#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 13 _journal_issue 1 _journal_year 2022 _journal_page_first 117 _journal_page_last 125 #============================================================================= data_krs3 _audit_creation_date 2022-01-23 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C41 H38 N Ni P2 S1, Cl O4' _chemical_formula_sum 'C41 H38 Cl N Ni O4 P2 S1' _chemical_formula_weight 828.92 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'orthorhombic' _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x+1/2, -y+1/2, -z' 3 '-x, y+1/2, -z+1/2' 4 '-x+1/2, -y, z+1/2' 5 '-x, -y, -z' 6 '-x-1/2, y-1/2, z' 7 'x, -y-1/2, z-1/2' 8 'x-1/2, y, -z-1/2' _cell_length_a 16.442(2) _cell_length_b 21.627(2) _cell_length_c 21.591(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7677.6(14) _cell_formula_units_Z 8 _cell_measurement_reflns_used 762 _cell_measurement_temperature 293 _cell_measurement_theta_max 24.21 _cell_measurement_theta_min 4.25 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 3440 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1043 _diffrn_reflns_av_unetI/netI 0.2598 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 45499 _diffrn_reflns_theta_full 28.45 _diffrn_reflns_theta_max 28.45 _diffrn_reflns_theta_min 1.82 _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device_type 'Bruker AXS smart with CCD' _diffrn_measurement_method ? _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4843 _reflns_number_total 9675 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.627 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 622 _refine_ls_number_reflns 9675 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1992 _refine_ls_R_factor_gt 0.0471 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.1124 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.46389(4) 0.18804(3) 0.71237(3) 0.0395(2) Uani 1 1 d . . . S1 S 0.53704(9) 0.20942(6) 0.79638(7) 0.0555(4) Uani 1 1 d . . . S2 S 0.44180(9) 0.10565(6) 0.76973(7) 0.0586(5) Uani 1 1 d . . . P1 P 0.38132(8) 0.15439(6) 0.63913(6) 0.0400(4) Uani 1 1 d . . . P2 P 0.51128(8) 0.27290(6) 0.66643(6) 0.0399(4) Uani 1 1 d . . . N1 N 0.5436(2) 0.10705(18) 0.8671(2) 0.0471(11) Uani 1 1 d . . . C1 C 0.5128(3) 0.1360(2) 0.8197(2) 0.0451(14) Uani 1 1 d . . . C2 C 0.6078(4) 0.1341(3) 0.9073(3) 0.0573(18) Uani 1 1 d . . . H2A H 0.587(3) 0.178(2) 0.924(2) 0.053(16) Uiso 1 1 d . . . H2B H 0.649(3) 0.143(2) 0.884(3) 0.08(2) Uiso 1 1 d . . . C3 C 0.6176(9) 0.0885(4) 0.9570(5) 0.114(4) Uani 1 1 d . . . H3A H 0.660(4) 0.090(3) 0.981(4) 0.21(3) Uiso 1 1 d . . . H3B H 0.584(6) 0.099(5) 0.999(5) 0.16(7) Uiso 1 1 d . . . C4 C 0.5762(10) 0.0338(7) 0.9416(7) 0.117(5) Uani 1 1 d . . . H4A H 0.561(4) 0.002(3) 0.964(3) 0.13(3) Uiso 1 1 d . . . H4B H 0.608(8) 0.010(6) 0.930(7) 0.18(9) Uiso 1 1 d . . . C5 C 0.5227(5) 0.0437(3) 0.8868(4) 0.064(2) Uani 1 1 d . . . H5A H 0.534(3) 0.014(3) 0.852(3) 0.09(3) Uiso 1 1 d . . . H5B H 0.468(3) 0.045(2) 0.896(2) 0.061(19) Uiso 1 1 d . . . C6 C 0.3184(3) 0.0881(2) 0.6611(3) 0.0438(14) Uani 1 1 d . . . C7 C 0.2599(4) 0.0941(3) 0.7064(3) 0.0652(18) Uani 1 1 d . . . H7 H 0.255(3) 0.136(2) 0.731(2) 0.071(18) Uiso 1 1 d . . . C8 C 0.2145(5) 0.0431(4) 0.7252(4) 0.083(2) Uani 1 1 d . . . H8 H 0.176(3) 0.051(3) 0.753(3) 0.08(2) Uiso 1 1 d . . . C9 C 0.2265(5) -0.0132(4) 0.6981(4) 0.086(3) Uani 1 1 d . . . H9 H 0.188(3) -0.046(3) 0.710(3) 0.11(2) Uiso 1 1 d . . . C10 C 0.2828(5) -0.0201(4) 0.6530(5) 0.092(3) Uani 1 1 d . . . H10 H 0.298(5) -0.056(4) 0.627(4) 0.18(4) Uiso 1 1 d . . . C11 C 0.3294(4) 0.0303(3) 0.6346(3) 0.0685(19) Uani 1 1 d . . . H11 H 0.370(3) 0.024(2) 0.602(2) 0.058(18) Uiso 1 1 d . . . C12 C 0.3068(3) 0.2132(2) 0.6190(3) 0.0397(13) Uani 1 1 d . . . C13 C 0.2794(3) 0.2264(3) 0.5595(3) 0.0492(15) Uani 1 1 d . . . H13 H 0.305(3) 0.202(2) 0.524(2) 0.061(17) Uiso 1 1 d . . . C14 C 0.2203(4) 0.2702(3) 0.5498(4) 0.069(2) Uani 1 1 d . . . H14 H 0.197(3) 0.278(2) 0.509(3) 0.10(2) Uiso 1 1 d . . . C15 C 0.1861(4) 0.3016(3) 0.5989(5) 0.079(2) Uani 1 1 d . . . H15 H 0.144(3) 0.329(2) 0.590(2) 0.070(19) Uiso 1 1 d . . . C16 C 0.2136(4) 0.2900(3) 0.6575(5) 0.072(2) Uani 1 1 d . . . H16 H 0.197(3) 0.309(2) 0.693(2) 0.073(2) Uiso 1 1 d . . . C17 C 0.2735(3) 0.2465(3) 0.6683(3) 0.0504(16) Uani 1 1 d . . . H17 H 0.288(3) 0.2381(19) 0.707(2) 0.056(16) Uiso 1 1 d . . . C18 C 0.4354(3) 0.1261(2) 0.5713(2) 0.0407(13) Uani 1 1 d . . . C19 C 0.5189(4) 0.1193(3) 0.5756(3) 0.0557(16) Uani 1 1 d . . . H19 H 0.549(3) 0.1279(19) 0.616(2) 0.053(15) Uiso 1 1 d . . . C20 C 0.5626(5) 0.0961(3) 0.5249(4) 0.076(2) Uani 1 1 d . . . H20 H 0.614(3) 0.089(2) 0.536(2) 0.077(17) Uiso 1 1 d . . . C21 C 0.5223(6) 0.0806(3) 0.4715(4) 0.080(2) Uani 1 1 d . . . H21 H 0.552(3) 0.067(2) 0.437(3) 0.10(2) Uiso 1 1 d . . . C22 C 0.4399(6) 0.0847(3) 0.4678(4) 0.078(2) Uani 1 1 d . . . H22 H 0.415(4) 0.071(3) 0.430(3) 0.14(3) Uiso 1 1 d . . . C23 C 0.3968(4) 0.1079(3) 0.5168(3) 0.0583(17) Uani 1 1 d . . . H23 H 0.340(3) 0.109(2) 0.515(2) 0.053(19) Uiso 1 1 d . . . C24 C 0.4682(3) 0.3014(2) 0.5938(2) 0.0392(12) Uani 1 1 d . . . C25 C 0.4122(3) 0.3495(3) 0.5924(3) 0.0504(15) Uani 1 1 d . . . H25 H 0.395(3) 0.3721(18) 0.630(2) 0.040(15) Uiso 1 1 d . . . C26 C 0.3786(4) 0.3672(3) 0.5362(4) 0.0611(18) Uani 1 1 d . . . H26 H 0.338(3) 0.397(2) 0.541(2) 0.063(17) Uiso 1 1 d . . . C27 C 0.3977(4) 0.3374(3) 0.4830(4) 0.068(2) Uani 1 1 d . . . H27 H 0.378(3) 0.350(2) 0.444(3) 0.061(19) Uiso 1 1 d . . . C28 C 0.4536(4) 0.2895(3) 0.4834(3) 0.0592(17) Uani 1 1 d . . . H28 H 0.467(2) 0.2660(17) 0.445(2) 0.061(13) Uiso 1 1 d . . . C29 C 0.4886(3) 0.2721(3) 0.5385(3) 0.0472(15) Uani 1 1 d . . . H29 H 0.526(2) 0.2378(17) 0.5381(18) 0.049(14) Uiso 1 1 d . . . C30 C 0.6193(3) 0.2667(2) 0.6483(2) 0.0401(13) Uani 1 1 d . . . C31 C 0.6651(4) 0.2162(3) 0.6663(3) 0.0508(16) Uani 1 1 d . . . H31 H 0.643(3) 0.1849(19) 0.683(2) 0.062(16) Uiso 1 1 d . . . C32 C 0.7476(4) 0.2132(3) 0.6551(3) 0.0608(18) Uani 1 1 d . . . H32 H 0.775(3) 0.174(2) 0.665(2) 0.063(19) Uiso 1 1 d . . . C33 C 0.7862(5) 0.2621(4) 0.6269(3) 0.073(2) Uani 1 1 d . . . H33 H 0.842(4) 0.263(3) 0.614(3) 0.10(2) Uiso 1 1 d . . . C34 C 0.7411(4) 0.3125(4) 0.6071(3) 0.0657(19) Uani 1 1 d . . . H34 H 0.766(3) 0.344(2) 0.587(2) 0.067(18) Uiso 1 1 d . . . C35 C 0.6588(4) 0.3138(3) 0.6166(3) 0.0538(16) Uani 1 1 d . . . H35 H 0.630(3) 0.3474(19) 0.605(2) 0.044(17) Uiso 1 1 d . . . C36 C 0.4999(3) 0.3384(2) 0.7192(2) 0.0408(13) Uani 1 1 d . . . C37 C 0.5540(4) 0.3873(3) 0.7218(3) 0.0564(16) Uani 1 1 d . . . H37 H 0.603(2) 0.3847(18) 0.6999(19) 0.057(14) Uiso 1 1 d . . . C38 C 0.5379(5) 0.4380(3) 0.7596(3) 0.0697(19) Uani 1 1 d . . . H38 H 0.581(3) 0.472(2) 0.756(3) 0.10(2) Uiso 1 1 d . . . C39 C 0.4707(5) 0.4408(3) 0.7946(3) 0.0682(18) Uani 1 1 d . . . H39 H 0.462(3) 0.475(2) 0.823(2) 0.062(16) Uiso 1 1 d . . . C40 C 0.4160(4) 0.3921(3) 0.7941(3) 0.0657(18) Uani 1 1 d . . . H40 H 0.358(3) 0.3913(19) 0.816(2) 0.063(16) Uiso 1 1 d . . . C41 C 0.4311(4) 0.3410(3) 0.7562(3) 0.0537(16) Uani 1 1 d . . . H41 H 0.395(2) 0.3064(18) 0.7574(19) 0.055(14) Uiso 1 1 d . . . Cl1 Cl 0.76158(12) 0.00870(9) 0.59314(10) 0.0783(5) Uani 1 1 d . . . O1 O 0.7803(6) 0.0650(3) 0.6084(4) 0.247(4) Uani 1 1 d . . . O2 O 0.6963(4) -0.0069(5) 0.6237(3) 0.272(5) Uani 1 1 d . . . O3 O 0.7460(3) 0.0069(3) 0.5291(3) 0.178(3) Uani 1 1 d . . . O4 O 0.8263(5) -0.0251(4) 0.6099(5) 0.269(5) Uani 1 1 d . . . 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 Ni 0.0423(4) 0.0383(4) 0.0379(4) 0.0040(3) -0.0038(3) -0.0057(3) S1 0.0711(10) 0.0496(8) 0.0457(9) 0.0097(7) -0.0156(8) -0.0193(8) S2 0.0664(10) 0.0495(9) 0.0599(11) 0.0173(7) -0.0206(8) -0.0186(8) P1 0.0401(8) 0.0407(8) 0.0392(9) 0.0009(7) -0.0003(7) -0.0048(7) P2 0.0431(9) 0.0399(8) 0.0368(9) 0.0022(6) -0.0011(7) -0.0037(7) N1 0.045(3) 0.045(3) 0.051(3) 0.012(2) -0.008(2) -0.004(2) C1 0.044(3) 0.050(3) 0.042(4) 0.002(3) 0.002(3) -0.008(3) C2 0.044(4) 0.080(5) 0.047(4) 0.010(4) -0.004(3) -0.005(4) C3 0.176(11) 0.075(6) 0.090(8) 0.026(5) -0.082(8) -0.020(7) C4 0.125(10) 0.128(10) 0.098(9) 0.079(8) -0.049(8) -0.029(10) C5 0.064(5) 0.052(4) 0.074(6) 0.022(4) -0.006(4) -0.001(4) C6 0.043(4) 0.044(3) 0.044(4) 0.006(3) -0.009(3) -0.006(3) C7 0.074(5) 0.071(5) 0.050(4) -0.001(4) -0.001(4) -0.030(4) C8 0.065(5) 0.107(7) 0.077(6) 0.012(5) 0.005(4) -0.035(5) C9 0.095(6) 0.069(6) 0.093(7) 0.037(5) -0.017(5) -0.032(5) C10 0.102(7) 0.059(5) 0.115(8) 0.012(5) 0.020(5) -0.010(5) C11 0.063(5) 0.045(4) 0.097(6) 0.005(4) 0.015(4) -0.005(3) C12 0.033(3) 0.043(3) 0.043(4) 0.003(3) -0.002(3) -0.007(2) C13 0.048(4) 0.044(4) 0.056(4) 0.005(3) -0.008(3) 0.001(3) C14 0.055(5) 0.058(5) 0.093(7) 0.016(5) -0.010(5) -0.004(4) C15 0.053(5) 0.058(5) 0.125(8) 0.018(5) -0.008(5) 0.006(4) C16 0.064(5) 0.053(5) 0.100(7) -0.010(5) 0.022(5) 0.003(4) C17 0.049(4) 0.051(4) 0.052(5) -0.001(3) 0.006(3) -0.004(3) C18 0.047(3) 0.036(3) 0.039(4) 0.002(2) 0.002(3) -0.001(3) C19 0.048(4) 0.055(4) 0.063(5) -0.009(3) 0.004(4) 0.001(3) C20 0.053(5) 0.069(5) 0.104(7) -0.001(4) 0.015(5) 0.004(4) C21 0.102(7) 0.069(5) 0.069(6) -0.016(4) 0.036(5) -0.002(5) C22 0.098(7) 0.081(5) 0.053(5) -0.019(4) 0.007(5) 0.010(5) C23 0.059(5) 0.058(4) 0.057(5) -0.003(3) 0.000(4) 0.006(4) C24 0.040(3) 0.039(3) 0.039(3) 0.010(2) -0.002(3) -0.010(3) C25 0.050(4) 0.046(4) 0.055(5) 0.005(3) -0.005(3) -0.001(3) C26 0.059(5) 0.047(4) 0.077(6) 0.012(4) -0.014(4) -0.001(4) C27 0.075(5) 0.068(5) 0.062(5) 0.021(4) -0.030(4) -0.031(4) C28 0.072(5) 0.060(4) 0.045(4) 0.006(3) -0.006(4) -0.023(4) C29 0.052(4) 0.048(4) 0.041(4) 0.002(3) 0.000(3) -0.008(3) C30 0.038(3) 0.044(3) 0.038(3) 0.001(3) -0.001(3) -0.007(3) C31 0.050(4) 0.053(4) 0.049(4) 0.002(3) -0.002(3) -0.008(4) C32 0.051(4) 0.075(5) 0.057(4) -0.013(4) 0.001(3) 0.013(4) C33 0.051(5) 0.110(7) 0.058(5) -0.028(4) 0.017(4) -0.015(5) C34 0.063(5) 0.076(5) 0.058(5) -0.001(4) 0.015(4) -0.016(5) C35 0.055(4) 0.058(4) 0.048(4) -0.001(3) 0.007(3) -0.005(4) C36 0.052(3) 0.038(3) 0.032(3) 0.009(2) -0.007(3) -0.005(3) C37 0.054(4) 0.053(4) 0.062(5) -0.006(3) 0.002(3) -0.006(3) C38 0.092(5) 0.050(4) 0.067(5) -0.010(4) -0.002(4) -0.015(4) C39 0.102(6) 0.052(4) 0.050(4) -0.009(4) -0.005(4) 0.007(4) C40 0.072(5) 0.069(5) 0.056(5) -0.009(4) 0.009(4) 0.013(4) C41 0.058(4) 0.051(4) 0.053(4) -0.004(3) 0.006(3) -0.008(3) Cl1 0.0759(13) 0.0776(14) 0.0815(15) -0.0055(11) 0.0087(11) -0.0094(11) O1 0.440(13) 0.094(5) 0.206(8) -0.022(5) -0.020(8) -0.079(6) O2 0.168(7) 0.540(15) 0.107(6) 0.073(7) 0.005(5) -0.202(8) O3 0.123(5) 0.321(9) 0.089(5) -0.058(5) 0.008(4) 0.033(5) O4 0.250(10) 0.213(8) 0.346(13) 0.006(7) -0.117(9) 0.104(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni S1 2.2250(15) . ? Ni S2 2.2002(15) . ? Ni P1 2.2076(15) . ? Ni P2 2.2268(14) . ? S1 C1 1.713(5) . ? S2 C1 1.720(5) . ? P1 C6 1.831(5) . ? P1 C12 1.818(5) . ? P1 C18 1.819(5) . ? P2 C24 1.827(5) . ? P2 C30 1.824(5) . ? P2 C36 1.827(5) . ? N1 C2 1.486(7) . ? N1 C5 1.475(7) . ? C1 N1 1.302(6) . ? C2 C3 1.466(9) . ? C3 C4 1.405(15) . ? C4 C5 1.491(11) . ? C6 C7 1.377(7) . ? C6 C11 1.387(7) . ? C7 C8 1.392(8) . ? C8 C9 1.365(10) . ? C9 C10 1.352(10) . ? C10 C11 1.389(9) . ? C12 C13 1.391(7) . ? C12 C17 1.398(7) . ? C13 C14 1.374(8) . ? C14 C15 1.378(9) . ? C15 C16 1.367(10) . ? C16 C17 1.381(8) . ? C18 C19 1.383(7) . ? C18 C23 1.396(7) . ? C19 C20 1.404(9) . ? C20 C21 1.372(10) . ? C21 C22 1.360(10) . ? C22 C23 1.368(8) . ? C24 C25 1.389(7) . ? C24 C29 1.394(7) . ? C26 C25 1.388(8) . ? C27 C26 1.354(8) . ? C28 C27 1.384(8) . ? C29 C28 1.374(7) . ? C30 C31 1.382(7) . ? C30 C35 1.388(7) . ? C31 C32 1.379(7) . ? C32 C33 1.377(9) . ? C33 C34 1.384(9) . ? C34 C35 1.370(8) . ? C36 C37 1.384(7) . ? C36 C41 1.386(7) . ? C37 C38 1.392(7) . ? C38 C39 1.341(8) . ? C39 C40 1.386(8) . ? C40 C41 1.395(7) . ? Cl1 O1 1.299(6) . ? Cl1 O2 1.304(6) . ? Cl1 O3 1.406(6) . ? Cl1 O4 1.341(7) . ? 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 S1 Ni P2 90.16(5) . . ? S2 Ni S1 78.38(5) . . ? S2 Ni P1 91.99(6) . . ? S2 Ni P2 167.40(6) . . ? P1 Ni S1 170.04(6) . . ? P1 Ni P2 99.66(5) . . ? C1 S1 Ni 85.49(18) . . ? C1 S2 Ni 86.10(18) . . ? C6 P1 Ni 114.83(17) . . ? C12 P1 Ni 110.82(17) . . ? C12 P1 C6 103.2(2) . . ? C18 P1 Ni 112.74(18) . . ? C18 P1 C6 102.8(2) . . ? C18 P1 C12 111.9(2) . . ? C24 P2 Ni 121.65(15) . . ? C30 P2 Ni 112.07(17) . . ? C30 P2 C24 102.6(2) . . ? C30 P2 C36 106.9(2) . . ? C36 P2 Ni 108.95(17) . . ? C36 P2 C24 103.5(2) . . ? C1 N1 C2 123.1(5) . . ? C1 N1 C5 125.6(5) . . ? C5 N1 C2 111.3(5) . . ? S1 C1 S2 109.1(3) . . ? N1 C1 S1 125.9(4) . . ? N1 C1 S2 125.0(4) . . ? C3 C2 N1 103.9(6) . . ? C4 C3 C2 109.8(7) . . ? C3 C4 C5 110.7(8) . . ? N1 C5 C4 102.9(7) . . ? C7 C6 P1 120.3(5) . . ? C7 C6 C11 117.9(6) . . ? C11 C6 P1 121.7(5) . . ? C6 C7 C8 120.5(7) . . ? C9 C8 C7 120.2(8) . . ? C10 C9 C8 120.4(8) . . ? C9 C10 C11 119.8(8) . . ? C10 C11 C6 121.1(7) . . ? C13 C12 P1 125.6(4) . . ? C13 C12 C17 118.1(5) . . ? C17 C12 P1 116.3(4) . . ? C14 C13 C12 120.7(6) . . ? C13 C14 C15 120.8(8) . . ? C16 C15 C14 119.1(7) . . ? C15 C16 C17 121.1(7) . . ? C16 C17 C12 120.2(7) . . ? C19 C18 P1 117.8(5) . . ? C19 C18 C23 118.6(6) . . ? C23 C18 P1 123.5(4) . . ? C18 C19 C20 119.6(7) . . ? C21 C20 C19 119.7(7) . . ? C22 C21 C20 121.0(8) . . ? C21 C22 C23 119.7(8) . . ? C22 C23 C18 121.4(7) . . ? C25 C24 P2 121.9(4) . . ? C25 C24 C29 118.8(5) . . ? C29 C24 P2 119.2(4) . . ? C26 C25 C24 119.4(6) . . ? C27 C26 C25 121.2(7) . . ? C26 C27 C28 120.3(7) . . ? C29 C28 C27 119.3(7) . . ? C28 C29 C24 121.1(6) . . ? C31 C30 P2 121.9(4) . . ? C31 C30 C35 117.6(6) . . ? C35 C30 P2 120.5(4) . . ? C32 C31 C30 121.6(6) . . ? C33 C32 C31 119.6(7) . . ? C32 C33 C34 119.6(7) . . ? C35 C34 C33 119.9(7) . . ? C34 C35 C30 121.4(7) . . ? C37 C36 P2 123.5(4) . . ? C41 C36 P2 118.4(4) . . ? C41 C36 C37 118.0(5) . . ? C36 C37 C38 120.3(6) . . ? C39 C38 C37 121.5(7) . . ? C38 C39 C40 119.7(6) . . ? C39 C40 C41 119.5(6) . . ? C36 C41 C40 121.0(6) . . ? O1 Cl1 O2 108.0(6) . . ? O1 Cl1 O3 108.6(5) . . ? O1 Cl1 O4 104.8(6) . . ? O2 Cl1 O3 109.9(4) . . ? O2 Cl1 O4 112.1(6) . . ? O4 Cl1 O3 113.2(5) . . ? _iucr_refine_instructions_details ; TITL KRS3 P bca CELL 0.71069 16.442 21.627 21.591 90.000 90.000 90.000 ZERR 2 .002 .002 .002 .00 .00 .00 LATT 1 SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5-X,-Y,0.5+Z SFAC NI S P N C H CL O UNIT 8 16 16 8 328 304 8 32 MERG 2 L.S. 4 ACTA WGHT 0.037600 EXTI 0.030383 FVAR 0.02481 NI1 1 0.463887 0.188046 0.712382 11.00000 0.04198 0.03803 = 0.03764 0.00396 -0.00371 -0.00563 S1 2 0.537018 0.209447 0.796392 11.00000 0.07058 0.04957 = 0.04535 0.00964 -0.01550 -0.01918 S2 2 0.441791 0.105655 0.769727 11.00000 0.06585 0.04939 = 0.05944 0.01733 -0.02046 -0.01865 C4 5 0.512748 0.136052 0.819658 11.00000 0.04403 0.04919 = 0.04203 0.00197 0.00246 -0.00820 N5 4 0.543565 0.107023 0.867055 11.00000 0.04494 0.04501 = 0.05074 0.01177 -0.00850 -0.00422 C6 5 0.607845 0.134278 0.907211 11.00000 0.04314 0.08044 = 0.04609 0.00859 -0.00384 -0.00451 C7 5 0.616878 0.088611 0.957458 11.00000 0.17614 0.07400 = 0.09348 0.02777 -0.08001 -0.01311 C8 5 0.576528 0.033701 0.941169 11.00000 0.11924 0.13075 = 0.09707 0.07728 -0.04700 -0.02713 C9 5 0.522799 0.043719 0.886736 11.00000 0.06586 0.05251 = 0.07359 0.02279 -0.00599 -0.00199 P1 3 0.381329 0.154380 0.639125 11.00000 0.03976 0.04043 = 0.03891 0.00091 -0.00035 -0.00471 C14 5 0.435454 0.126067 0.571310 11.00000 0.04788 0.03562 = 0.03856 0.00122 0.00228 -0.00067 C15 5 0.518925 0.119334 0.575631 11.00000 0.04784 0.05587 = 0.06532 -0.00931 0.00504 0.00118 C16 5 0.562514 0.095957 0.524913 11.00000 0.05352 0.06882 = 0.10438 -0.00123 0.01713 0.00354 C17 5 0.522538 0.080473 0.471462 11.00000 0.09658 0.07026 = 0.06895 -0.01669 0.03365 -0.00154 C18 5 0.440479 0.084719 0.467991 11.00000 0.10219 0.08111 = 0.05144 -0.01963 0.00598 0.00919 C19 5 0.396749 0.107896 0.516744 11.00000 0.06081 0.05793 = 0.05577 -0.00294 -0.00050 0.00652 C21 5 0.318327 0.088064 0.661146 11.00000 0.04241 0.04465 = 0.04369 0.00528 -0.00933 -0.00600 C22 5 0.259977 0.093917 0.706461 11.00000 0.07410 0.07281 = 0.04932 -0.00133 0.00022 -0.02951 C23 5 0.214547 0.043149 0.725223 11.00000 0.06678 0.10675 = 0.07509 0.01275 0.00497 -0.03688 C24 5 0.226179 -0.013132 0.698175 11.00000 0.09493 0.06869 = 0.09285 0.03594 -0.01435 -0.03145 C25 5 0.282446 -0.019599 0.653228 11.00000 0.10399 0.05686 = 0.11716 0.00969 0.01884 -0.01020 C26 5 0.329201 0.030228 0.634702 11.00000 0.06259 0.04482 = 0.09807 0.00533 0.01486 -0.00528 C28 5 0.306672 0.213288 0.619050 11.00000 0.03209 0.04320 = 0.04276 0.00320 -0.00175 -0.00642 C29 5 0.279369 0.226507 0.559610 11.00000 0.04802 0.04407 = 0.05594 0.00455 -0.00805 0.00089 C30 5 0.220241 0.270218 0.550066 11.00000 0.05517 0.05811 = 0.09285 0.01877 -0.01157 -0.00341 C31 5 0.186135 0.301617 0.598988 11.00000 0.05257 0.05742 = 0.12511 0.01602 -0.00555 0.00689 C32 5 0.213763 0.290054 0.657731 11.00000 0.06239 0.05248 = 0.10043 -0.00982 0.02101 0.00260 C33 5 0.273438 0.246495 0.668435 11.00000 0.04664 0.04992 = 0.05278 -0.00155 0.00637 -0.00423 P2 3 0.511275 0.272895 0.666449 11.00000 0.04255 0.03966 = 0.03675 0.00231 -0.00113 -0.00369 C35 5 0.619377 0.266721 0.648303 11.00000 0.03684 0.04497 = 0.03833 0.00013 -0.00028 -0.00668 C36 5 0.665012 0.215942 0.666430 11.00000 0.04914 0.05271 = 0.04860 0.00071 -0.00279 -0.00662 C37 5 0.747584 0.213150 0.655083 11.00000 0.04988 0.07567 = 0.05719 -0.01237 0.00149 0.01208 C38 5 0.785975 0.262198 0.626900 11.00000 0.04902 0.11131 = 0.05891 -0.02844 0.01655 -0.01375 C39 5 0.741192 0.312535 0.607043 11.00000 0.06234 0.07692 = 0.05776 -0.00225 0.01475 -0.01500 C40 5 0.658766 0.314029 0.616634 11.00000 0.05403 0.05912 = 0.04750 -0.00140 0.00669 -0.00641 C41 5 0.499988 0.338350 0.719274 11.00000 0.05113 0.03807 = 0.03212 0.00896 -0.00685 -0.00424 C42 5 0.554197 0.387326 0.721780 11.00000 0.05593 0.05074 = 0.06159 -0.00633 0.00077 -0.00608 C43 5 0.537880 0.437923 0.759513 11.00000 0.09118 0.04954 = 0.06811 -0.00894 -0.00343 -0.01539 C44 5 0.470655 0.440776 0.794700 11.00000 0.10076 0.05161 = 0.05106 -0.00816 -0.00409 0.00695 C45 5 0.416059 0.391983 0.794016 11.00000 0.07391 0.06797 = 0.05583 -0.00876 0.00921 0.01363 C46 5 0.431251 0.341130 0.756233 11.00000 0.05861 0.05133 = 0.05245 -0.00412 0.00638 -0.00850 C47 5 0.468127 0.301387 0.593808 11.00000 0.04004 0.03893 = 0.03866 0.00991 -0.00279 -0.01049 C48 5 0.488634 0.272005 0.538435 11.00000 0.05221 0.04859 = 0.04078 0.00152 -0.00063 -0.00878 C49 5 0.453672 0.289493 0.483352 11.00000 0.07102 0.06103 = 0.04553 0.00625 -0.00497 -0.02353 C50 5 0.397762 0.337399 0.482887 11.00000 0.07439 0.06620 = 0.06228 0.02139 -0.02916 -0.03031 C51 5 0.378428 0.367265 0.536264 11.00000 0.05916 0.04700 = 0.07727 0.01318 -0.01466 -0.00156 C52 5 0.412232 0.349639 0.592465 11.00000 0.04922 0.04536 = 0.05615 0.00528 -0.00526 -0.00182 H2A 6 0.588284 0.177034 0.923434 11.00000 0.05172 H2B 6 0.652197 0.141675 0.883864 11.00000 0.07005 H3A 6 0.667269 0.083291 0.970921 11.00000 0.11609 H3B 6 0.583613 0.098713 0.999376 11.00000 0.23615 H4A 6 0.552326 0.010332 0.968249 11.00000 0.11463 H4B 6 0.609361 0.009631 0.934018 11.00000 0.17398 H5A 6 0.533796 0.014590 0.852882 11.00000 0.08385 H5B 6 0.469114 0.044566 0.895849 11.00000 0.05820 H15 6 0.548958 0.128046 0.615750 11.00000 0.05413 H16 6 0.615231 0.089658 0.534146 11.00000 0.04806 H17 6 0.552016 0.067028 0.435960 11.00000 0.08156 H18 6 0.415397 0.072454 0.431208 11.00000 0.10222 H19 6 0.340018 0.108981 0.514211 11.00000 0.05466 H7 6 0.253118 0.134088 0.729697 11.00000 0.06571 H8 6 0.176242 0.049473 0.754398 11.00000 0.07420 H9 6 0.190664 -0.046634 0.710134 11.00000 0.08919 H10 6 0.293029 -0.053682 0.631176 11.00000 0.12102 H11 6 0.368621 0.024698 0.603123 11.00000 0.05525 H13 6 0.303179 0.203081 0.525536 11.00000 0.05611 H14 6 0.200190 0.278958 0.510168 11.00000 0.08174 H15 6 0.144483 0.329709 0.590847 11.00000 0.06233 H16 6 0.196284 0.310204 0.692185 11.00000 0.06191 H17 6 0.288831 0.238127 0.707968 11.00000 0.03887 H36 6 0.642217 0.182828 0.683214 11.00000 0.04503 H37 6 0.775318 0.174908 0.665149 11.00000 0.06294 H38 6 0.840630 0.262577 0.615976 11.00000 0.08122 H39 6 0.765761 0.344545 0.587768 11.00000 0.05168 H40 6 0.629763 0.347536 0.604005 11.00000 0.04651 H42 6 0.602475 0.385069 0.699293 11.00000 0.03930 H43 6 0.578823 0.470715 0.756774 11.00000 0.08277 H44 6 0.461686 0.475741 0.822346 11.00000 0.05696 H45 6 0.361444 0.391819 0.816885 11.00000 0.06119 H46 6 0.395630 0.307608 0.757162 11.00000 0.03555 H48 6 0.525760 0.237874 0.538304 11.00000 0.03256 H49 6 0.468221 0.266524 0.444838 11.00000 0.03634 H50 6 0.376750 0.350685 0.444717 11.00000 0.06126 H51 6 0.339028 0.397520 0.539517 11.00000 0.05015 H52 6 0.395151 0.371451 0.629784 11.00000 0.04446 CL1 7 0.761529 0.008701 0.593137 11.00000 0.07518 0.07681 = 0.08130 -0.00546 0.00856 -0.00964 O1 8 0.746086 0.006904 0.529045 11.00000 0.12213 0.31855 = 0.08792 -0.05647 0.00712 0.03387 O2 8 0.826242 -0.025138 0.609974 11.00000 0.24780 0.21377 = 0.34406 0.00884 -0.11580 0.10217 O3 8 0.780633 0.065043 0.608418 11.00000 0.43248 0.09236 = 0.20828 -0.02087 -0.01893 -0.07919 O4 8 0.696333 -0.007050 0.623796 11.00000 0.16683 0.53649 = 0.10789 0.07437 0.00599 -0.20105 FMAP 2 PLAN -20 LIST 4 HKLF 4 1 1 0 0 0 0 1 0 1 0 REM KRS3 P bca REM R1 = 0.0493 for 2855 Fo > 4sig(Fo) and 0.1979 for all 8987 data REM 623 parameters refined using 0 restraints END ; _olex2_submission_special_instructions 'No special instructions were received'