9015(12) 0.5355(7) 0.6996(12) 0.122(9) 4 1 d . . . H2c1f H Uiso 0.8969(12) 0.5907(7) 0.7444(12) 0.122(9) 4 1 d . . . H1c2f H Uiso 0.9880(12) 0.6058(7) 0.6448(12) 0.122(9) 4 1 d . . . H2c2f H Uiso 1.0299(12) 0.5730(7) 0.6982(12) 0.122(9) 4 1 d . . . H1c3f H Uiso 1.0907(12) 0.6890(7) 0.6560(12) 0.122(9) 4 1 d . . . H2c3f H Uiso 1.1270(12) 0.6533(7) 0.7097(12) 0.122(9) 4 1 d . . . H1c4f H Uiso 1.0877(12) 0.7328(7) 0.7634(12) 0.122(9) 4 1 d . . . H2c4f H Uiso 1.1572(12) 0.7492(7) 0.7176(12) 0.122(9) 4 1 d . . . H1c5f H Uiso 1.0503(12) 0.8398(7) 0.7634(12) 0.122(9) 4 1 d . . . H2c5f H Uiso 1.1215(12) 0.8506(7) 0.7173(12) 0.122(9) 4 1 d . . . H1c6f H Uiso 1.0205(12) 0.8840(7) 0.6532(12) 0.122(9) 4 1 d . . . H2c6f H Uiso 1.0247(12) 0.9281(7) 0.7073(12) 0.122(9) 4 1 d . . . O1g O Uani 0.3449(13) 0.5915(7) 0.5835(12) 0.082(3) 4 1 d . . . O2g O Uani 0.3148(17) 0.7149(9) 0.5777(14) 0.081(3) 4 1 d . . . C1g C Uani 0.4300(18) 0.5059(10) 0.5649(16) 0.116(6) 4 1 d . . . C2g C Uani 0.3470(17) 0.5337(9) 0.5606(14) 0.123(6) 4 1 d . . . C3g C Uani 0.2682(16) 0.6169(11) 0.5827(15) 0.122(7) 4 1 d . . . C4g C Uani 0.2661(17) 0.6753(11) 0.6080(15) 0.108(6) 4 1 d . . . C5g C Uani 0.310(2) 0.7726(11) 0.5999(17) 0.118(6) 4 1 d . . . C6g C Uani 0.361(3) 0.8136(10) 0.567(2) 0.124(6) 4 1 d . . . H1c1g H Uiso 0.4268(13) 0.4601(7) 0.5596(12) 0.122(9) 4 1 d . . . H2c1g H Uiso 0.4523(13) 0.5141(7) 0.6023(12) 0.122(9) 4 1 d . . . H1c2g H Uiso 0.3340(13) 0.5366(7) 0.5183(12) 0.122(9) 4 1 d . . . H2c2g H Uiso 0.3062(13) 0.5061(7) 0.5769(12) 0.122(9) 4 1 d . . . H1c3g H Uiso 0.2480(13) 0.6263(7) 0.5437(12) 0.122(9) 4 1 d . . . H2c3g H Uiso 0.2254(13) 0.5925(7) 0.6018(12) 0.122(9) 4 1 d . . . H1c4g H Uiso 0.2904(13) 0.6684(7) 0.6478(12) 0.122(9) 4 1 d . . . H2c4g H Uiso 0.2103(13) 0.6901(7) 0.6132(12) 0.122(9) 4 1 d . . . H1c5g H Uiso 0.3400(13) 0.7724(7) 0.6414(12) 0.122(9) 4 1 d . . . H2c5g H Uiso 0.2575(13) 0.7886(7) 0.6068(12) 0.122(9) 4 1 d . . . H1c6g H Uiso 0.3394(13) 0.8157(7) 0.5291(12) 0.122(9) 4 1 d . . . H2c6g H Uiso 0.3579(13) 0.8592(7) 0.5822(12) 0.122(9) 4 1 d . . . O1h O Uani 0.5470(17) 0.6278(6) 0.4726(10) 0.082(3) 4 1 d . . . O2h O Uani 0.545(2) 0.7506(8) 0.4963(12) 0.081(3) 4 1 d . . . C1h C Uani 0.526(2) 0.5248(10) 0.5002(13) 0.116(6) 4 1 d . . . C2h C Uani 0.582(2) 0.5706(9) 0.4746(12) 0.123(7) 4 1 d . . . C3h C Uani 0.596(2) 0.6701(10) 0.4467(12) 0.122(7) 4 1 d . . . C4h C Uani 0.558(2) 0.7282(10) 0.4431(12) 0.108(6) 4 1 d . . . C5h C Uani 0.513(2) 0.8084(11) 0.4936(15) 0.118(6) 4 1 d . . . C6h C Uani 0.502(3) 0.8315(11) 0.5501(18) 0.124(7) 4 1 d . . . H1c1h H Uiso 0.5446(17) 0.4819(6) 0.4905(10) 0.122(9) 4 1 d . . . H2c1h H Uiso 0.4707(17) 0.5309(6) 0.4854(10) 0.122(9) 4 1 d . . . H1c2h H Uiso 0.6339(17) 0.5722(6) 0.5000(10) 0.122(9) 4 1 d . . . H2c2h H Uiso 0.6006(17) 0.5561(6) 0.4380(10) 0.122(9) 4 1 d . . . H1c3h H Uiso 0.6473(17) 0.6799(6) 0.4682(10) 0.122(9) 4 1 d . . . H2c3h H Uiso 0.6117(17) 0.6594(6) 0.4080(10) 0.122(9) 4 1 d . . . H1c4h H Uiso 0.5017(17) 0.7198(6) 0.4234(10) 0.122(9) 4 1 d . . . H2c4h H Uiso 0.5880(17) 0.7560(6) 0.4191(10) 0.122(9) 4 1 d . . . H1c5h H Uiso 0.4495(17) 0.8051(6) 0.4770(10) 0.122(9) 4 1 d . . . H2c5h H Uiso 0.5386(17) 0.8368(6) 0.4701(10) 0.122(9) 4 1 d . . . H1c6h H Uiso 0.5544(17) 0.8348(6) 0.5683(10) 0.122(9) 4 1 d . . . H2c6h H Uiso 0.4772(17) 0.8766(6) 0.5500(10) 0.122(9) 4 1 d . . . O1i O Uani 0.5667(17) 0.6090(8) 0.6521(8) 0.082(3) 4 1 d . . . O2i O Uani 0.508(2) 0.7237(9) 0.6759(11) 0.081(3) 4 1 d . . . C1i C Uani 0.578(2) 0.5240(11) 0.5911(12) 0.116(6) 4 1 d . . . C2i C Uani 0.558(2) 0.5465(10) 0.6481(11) 0.123(7) 4 1 d . . . C3i C Uani 0.553(2) 0.6305(11) 0.7049(10) 0.122(7) 4 1 d . . . C4i C Uani 0.565(2) 0.6945(12) 0.7091(11) 0.108(6) 4 1 d . . . C5i C Uani 0.515(2) 0.7858(12) 0.6818(14) 0.118(6) 4 1 d . . . C6i C Uani 0.453(3) 0.8156(11) 0.6472(18) 0.124(6) 4 1 d . . . H1c1i H Uiso 0.5889(17) 0.4785(8) 0.5917(8) 0.122(9) 4 1 d . . . H2c1i H Uiso 0.6275(17) 0.5448(8) 0.5777(8) 0.122(9) 4 1 d . . . H1c2i H Uiso 0.4973(17) 0.5349(8) 0.6553(8) 0.122(9) 4 1 d . . . H2c2i H Uiso 0.5909(17) 0.5243(8) 0.6757(8) 0.122(9) 4 1 d . . . H1c3i H Uiso 0.4939(17) 0.6260(8) 0.7173(8) 0.122(9) 4 1 d . . . H2c3i H Uiso 0.5883(17) 0.6123(8) 0.7341(8) 0.122(9) 4 1 d . . . H1c4i H Uiso 0.6239(17) 0.7017(8) 0.6939(8) 0.122(9) 4 1 d . . . H2c4i H Uiso 0.5642(17) 0.7085(8) 0.7476(8) 0.122(9) 4 1 d . . . H1c5i H Uiso 0.5741(17) 0.8002(8) 0.6630(8) 0.122(9) 4 1 d . . . H2c5i H Uiso 0.5167(17) 0.8017(8) 0.7181(8) 0.122(9) 4 1 d . . . H1c6i H Uiso 0.3992(17) 0.8046(8) 0.6601(8) 0.122(9) 4 1 d . . . H2c6i H Uiso 0.4564(17) 0.8641(8) 0.6509(8) 0.122(9) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Ni2 Ni 0.049(2) 0.056(2) 0.0584(18) 0.0019(18) 0.0038(16) -0.0014(18) Ni3 Ni 0.0504(19) 0.074(3) 0.0557(19) 0.015(2) 0.0084(16) 0.026(2) Ni1 Ni 0.0468(17) 0.069(3) 0.0450(16) 0.0022(18) 0.0094(15) -0.006(2) P1 P 0.070(4) 0.057(5) 0.041(4) -0.005(4) 0.018(3) -0.004(4) P2 P 0.035(3) 0.088(6) 0.077(5) 0.005(4) 0.012(3) 0.029(5) P3 P 0.048(4) 0.104(7) 0.042(4) 0.014(4) 0.005(3) 0.011(4) S1 S 0.061(5) 0.080(6) 0.089(5) 0.006(4) 0.000(4) -0.017(5) S6 S 0.045(4) 0.067(5) 0.063(4) -0.002(4) 0.017(3) 0.016(4) S5 S 0.070(4) 0.083(6) 0.051(4) 0.001(4) 0.008(3) -0.018(4) S2 S 0.048(4) 0.064(6) 0.091(5) 0.000(4) 0.002(4) 0.030(4) S12 S 0.082(5) 0.121(8) 0.060(4) 0.021(5) -0.004(4) 0.004(5) S11 S 0.050(4) 0.113(7) 0.116(6) 0.006(4) 0.002(4) 0.070(6) S7 S 0.058(4) 0.089(6) 0.069(4) 0.017(4) 0.014(4) 0.014(4) S10 S 0.062(4) 0.149(8) 0.062(4) -0.026(5) 0.019(3) -0.054(5) S9 S 0.066(5) 0.076(6) 0.046(4) 0.000(4) 0.007(3) -0.004(4) S8 S 0.067(4) 0.088(6) 0.051(4) 0.025(4) 0.011(4) 0.025(4) S4 S 0.056(4) 0.073(5) 0.039(3) 0.008(4) 0.013(3) -0.013(4) S3 S 0.048(4) 0.084(6) 0.055(4) 0.018(4) 0.008(3) 0.015(4) K1a K 0.045(3) 0.067(4) 0.046(3) -0.002(3) 0.006(3) 0.014(3) N1a N 0.089(15) 0.047(16) 0.120(17) 0.008(12) -0.009(15) -0.033(14) N2a N 0.093(17) 0.11(2) 0.24(3) -0.057(15) -0.11(2) 0.10(2) K1c K 0.069(4) 0.096(5) 0.066(4) 0.012(4) 0.008(3) 0.004(4) N1c N 0.20(2) 0.039(16) 0.097(17) -0.006(16) 0.007(16) -0.030(14) N2c N 0.061(13) 0.087(17) 0.050(12) 0.007(11) -0.026(9) -0.027(11) K1b K 0.055(3) 0.078(5) 0.036(3) 0.016(3) -0.005(2) -0.009(3) N1b N 0.020(10) 0.077(17) 0.119(16) 0.016(10) -0.015(11) 0.020(14) N2b N 0.088(15) 0.055(16) 0.115(17) 0.009(14) -0.004(15) 0.033(13) O1a O 0.071(5) 0.079(5) 0.095(5) 0.026(4) 0.010(4) 0.003(4) O2a O 0.040(4) 0.101(6) 0.102(5) -0.017(4) -0.009(3) 0.008(5) C1a C 0.173(13) 0.039(7) 0.136(9) 0.030(7) -0.012(9) -0.006(6) C2a C 0.101(10) 0.117(11) 0.150(11) 0.053(9) 0.017(9) 0.009(10) C3a C 0.039(8) 0.206(16) 0.121(10) 0.053(9) 0.008(7) 0.048(11) C4a C 0.041(7) 0.169(14) 0.114(9) -0.005(9) -0.029(6) 0.047(10) C5a C 0.059(8) 0.131(13) 0.164(11) -0.024(8) -0.025(7) -0.018(10) C6a C 0.142(11) 0.105(11) 0.124(9) -0.066(9) 0.005(8) 0.004(9) O1b O 0.084(5) 0.094(5) 0.068(5) 0.000(4) -0.022(4) -0.017(4) O2b O 0.106(5) 0.082(6) 0.055(5) 0.014(4) -0.004(3) 0.028(4) C1b C 0.135(10) 0.079(8) 0.134(12) -0.040(7) 0.002(8) -0.057(7) C2b C 0.130(12) 0.147(12) 0.091(11) 0.001(9) -0.041(8) -0.035(9) C3b C 0.125(11) 0.208(15) 0.032(10) 0.059(10) -0.028(8) -0.008(9) C4b C 0.146(10) 0.142(13) 0.036(9) 0.049(9) 0.014(7) 0.025(8) C5b C 0.162(11) 0.112(12) 0.080(10) -0.014(9) -0.010(7) 0.048(8) C6b C 0.133(10) 0.065(12) 0.174(12) 0.013(8) 0.020(8) 0.035(9) O1c O 0.076(5) 0.096(5) 0.073(5) -0.019(4) 0.018(4) 0.009(4) O2c O 0.071(5) 0.090(6) 0.082(5) 0.020(4) 0.021(3) -0.027(4) C1c C 0.116(11) 0.067(8) 0.165(12) -0.049(7) -0.007(8) 0.033(7) C2c C 0.107(12) 0.152(12) 0.109(11) -0.039(9) 0.035(8) 0.018(9) C3c C 0.053(11) 0.238(15) 0.075(10) -0.008(10) 0.039(7) -0.018(10) C4c C 0.044(10) 0.170(14) 0.110(8) 0.023(9) 0.018(6) -0.049(9) C5c C 0.112(11) 0.103(12) 0.140(10) 0.038(9) 0.045(7) -0.022(9) C6c C 0.166(12) 0.077(12) 0.129(11) 0.020(8) -0.027(8) -0.041(9) O1d O 0.076(5) 0.097(5) 0.073(5) -0.018(4) 0.018(4) 0.010(4) O2d O 0.074(5) 0.089(6) 0.080(4) 0.019(4) 0.021(3) -0.029(4) C1d C 0.112(11) 0.070(8) 0.166(12) -0.050(7) -0.006(8) 0.032(7) C2d C 0.106(12) 0.155(12) 0.108(11) -0.038(9) 0.035(8) 0.018(9) C3d C 0.054(12) 0.239(15) 0.072(10) -0.002(10) 0.038(7) -0.015(9) C4d C 0.047(10) 0.170(14) 0.107(8) 0.026(9) 0.018(7) -0.049(9) C5d C 0.117(11) 0.101(13) 0.136(10) 0.036(8) 0.045(7) -0.026(9) C6d C 0.166(12) 0.077(12) 0.129(11) 0.016(8) -0.029(8) -0.041(9) O1e O 0.075(5) 0.096(5) 0.075(5) -0.002(4) -0.023(4) -0.015(4) O2e O 0.103(5) 0.078(6) 0.062(5) 0.019(4) -0.013(3) 0.026(4) C1e C 0.134(11) 0.086(9) 0.128(12) -0.052(7) -0.001(8) -0.050(7) C2e C 0.112(12) 0.151(12) 0.106(12) -0.003(9) -0.046(8) -0.032(9) C3e C 0.112(11) 0.208(15) 0.045(11) 0.060(10) -0.042(7) -0.010(9) C4e C 0.149(10) 0.139(13) 0.037(9) 0.054(9) -0.006(7) 0.020(8) C5e C 0.155(11) 0.106(12) 0.093(10) -0.003(9) -0.025(7) 0.052(8) C6e C 0.143(11) 0.062(12) 0.167(12) 0.017(8) 0.028(8) 0.025(8) O1f O 0.071(5) 0.077(5) 0.097(5) 0.025(4) 0.007(4) 0.006(4) O2f O 0.042(4) 0.103(6) 0.098(5) -0.015(4) -0.016(3) 0.006(5) C1f C 0.178(13) 0.036(7) 0.134(9) 0.024(7) -0.007(9) -0.002(6) C2f C 0.103(10) 0.113(11) 0.153(11) 0.052(9) 0.011(9) 0.014(10) C3f C 0.043(8) 0.201(16) 0.121(10) 0.054(9) 0.000(7) 0.055(11) C4f C 0.048(7) 0.170(14) 0.106(9) -0.005(9) -0.035(6) 0.047(10) C5f C 0.065(8) 0.133(13) 0.156(11) -0.019(8) -0.037(7) -0.019(10) C6f C 0.135(11) 0.111(11) 0.126(9) -0.068(9) 0.007(8) -0.005(9) O1g O 0.065(5) 0.081(5) 0.099(5) -0.023(4) 0.000(4) 0.011(4) O2g O 0.055(4) 0.099(6) 0.089(5) 0.021(4) 0.026(3) 0.000(5) C1g C 0.173(13) 0.042(7) 0.133(10) -0.037(7) -0.002(9) 0.004(6) C2g C 0.092(10) 0.122(12) 0.155(11) -0.046(9) 0.003(8) 0.026(10) C3g C 0.041(9) 0.208(16) 0.116(10) -0.025(9) 0.023(7) 0.062(11) C4g C 0.070(7) 0.167(14) 0.087(9) 0.025(9) 0.047(6) 0.040(10) C5g C 0.088(8) 0.129(13) 0.136(11) 0.019(8) 0.051(7) -0.027(10) C6g C 0.143(11) 0.099(11) 0.130(10) 0.062(9) -0.011(8) -0.018(9) O1h O 0.080(5) 0.096(5) 0.070(5) 0.001(4) 0.022(4) -0.016(4) O2h O 0.103(5) 0.081(6) 0.059(5) -0.018(4) 0.010(3) 0.028(4) C1h C 0.140(10) 0.080(9) 0.128(12) 0.043(7) -0.003(8) -0.055(7) C2h C 0.122(12) 0.151(12) 0.096(12) 0.002(9) 0.043(8) -0.035(9) C3h C 0.113(11) 0.215(15) 0.037(11) -0.055(10) 0.034(7) -0.006(9) C4h C 0.143(10) 0.145(13) 0.037(9) -0.052(9) -0.004(7) 0.026(8) C5h C 0.160(11) 0.106(12) 0.088(10) 0.005(9) 0.021(7) 0.050(8) C6h C 0.136(11) 0.064(12) 0.172(12) -0.019(8) -0.023(8) 0.029(8) O1i O 0.091(5) 0.088(5) 0.067(5) 0.014(4) -0.006(4) 0.023(4) O2i O 0.091(5) 0.101(6) 0.051(4) -0.001(4) -0.018(3) -0.026(4) C1i C 0.122(9) 0.050(8) 0.176(13) 0.029(6) -0.009(9) 0.032(7) C2i C 0.139(12) 0.136(12) 0.094(10) 0.030(9) -0.014(9) 0.045(9) C3i C 0.091(11) 0.234(15) 0.041(9) 0.025(10) -0.027(7) 0.026(9) C4i C 0.074(10) 0.186(14) 0.064(7) 0.013(9) -0.037(6) -0.033(9) C5i C 0.154(12) 0.117(13) 0.083(8) -0.017(9) -0.042(7) -0.032(8) C6i C 0.135(10) 0.096(11) 0.140(11) -0.005(8) 0.028(8) -0.058(9) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni2 S1 . . 2.225(7) yes Ni2 S6 . . 2.220(6) yes Ni2 S5 . . 2.212(7) yes Ni2 S2 . . 2.210(7) yes Ni3 S2 . . 2.233(7) yes Ni3 S7 . . 2.227(7) yes Ni3 S8 . . 2.214(7) yes Ni3 S3 . . 2.210(7) yes Ni1 S1 . . 2.204(8) yes Ni1 S9 . . 2.198(7) yes Ni1 S4 . . 2.204(6) yes Ni1 S3 . . 2.208(7) yes P1 S1 . . 2.188(9) yes P1 S5 . . 2.053(9) yes P1 S10 . . 1.887(8) yes P1 S4 . . 2.055(8) yes P2 S6 . . 2.054(9) yes P2 S2 . . 2.097(8) yes P2 S11 . . 1.944(8) yes P2 S7 . . 2.044(9) yes P3 S12 . . 1.931(8) yes P3 S9 . . 2.060(9) yes P3 S8 . . 2.044(9) yes P3 S3 . . 2.136(9) yes 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 Ni2 S6 . . . 179.3(3) yes S1 Ni2 S5 . . . 87.3(3) yes S1 Ni2 S2 . . . 94.2(3) yes S6 Ni2 S5 . . . 92.0(2) yes S6 Ni2 S2 . . . 86.5(2) yes S5 Ni2 S2 . . . 178.2(3) yes S2 Ni3 S7 . . . 87.4(2) yes S2 Ni3 S8 . . . 178.2(3) yes S2 Ni3 S3 . . . 92.3(2) yes S7 Ni3 S8 . . . 93.2(3) yes S7 Ni3 S3 . . . 179.4(3) yes S8 Ni3 S3 . . . 87.1(3) yes S1 Ni1 S9 . . . 178.3(3) yes S1 Ni1 S4 . . . 87.7(3) yes S1 Ni1 S3 . . . 93.5(3) yes S9 Ni1 S4 . . . 91.0(2) yes S9 Ni1 S3 . . . 87.9(2) yes S4 Ni1 S3 . . . 176.6(2) yes S1 P1 S5 . . . 92.3(3) yes S1 P1 S10 . . . 125.3(5) yes S1 P1 S4 . . . 92.0(3) yes S5 P1 S10 . . . 114.5(4) yes S5 P1 S4 . . . 113.8(4) yes S10 P1 S4 . . . 115.6(4) yes S6 P2 S2 . . . 94.0(3) yes S6 P2 S11 . . . 114.6(4) yes S6 P2 S7 . . . 114.1(4) yes S2 P2 S11 . . . 120.0(5) yes S2 P2 S7 . . . 96.1(3) yes S11 P2 S7 . . . 115.2(4) yes S12 P3 S9 . . . 115.6(4) yes S12 P3 S8 . . . 116.7(4) yes S12 P3 S3 . . . 119.8(5) yes S9 P3 S8 . . . 113.6(4) yes S9 P3 S3 . . . 93.6(3) yes S8 P3 S3 . . . 93.6(3) yes #======================================================================= data_KNiPS4_cryp_hex #(II).cifdata _database_code_CSD 185896 _cell_length_a 18.296(2) _cell_length_b 29.174(2) _cell_length_c 13.5323(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7222.9(12) _cell_measurement_pressure ? _cell_measurement_radiation ? _cell_measurement_reflns_used ? _cell_measurement_temperature ? _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_measurement_wavelength ? _cell_formula_units_Z 4 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_versus_stol_list K 0 0.201 0.249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 19.000 18.204 16.733 15.243 13.728 12.268 10.977 9.908 9.061 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 8.403 7.889 7.474 7.125 6.814 6.523 6.241 5.961 5.684 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 5.406 5.130 4.859 4.594 4.337 4.090 3.855 3.632 3.423 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 3.227 3.045 2.877 2.722 2.580 2.450 2.330 2.221 2.123 ; C 0 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 6.000 5.749 5.107 4.311 3.560 2.949 2.494 2.171 1.948 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 1.794 1.685 1.603 1.537 1.479 1.426 1.374 1.322 1.271 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.219 1.166 1.114 1.063 1.012 0.962 0.914 0.867 0.822 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.778 0.736 0.697 0.659 0.622 0.588 0.556 0.525 0.495 ; H 0 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 1.000 0.960 0.854 0.713 0.568 0.438 0.331 0.248 0.184 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 0.138 0.103 0.078 0.060 0.046 0.036 0.028 0.022 0.018 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 0.014 0.011 0.009 0.007 0.006 0.005 0.004 0.004 0.003 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.003 0.002 0.002 0.002 0.002 0.002 0.001 0.001 0.000 ; N 0 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 7.000 6.776 6.180 5.385 4.563 3.825 3.219 2.747 2.393 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 2.132 1.942 1.802 1.697 1.616 1.551 1.496 1.445 1.398 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.353 1.309 1.265 1.221 1.177 1.133 1.090 1.047 1.004 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 0.962 0.921 0.882 0.843 0.805 0.769 0.734 0.700 0.667 ; Ni 0 0.339 1.112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 28.000 27.356 25.807 23.973 22.150 20.390 18.696 17.084 15.576 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 14.196 12.956 11.862 10.909 10.090 9.392 8.802 8.301 7.879 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 7.519 7.212 6.944 6.708 6.495 6.301 6.118 5.944 5.776 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 5.612 5.451 5.292 5.133 4.975 4.819 4.664 4.511 4.360 ; P 0 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 15.000 14.458 13.138 11.629 10.327 9.335 8.600 8.029 7.547 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 7.103 6.674 6.250 5.829 5.418 5.020 4.640 4.284 3.953 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 3.649 3.372 3.122 2.898 2.698 2.521 2.364 2.226 2.104 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.997 1.903 1.820 1.747 1.683 1.626 1.575 1.530 1.490 ; S 0 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 16.000 15.484 14.177 12.583 11.109 9.927 9.039 8.376 7.856 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 7.417 7.017 6.633 6.254 5.877 5.505 5.141 4.790 4.454 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 4.138 3.842 3.570 3.320 3.092 2.885 2.699 2.533 2.384 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 2.251 2.133 2.028 1.935 1.853 1.779 1.713 1.655 1.604 ; O 0 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 8.000 7.798 7.245 6.472 5.623 4.808 4.089 3.489 3.006 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 2.629 2.338 2.115 1.946 1.816 1.714 1.635 1.568 1.512 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 1.463 1.419 1.377 1.337 1.298 1.259 1.221 1.183 1.145 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.107 1.070 1.033 0.997 0.961 0.926 0.891 0.857 0.824 ; _chemical_formula_sum 'K2 C45 H94 N5 Ni3 P3 S12 O12' _chemical_formula_weight 1629.2 _exptl_crystal_colour ? _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_meas ? _exptl_crystal_density_meas_temp ? _exptl_crystal_density_method ? _exptl_crystal_F_000 3368 _exptl_absorpt_correction_type none _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 1.000 _diffrn_measurement_device ? _diffrn_measurement_device_type unknown _diffrn_measurement_method ? _diffrn_radiation_probe 'X-ray' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_index_m_1_min ? _diffrn_reflns_limit_index_m_1_max ? _diffrn_reflns_limit_index_m_2_min ? _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _reflns_limit_index_m_1_min ? _reflns_limit_index_m_1_max ? _reflns_limit_index_m_2_min ? _diffrn_reflns_number 10801 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 23.94 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2160 _reflns_observed_criterion 2 _reflns_number_total 10801 _reflns_number_observed 5029 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.001024I^2^)' _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_gt 0.0836 _refine_ls_R_factor_all 0.1321 _refine_ls_wR_factor_ref 0.1049 _refine_ls_number_reflns 10801 _refine_ls_number_parameters 546 _refine_ls_goodness_of_fit_ref 0.77 _refine_ls_goodness_of_fit_obs 0.93 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0004 _refine_diff_density_max 1.83 _refine_diff_density_min -2.32 _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic' _refine_ls_extinction_coef 0.25(10) loop_ _atom_site_label _atom_site_type_symbol _atom_site_adp_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy Ni1 Ni Uani 0.43381(6) 0.58738(5) 0.72940(9) 0.0345(5) 4 1 Ni2 Ni Uani 0.48723(6) 0.48301(5) 0.67979(9) 0.0357(5) 4 1 Ni3 Ni Uani 0.44788(6) 0.55017(5) 0.49758(10) 0.0365(5) 4 1 P1 P Uani 0.46727(12) 0.51778(11) 0.8855(2) 0.0371(10) 4 1 P2 P Uani 0.49095(14) 0.45185(11) 0.4691(2) 0.0439(11) 4 1 P3 P Uani 0.38453(13) 0.64151(11) 0.5530(2) 0.0434(12) 4 1 S1 S Uani 0.52796(11) 0.54238(9) 0.76441(18) 0.0331(9) 4 1 S2 S Uani 0.54167(12) 0.50768(10) 0.5436(2) 0.0368(10) 4 1 S3 S Uani 0.48442(12) 0.60903(10) 0.5887(2) 0.0368(10) 4 1 S4 S Uani 0.38747(13) 0.56740(10) 0.8753(2) 0.0413(11) 4 1 S5 S Uani 0.43699(14) 0.45790(10) 0.8180(2) 0.0425(11) 4 1 S6 S Uani 0.45057(14) 0.42193(10) 0.5963(2) 0.0428(11) 4 1 S7 S Uani 0.41483(14) 0.49268(11) 0.4020(2) 0.0478(12) 4 1 S8 S Uani 0.35271(13) 0.59198(11) 0.4543(2) 0.0463(12) 4 1 S9 S Uani 0.34016(12) 0.63248(10) 0.6912(2) 0.0405(11) 4 1 S10 S Uani 0.51498(14) 0.51183(11) 1.0127(2) 0.0471(11) 4 1 S11 S Uani 0.55010(16) 0.41259(12) 0.3850(2) 0.0593(12) 4 1 S12 S Uani 0.38655(14) 0.70432(11) 0.5035(2) 0.0570(13) 4 1 N' N Uani 0.2075(4) 0.5066(3) 0.6378(7) 0.050(4) 4 1 C1' C Uani -0.0816(6) 0.6368(5) 0.4800(12) 0.097(7) 4 1 C2' C Uani -0.0351(7) 0.6617(5) 0.5608(10) 0.082(6) 4 1 C3' C Uani 0.0081(8) 0.6305(4) 0.6244(10) 0.078(6) 4 1 C4' C Uani 0.0746(7) 0.6085(5) 0.5794(9) 0.074(6) 4 1 C5' C Uani 0.1128(7) 0.5720(4) 0.6465(8) 0.064(5) 4 1 C6' C Uani 0.1701(6) 0.5473(4) 0.5881(8) 0.056(5) 4 1 C7' C Uani 0.1532(5) 0.4685(4) 0.6656(8) 0.054(5) 4 1 C8' C Uani 0.2477(5) 0.5216(4) 0.7274(8) 0.061(5) 4 1 C9' C Uani 0.2602(5) 0.4875(5) 0.5641(9) 0.078(6) 4 1 K1 K Uani 0.34254(12) 0.25258(9) 0.61508(18) 0.0475(10) 4 1 K2 K Uani 0.78917(11) 0.36579(9) 0.83686(17) 0.0446(10) 4 1 N1a N Uani 0.2263(4) 0.3173(4) 0.6696(8) 0.067(4) 4 1 N2a N Uani 0.4571(5) 0.1876(3) 0.5584(8) 0.063(4) 4 1 N1b N Uani 0.8325(4) 0.2700(3) 0.8804(7) 0.051(4) 4 1 N2b N Uani 0.7461(4) 0.4614(3) 0.8032(7) 0.053(4) 4 1 C1e C Uani 0.2194(6) 0.3537(4) 0.5962(11) 0.075(6) 4 1 C2e C Uani 0.2405(6) 0.3453(5) 0.4972(11) 0.085(6) 4 1 C3e C Uani 0.3521(7) 0.3364(4) 0.4073(8) 0.067(6) 4 1 C4e C Uani 0.4238(6) 0.3131(4) 0.4184(10) 0.077(6) 4 1 C5e C Uani 0.4831(5) 0.2420(4) 0.4231(9) 0.064(5) 4 1 C6e C Uani 0.4696(6) 0.1931(5) 0.4541(12) 0.075(6) 4 1 O1e O Uani 0.3115(3) 0.3254(2) 0.4963(5) 0.063(3) 4 1 O2e O Uani 0.4127(3) 0.2645(3) 0.4346(4) 0.060(3) 4 1 C1f C Uani 0.8440(6) 0.2638(4) 0.9847(9) 0.068(5) 4 1 C2f C Uani 0.7876(6) 0.2824(4) 1.0498(9) 0.070(6) 4 1 C3f C Uani 0.8150(8) 0.3626(7) 1.0834(9) 0.119(10) 4 1 C4f C Uani 0.7795(7) 0.4061(5) 1.0884(8) 0.078(7) 4 1 C5f C Uani 0.7290(7) 0.4658(3) 0.9878(11) 0.083(6) 4 1 C6f C Uani 0.6988(6) 0.4738(4) 0.8878(11) 0.073(6) 4 1 O1f O Uani 0.7736(5) 0.3302(3) 1.0307(6) 0.098(4) 4 1 O2f O Uani 0.7552(4) 0.4192(3) 0.9918(5) 0.069(3) 4 1 H1c2' H Uiso 0.000299 0.683009 0.528264 0.095(5) 4 1 H2c2' H Uiso -0.068158 0.679524 0.605332 0.095(5) 4 1 H1c3' H Uiso -0.025453 0.605377 0.646303 0.095(5) 4 1 H2c3' H Uiso 0.024352 0.648574 0.683117 0.095(5) 4 1 H1c4' H Uiso 0.110073 0.633661 0.564421 0.095(5) 4 1 H2c4' H Uiso 0.058784 0.59362 0.516439 0.095(5) 4 1 H1c5' H Uiso 0.136801 0.587187 0.704253 0.095(5) 4 1 H2c5' H Uiso 0.07633 0.54907 0.670706 0.095(5) 4 1 H1c6' H Uiso 0.208482 0.570358 0.570929 0.095(5) 4 1 H2c6' H Uiso 0.146069 0.536119 0.526283 0.095(5) 4 1 H1c1e H Uiso 0.252506 0.380658 0.619722 0.095(5) 4 1 H2c1e H Uiso 0.167837 0.366221 0.597598 0.095(5) 4 1 H1c2e H Uiso 0.204091 0.321904 0.464861 0.095(5) 4 1 H2c2e H Uiso 0.239073 0.37306 0.452118 0.095(5) 4 1 H1c3e H Uiso 0.355927 0.371427 0.399609 0.095(5) 4 1 H2c3e H Uiso 0.323699 0.32563 0.345614 0.095(5) 4 1 H1c4e H Uiso 0.455928 0.316949 0.356963 0.095(5) 4 1 H2c4e H Uiso 0.452114 0.326201 0.475865 0.095(5) 4 1 H1c5e H Uiso 0.520838 0.257254 0.468723 0.095(5) 4 1 H2c5e H Uiso 0.502028 0.246325 0.353137 0.095(5) 4 1 H1c6e H Uiso 0.425738 0.182288 0.412821 0.095(5) 4 1 H2c6e H Uiso 0.513144 0.174235 0.430027 0.095(5) 4 1 H1c1f H Uiso 0.892595 0.278834 1.004767 0.095(5) 4 1 H2c1f H Uiso 0.850104 0.229658 1.000022 0.095(5) 4 1 H1c2f H Uiso 0.740128 0.264879 1.040519 0.095(5) 4 1 H2c2f H Uiso 0.801202 0.278803 1.123242 0.095(5) 4 1 H1c3f H Uiso 0.864769 0.366304 1.048607 0.095(5) 4 1 H2c3f H Uiso 0.826155 0.350272 1.151768 0.095(5) 4 1 H1c4f H Uiso 0.73739 0.404692 1.136267 0.095(5) 4 1 H2c4f H Uiso 0.814922 0.430717 1.115611 0.095(5) 4 1 H1c5f H Uiso 0.771315 0.487094 1.000636 0.095(5) 4 1 H2c5f H Uiso 0.691974 0.470251 1.042316 0.095(5) 4 1 H1c6f H Uiso 0.683657 0.507698 0.884334 0.095(5) 4 1 H2c6f H Uiso 0.650201 0.455805 0.884086 0.095(5) 4 1 C1a C Uani 0.2381(4) 0.3335(3) 0.7691(7) 0.078(3) 4 1 C2a C Uani 0.3151(6) 0.3476(4) 0.7826(13) 0.073(3) 4 1 C3a C Uani 0.4351(7) 0.3197(6) 0.8015(16) 0.068(3) 4 1 C4a C Uani 0.4789(7) 0.2775(7) 0.8074(16) 0.068(2) 4 1 C5a C Uani 0.5204(9) 0.2145(8) 0.7148(19) 0.076(3) 4 1 C6a C Uani 0.5253(11) 0.1968(9) 0.612(2) 0.065(2) 4 1 O1a O Uani 0.3616(6) 0.3078(5) 0.7842(11) 0.0651(18) 4 1 O2a O Uani 0.4768(7) 0.2550(7) 0.7144(15) 0.0629(17) 4 1 H1c1a H Uiso 0.2251(4) 0.3077(3) 0.8145(7) 0.095(5) 4 1 H2c1a H Uiso 0.2054(4) 0.3602(3) 0.7826(7) 0.095(5) 4 1 H1c2a H Uiso 0.3313(4) 0.3680(3) 0.7311(7) 0.095(5) 4 1 H2c2a H Uiso 0.3201(4) 0.3627(3) 0.8503(7) 0.095(5) 4 1 H1c3a H Uiso 0.4371(4) 0.3347(3) 0.8690(7) 0.095(5) 4 1 H2c3a H Uiso 0.4528(4) 0.3386(3) 0.7505(7) 0.095(5) 4 1 H1c4a H Uiso 0.5296(4) 0.2826(3) 0.8264(7) 0.095(5) 4 1 H2c4a H Uiso 0.4565(4) 0.2540(3) 0.8580(7) 0.095(5) 4 1 H1c5a H Uiso 0.4954(4) 0.1902(3) 0.7545(7) 0.095(5) 4 1 H2c5a H Uiso 0.5690(4) 0.2211(3) 0.7394(7) 0.095(5) 4 1 H1c6a H Uiso 0.5536(4) 0.2210(3) 0.5701(7) 0.095(5) 4 1 H2c6a H Uiso 0.5526(4) 0.1680(3) 0.6085(7) 0.095(5) 4 1 C1b C Uani 0.1556(4) 0.2936(3) 0.6746(8) 0.078(3) 4 1 C2b C Uani 0.1546(8) 0.2463(4) 0.7135(12) 0.073(3) 4 1 C3b C Uani 0.1963(10) 0.1711(4) 0.6841(15) 0.068(3) 4 1 C4b C Uani 0.2389(11) 0.1427(5) 0.6152(16) 0.068(3) 4 1 C5b C Uani 0.3577(13) 0.1291(6) 0.5561(18) 0.076(3) 4 1 C6b C Uani 0.4359(14) 0.1405(7) 0.575(2) 0.065(2) 4 1 O1b O Uani 0.1985(7) 0.2170(4) 0.6520(11) 0.0651(18) 4 1 O2b O Uani 0.3132(10) 0.1566(5) 0.6192(15) 0.0629(18) 4 1 H1c1b H Uiso 0.1467(4) 0.2940(3) 0.6016(8) 0.095(5) 4 1 H2c1b H Uiso 0.1169(4) 0.3121(3) 0.7085(8) 0.095(5) 4 1 H1c2b H Uiso 0.1725(4) 0.2447(3) 0.7805(8) 0.095(5) 4 1 H2c2b H Uiso 0.1024(4) 0.2341(3) 0.7094(8) 0.095(5) 4 1 H1c3b H Uiso 0.1436(4) 0.1607(3) 0.6789(8) 0.095(5) 4 1 H2c3b H Uiso 0.2155(4) 0.1685(3) 0.7483(8) 0.095(5) 4 1 H1c4b H Uiso 0.2357(4) 0.1100(3) 0.6284(8) 0.095(5) 4 1 H2c4b H Uiso 0.2226(4) 0.1480(3) 0.5416(8) 0.095(5) 4 1 H1c5b H Uiso 0.3480(4) 0.1375(3) 0.4855(8) 0.095(5) 4 1 H2c5b H Uiso 0.3494(4) 0.0969(3) 0.5685(8) 0.095(5) 4 1 H1c6b H Uiso 0.4476(4) 0.1304(3) 0.6476(8) 0.095(5) 4 1 H2c6b H Uiso 0.4687(4) 0.1236(3) 0.5313(8) 0.095(5) 4 1 C1c C Uani 0.7745(5) 0.2388(2) 0.8435(7) 0.078(3) 4 1 C2c C Uani 0.7458(9) 0.2506(4) 0.7446(10) 0.073(3) 4 1 C3c C Uani 0.6779(11) 0.3057(6) 0.6564(12) 0.068(3) 4 1 C4c C Uani 0.6379(11) 0.3492(6) 0.6665(13) 0.068(3) 4 1 C5c C Uani 0.6531(13) 0.4278(7) 0.6974(15) 0.076(3) 4 1 C6c C Uani 0.7101(15) 0.4641(8) 0.7063(18) 0.065(2) 4 1 O1c O Uani 0.7090(7) 0.2942(4) 0.7482(10) 0.0651(18) 4 1 O2c O Uani 0.6885(10) 0.3845(6) 0.6899(12) 0.0629(18) 4 1 H1c1c H Uiso 0.7366(5) 0.2437(2) 0.8957(7) 0.095(5) 4 1 H2c1c H Uiso 0.7903(5) 0.2060(2) 0.8439(7) 0.095(5) 4 1 H1c2c H Uiso 0.7839(5) 0.2519(2) 0.6956(7) 0.095(5) 4 1 H2c2c H Uiso 0.7072(5) 0.2269(2) 0.7255(7) 0.095(5) 4 1 H1c3c H Uiso 0.6404(5) 0.2811(2) 0.6406(7) 0.095(5) 4 1 H2c3c H Uiso 0.7144(5) 0.3085(2) 0.6078(7) 0.095(5) 4 1 H1c4c H Uiso 0.6104(5) 0.3578(2) 0.6078(7) 0.095(5) 4 1 H2c4c H Uiso 0.6011(5) 0.3482(2) 0.7260(7) 0.095(5) 4 1 H1c5c H Uiso 0.6238(5) 0.4290(2) 0.7599(7) 0.095(5) 4 1 H2c5c H Uiso 0.6232(5) 0.4336(2) 0.6396(7) 0.095(5) 4 1 H1c6c H Uiso 0.7394(5) 0.4645(2) 0.6402(7) 0.095(5) 4 1 H2c6c H Uiso 0.6884(5) 0.4945(2) 0.7152(7) 0.095(5) 4 1 C1d C Uani 0.9003(4) 0.2611(2) 0.8215(8) 0.078(3) 4 1 C2d C Uani 0.9562(7) 0.2972(4) 0.8343(13) 0.073(3) 4 1 C3d C Uani 0.9858(10) 0.3735(4) 0.7941(16) 0.068(3) 4 1 C4d C Uani 0.9599(11) 0.4142(5) 0.7405(16) 0.068(3) 4 1 C5d C Uani 0.8701(12) 0.4718(6) 0.7411(19) 0.076(3) 4 1 C6d C Uani 0.8110(14) 0.4919(7) 0.803(2) 0.065(2) 4 1 O1d O Uani 0.9325(7) 0.3389(4) 0.7875(11) 0.0651(18) 4 1 O2d O Uani 0.8964(10) 0.4313(5) 0.7881(15) 0.0629(18) 4 1 H1c1d H Uiso 0.8831(4) 0.2596(2) 0.7514(8) 0.095(5) 4 1 H2c1d H Uiso 0.9213(4) 0.2308(2) 0.8411(8) 0.095(5) 4 1 H1c2d H Uiso 0.9662(4) 0.3032(2) 0.9030(8) 0.095(5) 4 1 H2c2d H Uiso 1.0027(4) 0.2871(2) 0.7985(8) 0.095(5) 4 1 H1c3d H Uiso 1.0307(4) 0.3619(2) 0.7580(8) 0.095(5) 4 1 H2c3d H Uiso 0.9950(4) 0.3810(2) 0.8607(8) 0.095(5) 4 1 H1c4d H Uiso 0.9961(4) 0.4386(2) 0.7356(8) 0.095(5) 4 1 H2c4d H Uiso 0.9434(4) 0.4060(2) 0.6683(8) 0.095(5) 4 1 H1c5d H Uiso 0.8470(4) 0.4635(2) 0.6764(8) 0.095(5) 4 1 H2c5d H Uiso 0.9092(4) 0.4939(2) 0.7332(8) 0.095(5) 4 1 H1c6d H Uiso 0.8347(4) 0.5022(2) 0.8698(8) 0.095(5) 4 1 H2c6d H Uiso 0.7893(4) 0.5190(2) 0.7724(8) 0.095(5) 4 1 loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_adp_type _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 Ni1 Ni Uani 0.0287(7) 0.0334(10) 0.0415(9) 0.0020(6) 0.0003(6) 0.0024(7) Ni2 Ni Uani 0.0349(7) 0.0353(10) 0.0367(8) 0.0007(6) -0.0010(6) 0.0031(7) Ni3 Ni Uani 0.0320(6) 0.0363(10) 0.0411(8) 0.0029(6) -0.0006(6) 0.0019(7) P1 P Uani 0.0337(15) 0.038(2) 0.0402(17) -0.0024(14) -0.0033(13) 0.0020(16) P2 P Uani 0.0421(15) 0.047(2) 0.0428(19) 0.0026(15) 0.0019(13) -0.0011(16) P3 P Uani 0.0295(15) 0.047(2) 0.054(2) 0.0051(15) 0.0021(14) 0.0054(17) S1 S Uani 0.0314(14) 0.031(2) 0.0371(16) 0.0003(12) -0.0061(12) -0.0006(14) S2 S Uani 0.0341(14) 0.034(2) 0.0423(16) 0.0051(12) 0.0030(12) 0.0023(14) S3 S Uani 0.0301(13) 0.033(2) 0.0470(19) 0.0058(13) 0.0029(13) 0.0028(14) S4 S Uani 0.0322(14) 0.048(2) 0.0437(18) 0.0042(14) 0.0007(13) 0.0009(15) S5 S Uani 0.0570(17) 0.037(2) 0.0332(16) -0.0086(14) 0.0055(14) -0.0004(15) S6 S Uani 0.0535(16) 0.034(2) 0.0414(18) -0.0077(15) -0.0022(14) -0.0040(15) S7 S Uani 0.0509(18) 0.049(2) 0.0435(18) 0.0018(15) -0.0094(14) -0.0037(17) S8 S Uani 0.0357(14) 0.054(2) 0.050(2) 0.0050(14) -0.0049(13) 0.0068(17) S9 S Uani 0.0338(14) 0.033(2) 0.054(2) 0.0051(13) 0.0047(13) 0.0038(16) S10 S Uani 0.0506(15) 0.058(2) 0.0332(16) -0.0033(15) -0.0063(14) 0.0026(16) S11 S Uani 0.0606(18) 0.047(2) 0.070(2) 0.0043(17) 0.0133(17) -0.0123(19) S12 S Uani 0.0480(16) 0.048(2) 0.075(2) 0.0134(15) 0.0154(18) 0.023(2) N' N Uani 0.058(6) 0.027(7) 0.065(7) -0.008(5) 0.004(5) -0.001(5) C1' C Uani 0.052(7) 0.105(15) 0.134(14) -0.026(7) -0.017(8) -0.040(11) C2' C Uani 0.104(11) 0.059(12) 0.084(10) 0.000(8) 0.029(9) 0.034(8) C3' C Uani 0.118(11) 0.032(10) 0.083(10) 0.006(8) 0.010(9) 0.019(8) C4' C Uani 0.124(12) 0.040(11) 0.059(9) 0.005(8) 0.013(8) 0.016(7) C5' C Uani 0.103(9) 0.031(10) 0.058(9) -0.026(7) 0.030(8) -0.013(7) C6' C Uani 0.055(7) 0.058(11) 0.055(8) -0.040(7) -0.009(6) 0.008(7) C7' C Uani 0.035(5) 0.057(10) 0.069(9) -0.027(5) 0.009(5) -0.008(7) C8' C Uani 0.048(6) 0.085(11) 0.050(7) -0.029(6) -0.036(6) 0.009(7) C9' C Uani 0.048(7) 0.090(12) 0.095(10) -0.011(7) 0.063(7) -0.015(9) K1 K Uani 0.0452(14) 0.038(2) 0.0596(18) 0.0052(12) -0.0039(12) -0.0015(15) K2 K Uani 0.0362(12) 0.042(2) 0.0556(18) 0.0022(11) 0.0014(12) 0.0053(14) N1a N Uani 0.045(5) 0.086(10) 0.072(8) 0.006(5) 0.007(5) 0.003(7) N2a N Uani 0.056(6) 0.052(8) 0.081(8) -0.005(5) -0.016(6) 0.002(6) N1b N Uani 0.056(5) 0.050(8) 0.048(6) 0.001(5) -0.009(5) 0.020(5) N2b N Uani 0.058(5) 0.035(7) 0.066(7) 0.000(4) 0.006(5) 0.014(5) C1e C Uani 0.082(9) 0.052(11) 0.091(11) 0.054(8) 0.016(8) 0.027(9) C2e C Uani 0.085(9) 0.084(13) 0.086(11) 0.030(8) 0.004(9) 0.023(10) C3e C Uani 0.096(10) 0.052(11) 0.054(9) -0.001(8) 0.005(8) 0.011(7) C4e C Uani 0.066(9) 0.081(14) 0.084(11) -0.010(8) 0.014(8) -0.003(9) C5e C Uani 0.043(6) 0.074(12) 0.075(9) -0.010(7) 0.015(6) 0.011(8) C6e C Uani 0.057(8) 0.072(13) 0.097(12) 0.007(7) 0.014(8) -0.031(10) O1e O Uani 0.066(5) 0.057(6) 0.067(6) 0.013(4) -0.004(5) 0.019(5) O2e O Uani 0.063(5) 0.042(7) 0.075(6) 0.000(4) -0.005(4) 0.003(5) C1f C Uani 0.093(9) 0.071(11) 0.040(8) 0.027(8) 0.008(7) 0.023(7) C2f C Uani 0.082(9) 0.064(13) 0.065(9) 0.010(8) 0.001(7) -0.001(8) C3f C Uani 0.105(12) 0.23(2) 0.021(8) -0.037(15) -0.041(8) 0.020(12) C4f C Uani 0.072(9) 0.062(13) 0.099(13) 0.015(8) 0.013(9) -0.009(10) C5f C Uani 0.108(10) 0.036(11) 0.104(13) 0.014(8) 0.064(10) -0.011(9) C6f C Uani 0.090(10) 0.052(12) 0.077(10) 0.017(7) 0.005(8) 0.027(8) O1f O Uani 0.148(8) 0.023(7) 0.121(9) 0.017(6) -0.039(7) 0.022(6) O2f O Uani 0.092(6) 0.067(8) 0.049(6) 0.001(5) 0.000(5) 0.008(5) C1a C Uani 0.085(5) 0.059(4) 0.089(5) 0.018(4) 0.004(4) -0.027(4) C2a C Uani 0.065(5) 0.066(5) 0.088(5) -0.005(4) 0.014(4) -0.033(4) C3a C Uani 0.047(4) 0.086(5) 0.070(4) -0.006(4) 0.000(3) -0.013(4) C4a C Uani 0.049(4) 0.092(5) 0.063(4) 0.003(4) -0.023(3) -0.010(4) C5a C Uani 0.060(4) 0.087(5) 0.081(5) 0.043(4) -0.019(4) -0.010(4) C6a C Uani 0.036(4) 0.065(4) 0.095(5) 0.019(3) -0.007(3) -0.023(4) O1a O Uani 0.044(2) 0.064(3) 0.087(3) 0.003(2) 0.000(2) -0.017(2) O2a O Uani 0.054(2) 0.079(3) 0.055(2) 0.007(2) -0.013(2) -0.014(2) C1b C Uani 0.051(5) 0.087(5) 0.094(5) 0.010(4) 0.025(3) -0.005(4) C2b C Uani 0.048(5) 0.077(5) 0.094(5) 0.009(4) 0.019(3) 0.023(4) C3b C Uani 0.064(5) 0.050(4) 0.090(5) 0.000(3) -0.003(3) 0.013(4) C4b C Uani 0.070(5) 0.036(4) 0.097(5) -0.013(3) -0.003(3) -0.005(3) C5b C Uani 0.069(5) 0.049(4) 0.111(5) 0.012(4) 0.011(4) -0.036(4) C6b C Uani 0.062(5) 0.036(4) 0.097(5) 0.016(3) 0.025(3) -0.002(3) O1b O Uani 0.063(3) 0.049(3) 0.084(3) 0.010(2) 0.016(2) 0.009(2) O2b O Uani 0.053(3) 0.046(2) 0.089(3) -0.008(2) 0.000(2) -0.006(2) C1c C Uani 0.099(5) 0.039(5) 0.095(5) 0.000(4) -0.008(4) -0.011(3) C2c C Uani 0.111(5) 0.046(5) 0.062(5) -0.014(4) -0.011(4) -0.003(3) C3c C Uani 0.078(5) 0.068(5) 0.058(5) -0.008(3) -0.017(3) 0.012(3) C4c C Uani 0.054(4) 0.077(5) 0.072(5) -0.001(3) -0.030(3) 0.008(3) C5c C Uani 0.064(5) 0.048(5) 0.117(5) 0.021(4) -0.027(4) 0.012(3) C6c C Uani 0.089(5) 0.038(5) 0.069(4) 0.016(3) -0.029(3) 0.007(3) O1c O Uani 0.088(3) 0.050(3) 0.057(3) 0.006(2) -0.017(2) 0.004(2) O2c O Uani 0.055(3) 0.059(3) 0.074(3) -0.006(2) -0.022(2) 0.004(2) C1d C Uani 0.066(5) 0.062(5) 0.105(5) 0.026(4) -0.001(4) 0.007(4) C2d C Uani 0.051(5) 0.059(5) 0.110(5) 0.012(4) -0.007(3) -0.016(4) C3d C Uani 0.059(5) 0.056(5) 0.088(5) -0.012(3) 0.008(3) -0.010(3) C4d C Uani 0.058(5) 0.062(4) 0.084(5) -0.018(3) 0.023(3) 0.009(3) C5d C Uani 0.091(5) 0.040(5) 0.098(5) 0.006(3) 0.024(4) 0.031(4) C6d C Uani 0.059(5) 0.029(4) 0.108(5) -0.001(3) 0.000(3) 0.014(3) O1d O Uani 0.056(3) 0.044(3) 0.095(3) -0.003(2) -0.005(2) 0.001(2) O2d O Uani 0.054(3) 0.056(3) 0.078(3) -0.004(2) 0.020(2) 0.005(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni1 P1 2.993(3) . . Ni1 S1 2.217(2) . . Ni1 S3 2.209(2) . . Ni1 S4 2.226(3) . . Ni1 S9 2.221(2) . . Ni2 P1 2.986(3) . . Ni2 P2 2.993(3) . . Ni2 S1 2.206(3) . . Ni2 S2 2.215(2) . . Ni2 S5 2.209(3) . . Ni2 S6 2.214(3) . . Ni2 H2c5c 2.927(9) . . Ni3 P2 2.999(3) . . Ni3 S2 2.206(2) . . Ni3 S3 2.217(3) . . Ni3 S7 2.203(3) . . Ni3 S8 2.205(3) . . Ni3 H2c3d 2.926(9) . 2_664 P1 Ni1 2.993(3) . . P1 Ni2 2.986(3) . . P1 S1 2.106(3) . . P1 S4 2.061(4) . . P1 S5 2.048(4) . . P1 S10 1.937(3) . . P2 Ni2 2.993(3) . . P2 Ni3 2.999(3) . . P2 S2 2.128(4) . . P2 S6 2.066(4) . . P2 S7 2.045(4) . . P2 S11 1.944(4) . . P3 S3 2.115(3) . . P3 S8 2.052(4) . . P3 S9 2.056(4) . . P3 S12 1.951(4) . . C2' C1' 1.56(2) . . C2' C3' 1.48(2) . . C2' C4' 2.55(2) . . C2' H1c2' 0.999(14) . . C2' H2c2' 1.000(14) . . C2' H1c3' 2.018(14) . . C2' H2c3' 2.017(14) . . C2' H1c4' 2.779(14) . . C2' H2c4' 2.693(14) . . C3' C1' 2.56(2) . . C3' C2' 1.48(2) . . C3' C4' 1.50(2) . . C3' C5' 2.58(2) . . C3' H1c2' 2.016(14) . . C3' H2c2' 2.015(14) . . C3' H1c3' 1.000(14) . . C3' H2c3' 0.999(14) . . C3' H1c4' 2.037(14) . . C3' H2c4' 2.038(14) . . C3' H1c5' 2.883(14) . . C3' H2c5' 2.755(14) . . C4' C2' 2.55(2) . . C4' C3' 1.50(2) . . C4' C5' 1.563(18) . . C4' C6' 2.501(19) . . C4' H1c2' 2.655(14) . . C4' H1c3' 2.044(14) . . C4' H2c3' 2.045(13) . . C4' H1c4' 1.001(14) . . C4' H2c4' 0.999(13) . . C4' H1c5' 2.130(13) . . C4' H2c5' 2.129(13) . . C4' H1c6' 2.693(14) . . C4' H2c6' 2.586(14) . . C5' N' 2.581(16) . . C5' C3' 2.58(2) . . C5' C4' 1.563(18) . . C5' C6' 1.498(17) . . C5' H1c3' 2.710(13) . . C5' H2c3' 2.802(13) . . C5' H1c4' 2.114(12) . . C5' H2c4' 2.114(12) . . C5' H1c5' 1.000(12) . . C5' H2c5' 1.000(13) . . C5' H1c6' 2.028(13) . . C5' H2c6' 2.028(12) . . 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_2 _geom_angle_site_symmetry_3 P1 Ni1 S1 44.65(8) . . . P1 Ni1 S3 135.76(10) . . . P1 Ni1 S4 43.49(9) . . . P1 Ni1 S9 136.37(10) . . . S1 Ni1 S3 91.59(10) . . . S1 Ni1 S4 87.21(11) . . . S1 Ni1 S9 178.86(12) . . . S3 Ni1 S4 177.04(12) . . . S3 Ni1 S9 87.33(11) . . . S4 Ni1 S9 93.88(11) . . . P1 Ni2 P2 173.83(8) . . . P1 Ni2 S1 44.80(9) . . . P1 Ni2 S2 136.10(11) . . . P1 Ni2 S5 43.30(10) . . . P1 Ni2 S6 135.42(11) . . . P1 Ni2 H2c5c 116.4(2) . . . P2 Ni2 S1 136.49(11) . . . P2 Ni2 S2 45.25(10) . . . P2 Ni2 S5 135.65(11) . . . P2 Ni2 S6 43.64(10) . . . P2 Ni2 H2c5c 69.8(2) . . . S1 Ni2 S2 91.43(11) . . . S1 Ni2 S5 87.79(11) . . . S1 Ni2 S6 177.65(11) . . . S1 Ni2 H2c5c 101.30(19) . . . S2 Ni2 S5 177.87(11) . . . S2 Ni2 S6 88.46(11) . . . S2 Ni2 H2c5c 67.86(19) . . . S5 Ni2 S6 92.24(12) . . . S5 Ni2 H2c5c 110.3(2) . . . S6 Ni2 H2c5c 76.49(19) . . . P2 Ni3 S2 45.14(9) . . . P2 Ni3 S3 137.11(10) . . . P2 Ni3 S7 42.99(10) . . . P2 Ni3 S8 134.62(11) . . . P2 Ni3 H2c3d 118.79(18) . . 2_664 S2 Ni3 S3 92.50(11) . . . S2 Ni3 S7 87.21(12) . . . S2 Ni3 S8 178.74(12) . . . S2 Ni3 H2c3d 106.64(18) . . 2_664 S3 Ni3 S7 177.54(12) . . . S3 Ni3 S8 87.56(12) . . . S3 Ni3 H2c3d 73.3(2) . . 2_664 S7 Ni3 S8 92.78(12) . . . S7 Ni3 H2c3d 104.4(2) . . 2_664 S8 Ni3 H2c3d 74.58(18) . . 2_664 Ni1 P1 Ni2 66.25(7) . . . Ni1 P1 S1 47.73(9) . . . Ni1 P1 S4 48.02(10) . . . Ni1 P1 S5 102.03(13) . . . Ni1 P1 S10 141.25(18) . . . Ni2 P1 S1 47.58(10) . . . Ni2 P1 S4 105.22(13) . . . Ni2 P1 S5 47.71(10) . . . Ni2 P1 S10 137.97(15) . . . S1 P1 S4 94.69(16) . . . S1 P1 S5 94.94(16) . . . S1 P1 S10 118.97(16) . . . S4 P1 S5 112.18(16) . . . S4 P1 S10 116.23(19) . . . S5 P1 S10 116.2(2) . . . Ni2 P2 Ni3 65.25(8) . . . Ni2 P2 S2 47.67(10) . . . Ni2 P2 S6 47.69(10) . . . Ni2 P2 S7 103.34(15) . . . Ni2 P2 S11 138.54(16) . . . Ni3 P2 S2 47.30(10) . . . Ni3 P2 S6 101.72(14) . . . Ni3 P2 S7 47.25(12) . . . Ni3 P2 S11 141.71(17) . . . S2 P2 S6 94.88(16) . . . S2 P2 S7 93.52(18) . . . S2 P2 S11 119.04(17) . . . S6 P2 S7 111.87(16) . . . S6 P2 S11 116.0(2) . . . S7 P2 S11 117.52(19) . . . S3 P3 S8 94.50(17) . . . S3 P3 S9 94.34(16) . . . S3 P3 S12 118.88(17) . . . S8 P3 S9 112.95(18) . . . S8 P3 S12 116.3(2) . . . S9 P3 S12 116.1(2) . . . C1' C2' C3' 114.2(12) . . . C1' C2' C4' 102.4(9) . . . C1' C2' H1c2' 109.5(12) . . . C1' C2' H2c2' 109.5(12) . . . C1' C2' H1c3' 94.0(9) . . . C1' C2' H2c3' 141.1(10) . . . C1' C2' H1c4' 113.3(8) . . . C1' C2' H2c4' 81.3(7) . . . C3' C2' C4' 31.7(7) . . . C3' C2' H1c2' 107.1(12) . . . C3' C2' H2c2' 106.9(12) . . . C3' C2' H1c3' 28.2(6) . . . C3' C2' H2c3' 28.2(6) . . . C3' C2' H1c4' 45.6(6) . . . C3' C2' H2c4' 48.4(6) . . . C4' C2' H1c2' 85.0(9) . . . C4' C2' H2c2' 137.2(11) . . . C4' C2' H1c3' 51.6(4) . . . C4' C2' H2c3' 51.6(4) . . . C4' C2' H1c4' 21.1(3) . . . C4' C2' H2c4' 21.7(3) . . . H1c2' C2' H2c2' 109.5(13) . . . H1c2' C2' H1c3' 134.7(11) . . . H1c2' C2' H2c3' 97.5(9) . . . H1c2' C2' H1c4' 64.7(7) . . . H1c2' C2' H2c4' 87.0(8) . . . H2c2' C2' H1c3' 97.5(9) . . . H2c2' C2' H2c3' 86.0(8) . . . H2c2' C2' H1c4' 136.1(10) . . . H2c2' C2' H2c4' 154.6(11) . . . H1c3' C2' H2c3' 47.7(3) . . . H1c3' C2' H1c4' 70.5(4) . . . H1c3' C2' H2c4' 58.1(3) . . . H2c3' C2' H1c4' 54.2(3) . . . H2c3' C2' H2c4' 72.5(4) . . . H1c4' C2' H2c4' 34.68(18) . . . C1' C3' C2' 33.9(7) . . . C1' C3' C4' 103.9(9) . . . C1' C3' C5' 127.7(7) . . . C1' C3' H1c2' 53.6(4) . . . C1' C3' H2c2' 53.6(4) . . . C1' C3' H1c3' 83.5(9) . . . C1' C3' H2c3' 139.5(11) . . . C1' C3' H1c4' 106.2(6) . . . C1' C3' H2c4' 77.4(5) . . . C1' C3' H1c5' 147.3(6) . . . C1' C3' H2c5' 121.8(6) . . . C2' C3' C4' 117.2(11) . . . C2' C3' C5' 150.3(10) . . . C2' C3' H1c2' 28.3(6) . . . C2' C3' H2c2' 28.4(6) . . . C2' C3' H1c3' 107.2(12) . . . C2' C3' H2c3' 107.2(12) . . . C2' C3' H1c4' 103.2(9) . . . C2' C3' H2c4' 98.6(9) . . . C2' C3' H1c5' 157.3(10) . . . C2' C3' H2c5' 154.7(9) . . . C4' C3' C5' 33.4(6) . . . C4' C3' H1c2' 96.9(8) . . . C4' C3' H2c2' 144.2(10) . . . C4' C3' H1c3' 107.7(12) . . . C4' C3' H2c3' 107.8(12) . . . C4' C3' H1c4' 28.0(6) . . . C4' C3' H2c4' 27.9(5) . . . C4' C3' H1c5' 45.9(6) . . . C4' C3' H2c5' 50.1(6) . . . C5' C3' H1c2' 129.0(7) . . . C5' C3' H2c2' 175.9(7) . . . C5' C3' H1c3' 86.4(9) . . . C5' C3' H2c3' 92.1(9) . . . C5' C3' H1c4' 52.9(4) . . . C5' C3' H2c4' 52.9(4) . . . C5' C3' H1c5' 20.1(3) . . . C5' C3' H2c5' 21.3(3) . . . H1c2' C3' H2c2' 47.8(3) . . . H1c2' C3' H1c3' 134.8(11) . . . H1c2' C3' H2c3' 97.6(9) . . . H1c2' C3' H1c4' 76.9(5) . . . H1c2' C3' H2c4' 88.3(5) . . . H1c2' C3' H1c5' 129.2(6) . . . H1c2' C3' H2c5' 146.5(6) . . . H2c2' C3' H1c3' 97.7(10) . . . H2c2' C3' H2c3' 86.2(8) . . . H2c2' C3' H1c4' 123.4(7) . . . H2c2' C3' H2c4' 126.7(7) . . . H2c2' C3' H1c5' 157.6(6) . . . H2c2' C3' H2c5' 162.8(7) . . . H1c3' C3' H2c3' 109.5(13) . . . H1c3' C3' H1c4' 135.5(11) . . . H1c3' C3' H2c4' 96.1(9) . . . H1c3' C3' H1c5' 94.0(8) . . . H1c3' C3' H2c5' 65.1(7) . . . H2c3' C3' H1c4' 91.1(9) . . . H2c3' C3' H2c4' 135.5(12) . . . H2c3' C3' H1c5' 71.9(8) . . . H2c3' C3' H2c5' 98.0(9) . . . H1c4' C3' H2c4' 47.2(3) . . . H1c4' C3' H1c5' 54.6(3) . . . H1c4' C3' H2c5' 73.4(4) . . . H2c4' C3' H1c5' 70.5(4) . . . H2c4' C3' H2c5' 60.1(3) . . . H1c5' C3' H2c5' 33.58(17) . . . C2' C4' C3' 31.1(6) . . . C2' C4' C5' 145.4(9) . . . C2' C4' C6' 171.6(7) . . . C2' C4' H1c2' 22.0(3) . . . C2' C4' H1c3' 50.7(4) . . . C2' C4' H2c3' 50.7(4) . . . C2' C4' H1c4' 92.5(9) . . . C2' C4' H2c4' 87.3(9) . . . C2' C4' H1c5' 132.6(6) . . . C2' C4' H2c5' 124.4(7) . . . C2' C4' H1c6' 164.4(6) . . . C2' C4' H2c6' 150.2(6) . . . C3' C4' C5' 114.6(10) . . . C3' C4' C6' 148.2(9) . . . C3' C4' H1c2' 48.9(6) . . . C3' C4' H1c3' 27.8(6) . . . C3' C4' H2c3' 27.7(6) . . . C3' C4' H1c4' 107.1(12) . . . C3' C4' H2c4' 107.2(12) . . . C3' C4' H1c5' 103.6(8) . . . C3' C4' H2c5' 97.1(8) . . . C3' C4' H1c6' 158.3(9) . . . C3' C4' H2c6' 150.4(10) . . . C5' C4' C6' 34.4(6) . . . C5' C4' H1c2' 159.6(8) . . . C5' C4' H1c3' 96.5(8) . . . C5' C4' H2c3' 101.0(7) . . . C5' C4' H1c4' 109.1(12) . . . C5' C4' H2c4' 109.2(12) . . . C5' C4' H1c5' 26.1(5) . . . C5' C4' H2c5' 26.1(5) . . . C5' C4' H1c6' 48.5(6) . . . C5' C4' H2c6' 51.6(6) . . . C6' C4' H1c2' 162.6(6) . . . C6' C4' H1c3' 125.0(7) . . . C6' C4' H2c3' 133.6(6) . . . C6' C4' H1c4' 94.6(9) . . . C6' C4' H2c4' 86.1(9) . . . C6' C4' H1c5' 51.8(4) . . . C6' C4' H2c5' 51.7(4) . . . C6' C4' H1c6' 21.8(3) . . . C6' C4' H2c6' 22.6(3) . . . H1c2' C4' H1c3' 72.2(4) . . . H1c2' C4' H2c3' 58.7(3) . . . H1c2' C4' H1c4' 71.3(7) . . . H1c2' C4' H2c4' 89.2(8) . . . H1c2' C4' H1c5' 136.0(6) . . . H1c2' C4' H2c5' 145.6(6) . . . H1c2' C4' H1c6' 142.4(5) . . . H1c2' C4' H2c6' 148.8(5) . . . H1c3' C4' H2c3' 47.1(3) . . . H1c3' C4' H1c4' 134.7(11) . . . H1c3' C4' H2c4' 95.7(9) . . . H1c3' C4' H1c5' 96.6(5) . . . H1c3' C4' H2c5' 73.7(4) . . . H1c3' C4' H1c6' 144.6(6) . . . H1c3' C4' H2c6' 122.7(6) . . . H2c3' C4' H1c4' 90.6(9) . . . H2c3' C4' H2c4' 134.7(11) . . . H2c3' C4' H1c5' 82.1(4) . . . H2c3' C4' H2c5' 94.2(5) . . . H2c3' C4' H1c6' 132.4(6) . . . H2c3' C4' H2c6' 152.3(6) . . . H1c4' C4' H2c4' 109.5(12) . . . H1c4' C4' H1c5' 91.6(8) . . . H1c4' C4' H2c5' 134.8(11) . . . H1c4' C4' H1c6' 72.8(7) . . . H1c4' C4' H2c6' 102.4(9) . . . H2c4' C4' H1c5' 134.8(11) . . . H2c4' C4' H2c5' 98.4(9) . . . H2c4' C4' H1c6' 92.7(8) . . . H2c4' C4' H2c6' 63.5(7) . . . H1c5' C4' H2c5' 45.1(2) . . . H1c5' C4' H1c6' 55.0(3) . . . H1c5' C4' H2c6' 73.3(4) . . . H2c5' C4' H1c6' 71.0(4) . . . H2c5' C4' H2c6' 59.3(3) . . . H1c6' C4' H2c6' 35.97(19) . . . N' C5' C3' 168.9(6) . . . N' C5' C4' 141.0(8) . . . N' C5' C6' 31.8(6) . . . N' C5' H1c3' 153.1(5) . . . N' C5' H2c3' 170.2(5) . . . N' C5' H1c4' 128.4(6) . . . N' C5' H2c4' 119.8(5) . . . N' C5' H1c5' 93.9(8) . . . N' C5' H2c5' 88.1(8) . . . N' C5' H1c6' 51.7(3) . . . N' C5' H2c6' 51.7(3) . . . C3' C5' C4' 32.0(6) . . . C3' C5' C6' 140.9(8) . . . C3' C5' H1c3' 21.6(3) . . . C3' C5' H2c3' 20.9(3) . . . C3' C5' H1c4' 50.2(4) . . . C3' C5' H2c4' 50.2(4) . . . C3' C5' H1c5' 97.2(9) . . . C3' C5' H2c5' 89.2(8) . . . C3' C5' H1c6' 126.7(6) . . . C3' C5' H2c6' 118.1(6) . . . C4' C5' C6' 109.5(10) . . . C4' C5' H1c3' 48.6(6) . . . C4' C5' H2c3' 45.8(6) . . . C4' C5' H1c4' 26.6(5) . . . C4' C5' H2c4' 26.5(5) . . . C4' C5' H1c5' 110.4(11) . . . C4' C5' H2c5' 110.4(11) . . . C4' C5' H1c6' 96.3(7) . . . C4' C5' H2c6' 91.2(7) . . . C6' C5' H1c3' 145.7(8) . . . C6' C5' H2c3' 151.8(8) . . . C6' C5' H1c4' 98.6(8) . . . C6' C5' H2c4' 91.8(7) . . . C6' C5' H1c5' 108.5(11) . . . C6' C5' H2c5' 108.5(11) . . . C6' C5' H1c6' 28.2(5) . . . C6' C5' H2c6' 28.1(5) . . . H1c3' C5' H2c3' 34.42(17) . . . H1c3' C5' H1c4' 70.9(3) . . . H1c3' C5' H2c4' 57.1(3) . . . H1c3' C5' H1c5' 104.6(8) . . . H1c3' C5' H2c5' 67.6(7) . . . H1c3' C5' H1c6' 144.5(5) . . . H1c3' C5' H2c6' 117.7(5) . . . H2c3' C5' H1c4' 53.2(2) . . . H2c3' C5' H2c4' 68.9(3) . . . H2c3' C5' H1c5' 76.3(7) . . . H2c3' C5' H2c5' 95.2(8) . . . H2c3' C5' H1c6' 127.4(5) . . . H2c3' C5' H2c6' 136.6(5) . . . H1c4' C5' H2c4' 45.4(2) . . . H1c4' C5' H1c5' 92.6(8) . . . H1c4' C5' H2c5' 136.6(10) . . . H1c4' C5' H1c6' 77.1(4) . . . H1c4' C5' H2c6' 91.4(4) . . . H2c4' C5' H1c5' 136.4(10) . . . H2c4' C5' H2c5' 99.3(8) . . . H2c4' C5' H1c6' 89.5(4) . . . H2c4' C5' H2c6' 68.1(3) . . . H1c5' C5' H2c5' 109.4(11) . . . H1c5' C5' H1c6' 91.4(8) . . . H1c5' C5' H2c6' 136.3(10) . . . H2c5' C5' H1c6' 136.4(10) . . . H2c5' C5' H2c6' 96.7(8) . . . H1c6' C5' H2c6' 47.5(2) . . .