# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kyritsis, Panayotis' _publ_contact_author_email kyritsis@chem.uoa.gr _publ_section_title ; Conversion of tetrahedral to octahedral structures upon solvent coordination: Studies on the M[(OPPh2)(SePPh2)N]2 (M = Co, Ni) and [Ni{(OPPh2)(EPPh2)N}2(dmf)2] (E = S, Se) complexes ; _publ_author_name P.Kyritsis # Attachment '- Ferentinos_Dalton.cif' data_Complex1 _database_code_depnum_ccdc_archive 'CCDC 764424' #TrackingRef '- Ferentinos_Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Co N2 O2 P4 Se2' _chemical_formula_weight 1017.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.593(3) _cell_length_b 18.466(5) _cell_length_c 19.534(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.920(10) _cell_angle_gamma 90.00 _cell_volume 4475(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 11.0 _exptl_crystal_description parall _exptl_crystal_colour blue _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2052 _exptl_absorpt_coefficient_mu 2.195 _exptl_absorpt_correction_type 'psi scan empirical' _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Crystal Logic Dual Goniometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 6433 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6221 _reflns_number_gt 4828 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+2.6930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6221 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.20018(6) 0.21505(4) 0.09491(4) 0.0408(2) Uani 1 1 d . . . Se1 Se 0.17905(5) 0.08480(3) 0.11434(3) 0.04780(19) Uani 1 1 d . . . O1 O 0.0622(3) 0.2484(2) 0.0433(2) 0.0519(10) Uani 1 1 d . . . P1 P 0.02307(11) 0.10166(7) 0.14592(7) 0.0383(3) Uani 1 1 d . . . P2 P -0.05000(11) 0.22515(7) 0.05611(8) 0.0407(3) Uani 1 1 d . . . N1 N -0.0588(4) 0.1534(2) 0.0992(2) 0.0482(12) Uani 1 1 d . . . N2 N 0.4294(4) 0.3321(3) 0.1207(3) 0.0525(12) Uani 1 1 d . . . Se2 Se 0.25307(6) 0.27101(3) 0.20830(4) 0.0465(3) Uani 0.881(3) 1 d P . . O3 O 0.282(4) 0.284(2) 0.174(3) 0.076(13) Uiso 0.119(3) 1 d P . . P3 P 0.35159(12) 0.35505(7) 0.17162(8) 0.0428(4) Uani 1 1 d . . . P4 P 0.42259(12) 0.27392(8) 0.06055(9) 0.0493(4) Uani 1 1 d . . . O2 O 0.3121(4) 0.2357(3) 0.0385(4) 0.0525(14) Uani 0.881(3) 1 d P . . Se3 Se 0.2968(5) 0.2206(3) 0.0007(4) 0.048(2) Uani 0.119(3) 1 d P . . C1 C 0.0468(5) 0.1322(3) 0.2356(3) 0.0430(13) Uani 1 1 d . . . C2 C 0.1352(5) 0.1105(3) 0.2835(3) 0.0543(16) Uani 1 1 d . . . C3 C 0.1485(7) 0.1330(4) 0.3512(4) 0.067(2) Uani 1 1 d . . . C4 C 0.0757(8) 0.1787(4) 0.3725(4) 0.077(2) Uani 1 1 d . . . C5 C -0.0122(9) 0.2014(4) 0.3267(5) 0.082(2) Uani 1 1 d . . . C6 C -0.0286(6) 0.1778(4) 0.2574(4) 0.0605(17) Uani 1 1 d . . . C7 C -0.0408(4) 0.0135(3) 0.1451(3) 0.0393(12) Uani 1 1 d . . . C8 C -0.0238(6) -0.0314(4) 0.2009(4) 0.069(2) Uani 1 1 d . . . C9 C -0.0712(7) -0.0993(4) 0.1989(4) 0.075(2) Uani 1 1 d . . . C10 C -0.1340(6) -0.1227(4) 0.1395(4) 0.0660(19) Uani 1 1 d . . . C11 C -0.1527(7) -0.0777(4) 0.0830(4) 0.068(2) Uani 1 1 d . . . C12 C -0.1065(6) -0.0107(4) 0.0852(3) 0.0575(17) Uani 1 1 d . . . C13 C -0.1077(4) 0.2994(3) 0.0978(3) 0.0430(13) Uani 1 1 d . . . C14 C -0.0604(6) 0.3663(3) 0.1030(3) 0.0515(16) Uani 1 1 d . . . C15 C -0.1095(7) 0.4237(3) 0.1318(3) 0.0640(19) Uani 1 1 d . . . C16 C -0.2051(6) 0.4143(4) 0.1543(3) 0.0636(18) Uani 1 1 d . . . C17 C -0.2524(6) 0.3467(4) 0.1502(4) 0.0599(17) Uani 1 1 d . . . C18 C -0.2040(5) 0.2897(3) 0.1215(3) 0.0522(15) Uani 1 1 d . . . C19 C -0.1369(4) 0.2130(3) -0.0265(3) 0.0412(12) Uani 1 1 d . . . C20 C -0.1269(6) 0.1503(3) -0.0641(4) 0.0575(16) Uani 1 1 d . . . C21 C -0.1936(7) 0.1376(4) -0.1272(4) 0.071(2) Uani 1 1 d . . . C22 C -0.2705(7) 0.1877(5) -0.1528(4) 0.076(2) Uani 1 1 d . . . C23 C -0.2803(6) 0.2509(4) -0.1174(4) 0.071(2) Uani 1 1 d . . . C24 C -0.2138(5) 0.2630(4) -0.0542(3) 0.0529(16) Uani 1 1 d . . . C25 C 0.2633(5) 0.4275(3) 0.1340(3) 0.0484(14) Uani 1 1 d . . . C26 C 0.2274(6) 0.4800(4) 0.1733(4) 0.0676(19) Uani 1 1 d . . . C27 C 0.1587(8) 0.5331(5) 0.1425(6) 0.092(3) Uani 1 1 d . . . C28 C 0.1286(7) 0.5365(4) 0.0730(5) 0.078(2) Uani 1 1 d . . . C29 C 0.1616(7) 0.4847(5) 0.0325(4) 0.084(2) Uani 1 1 d . . . C30 C 0.2298(6) 0.4294(4) 0.0624(4) 0.070(2) Uani 1 1 d . . . C31 C 0.4332(5) 0.3963(3) 0.2462(3) 0.0472(14) Uani 1 1 d . . . C32 C 0.5168(5) 0.4401(4) 0.2371(4) 0.0587(17) Uani 1 1 d . . . C33 C 0.5765(7) 0.4768(4) 0.2913(4) 0.075(2) Uani 1 1 d . . . C34 C 0.5532(7) 0.4709(5) 0.3570(4) 0.082(2) Uani 1 1 d . . . C35 C 0.4693(7) 0.4285(5) 0.3674(4) 0.078(2) Uani 1 1 d . . . C36 C 0.4092(6) 0.3901(4) 0.3134(3) 0.0636(18) Uani 1 1 d . . . C37 C 0.4568(5) 0.3180(3) -0.0137(3) 0.0558(15) Uani 1 1 d . . . C38 C 0.4136(6) 0.2944(5) -0.0806(4) 0.075(2) Uani 1 1 d . . . C39 C 0.4383(8) 0.3306(6) -0.1383(5) 0.092(3) Uani 1 1 d . . . C40 C 0.5029(9) 0.3900(6) -0.1299(5) 0.088(3) Uani 1 1 d . . . C41 C 0.5476(10) 0.4145(5) -0.0646(5) 0.096(3) Uani 1 1 d . . . C42 C 0.5225(8) 0.3782(4) -0.0075(5) 0.076(2) Uani 1 1 d . . . C43 C 0.5238(5) 0.2061(3) 0.0884(3) 0.0500(14) Uani 1 1 d . . . C44 C 0.5511(6) 0.1894(4) 0.1588(4) 0.0684(19) Uani 1 1 d . . . C45 C 0.6270(7) 0.1355(5) 0.1806(5) 0.085(2) Uani 1 1 d . . . C46 C 0.6728(7) 0.0973(4) 0.1318(5) 0.078(2) Uani 1 1 d . . . C47 C 0.6474(7) 0.1139(4) 0.0633(5) 0.076(2) Uani 1 1 d . . . C48 C 0.5724(6) 0.1678(4) 0.0417(4) 0.0660(19) Uani 1 1 d . . . H2 H 0.184(5) 0.078(3) 0.269(3) 0.060(19) Uiso 1 1 d . . . H3 H 0.208(4) 0.121(3) 0.377(3) 0.036(16) Uiso 1 1 d . . . H4 H 0.090(4) 0.197(3) 0.412(3) 0.043(16) Uiso 1 1 d . . . H5 H -0.070(7) 0.237(5) 0.342(4) 0.11(3) Uiso 1 1 d . . . H6 H -0.086(5) 0.190(3) 0.225(3) 0.046(17) Uiso 1 1 d . . . H8 H 0.018(5) -0.014(3) 0.244(3) 0.062(18) Uiso 1 1 d . . . H9 H -0.051(6) -0.124(4) 0.242(4) 0.08(2) Uiso 1 1 d . . . H10 H -0.174(5) -0.166(4) 0.145(3) 0.08(2) Uiso 1 1 d . . . H11 H -0.197(5) -0.094(3) 0.051(3) 0.043(17) Uiso 1 1 d . . . H12 H -0.115(5) 0.018(3) 0.053(3) 0.054(19) Uiso 1 1 d . . . H14 H 0.001(5) 0.373(3) 0.092(3) 0.043(17) Uiso 1 1 d . . . H15 H -0.070(4) 0.470(3) 0.135(3) 0.052(16) Uiso 1 1 d . . . H16 H -0.246(5) 0.452(3) 0.173(3) 0.059(18) Uiso 1 1 d . . . H17 H -0.321(5) 0.341(3) 0.171(3) 0.062(19) Uiso 1 1 d . . . H18 H -0.242(5) 0.246(4) 0.119(3) 0.067(19) Uiso 1 1 d . . . H20 H -0.077(4) 0.123(3) -0.041(3) 0.033(14) Uiso 1 1 d . . . H21 H -0.183(6) 0.096(4) -0.148(4) 0.08(2) Uiso 1 1 d . . . H22 H -0.306(8) 0.174(5) -0.196(5) 0.13(3) Uiso 1 1 d . . . H23 H -0.333(6) 0.286(4) -0.135(4) 0.09(2) Uiso 1 1 d . . . H24 H -0.225(5) 0.302(3) -0.036(3) 0.055(19) Uiso 1 1 d . . . H26 H 0.245(5) 0.474(3) 0.221(3) 0.061(19) Uiso 1 1 d . . . H27 H 0.139(6) 0.561(4) 0.165(4) 0.07(3) Uiso 1 1 d . . . H28 H 0.084(6) 0.572(4) 0.051(4) 0.08(2) Uiso 1 1 d . . . H29 H 0.133(6) 0.484(4) -0.016(4) 0.09(3) Uiso 1 1 d . . . H30 H 0.273(8) 0.395(5) 0.028(5) 0.14(4) Uiso 1 1 d . . . H32 H 0.541(6) 0.440(4) 0.198(4) 0.08(3) Uiso 1 1 d . . . H33 H 0.636(5) 0.501(3) 0.283(3) 0.06(2) Uiso 1 1 d . . . H34 H 0.586(6) 0.499(4) 0.399(4) 0.10(3) Uiso 1 1 d . . . H35 H 0.463(6) 0.425(4) 0.410(4) 0.07(2) Uiso 1 1 d . . . H36 H 0.348(5) 0.356(3) 0.315(3) 0.063(19) Uiso 1 1 d . . . H38 H 0.371(6) 0.245(4) -0.090(4) 0.09(2) Uiso 1 1 d . . . H39 H 0.411(7) 0.316(5) -0.189(4) 0.11(3) Uiso 1 1 d . . . H40 H 0.524(7) 0.412(4) -0.163(5) 0.10(3) Uiso 1 1 d . . . H41 H 0.588(7) 0.446(5) -0.054(5) 0.09(3) Uiso 1 1 d . . . H42 H 0.566(6) 0.383(4) 0.025(4) 0.07(3) Uiso 1 1 d . . . H44 H 0.507(8) 0.215(5) 0.197(5) 0.15(4) Uiso 1 1 d . . . H45 H 0.642(5) 0.125(3) 0.225(3) 0.059(19) Uiso 1 1 d . . . H46 H 0.720(5) 0.064(3) 0.145(3) 0.043(16) Uiso 1 1 d . . . H47 H 0.678(6) 0.093(4) 0.037(4) 0.08(3) Uiso 1 1 d . . . H48 H 0.562(5) 0.176(3) -0.001(3) 0.044(17) Uiso 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 Co 0.0362(4) 0.0406(4) 0.0447(4) 0.0028(3) 0.0045(3) -0.0007(3) Se1 0.0483(4) 0.0402(3) 0.0561(4) 0.0056(3) 0.0124(3) 0.0066(3) O1 0.039(2) 0.053(2) 0.061(2) 0.015(2) -0.0021(18) 0.0040(18) P1 0.0406(8) 0.0321(7) 0.0411(8) 0.0076(6) 0.0042(6) 0.0031(6) P2 0.0363(7) 0.0368(7) 0.0464(8) 0.0117(6) -0.0003(6) 0.0004(6) N1 0.042(3) 0.043(3) 0.058(3) 0.017(2) 0.003(2) 0.002(2) N2 0.046(3) 0.051(3) 0.059(3) -0.016(2) 0.006(2) -0.006(2) Se2 0.0563(5) 0.0403(4) 0.0430(5) -0.0015(3) 0.0090(3) -0.0071(3) P3 0.0408(8) 0.0359(7) 0.0496(8) -0.0004(6) 0.0023(6) 0.0010(6) P4 0.0446(8) 0.0439(8) 0.0573(9) -0.0085(7) 0.0029(7) -0.0010(7) O2 0.043(3) 0.060(3) 0.057(4) -0.009(3) 0.015(3) -0.008(2) Se3 0.039(3) 0.059(4) 0.049(4) -0.019(3) 0.016(3) -0.025(2) C1 0.054(3) 0.031(3) 0.045(3) 0.002(2) 0.012(3) -0.002(2) C2 0.061(4) 0.053(4) 0.045(4) -0.004(3) -0.005(3) -0.002(3) C3 0.078(5) 0.071(5) 0.047(4) -0.001(4) -0.008(4) -0.019(4) C4 0.122(8) 0.069(5) 0.042(4) -0.015(4) 0.016(5) -0.031(5) C5 0.127(8) 0.050(4) 0.080(6) -0.015(4) 0.046(6) -0.007(4) C6 0.074(5) 0.051(4) 0.058(4) 0.007(3) 0.017(4) 0.005(3) C7 0.049(3) 0.031(3) 0.039(3) 0.001(2) 0.010(2) 0.002(2) C8 0.088(5) 0.052(4) 0.057(4) 0.019(3) -0.013(4) -0.016(4) C9 0.108(6) 0.053(4) 0.059(4) 0.017(4) -0.004(4) -0.024(4) C10 0.075(5) 0.040(4) 0.087(5) -0.003(4) 0.026(4) -0.012(3) C11 0.080(5) 0.052(4) 0.069(5) -0.016(4) 0.005(4) -0.021(4) C12 0.076(5) 0.053(4) 0.043(4) 0.007(3) 0.008(3) -0.007(3) C13 0.047(3) 0.041(3) 0.037(3) 0.010(2) -0.004(2) 0.001(2) C14 0.067(4) 0.045(4) 0.039(3) 0.004(3) -0.002(3) -0.015(3) C15 0.103(6) 0.039(4) 0.043(4) -0.002(3) -0.007(4) -0.005(4) C16 0.080(5) 0.054(4) 0.052(4) -0.013(3) 0.000(4) 0.013(4) C17 0.057(4) 0.059(4) 0.062(4) -0.008(3) 0.006(3) 0.002(3) C18 0.057(4) 0.040(3) 0.057(4) 0.001(3) 0.003(3) 0.000(3) C19 0.040(3) 0.038(3) 0.046(3) 0.007(2) 0.007(2) 0.003(2) C20 0.058(4) 0.047(4) 0.066(4) 0.007(3) 0.007(3) 0.008(3) C21 0.084(5) 0.059(4) 0.068(5) -0.018(4) 0.011(4) -0.006(4) C22 0.073(5) 0.084(5) 0.065(5) -0.012(4) -0.008(4) 0.002(4) C23 0.065(5) 0.078(5) 0.062(4) 0.002(4) -0.009(4) 0.019(4) C24 0.054(4) 0.048(4) 0.051(4) -0.001(3) -0.005(3) 0.014(3) C25 0.049(3) 0.044(3) 0.050(3) 0.008(3) 0.003(3) -0.006(3) C26 0.082(5) 0.061(4) 0.058(4) -0.001(4) 0.007(4) 0.028(4) C27 0.105(7) 0.065(5) 0.102(7) -0.009(5) 0.009(6) 0.034(5) C28 0.077(5) 0.061(5) 0.091(6) 0.019(5) -0.003(4) 0.018(4) C29 0.099(6) 0.084(6) 0.062(5) 0.025(4) -0.006(4) 0.017(5) C30 0.079(5) 0.073(5) 0.055(4) 0.007(4) -0.003(4) 0.021(4) C31 0.042(3) 0.046(3) 0.051(3) 0.002(3) 0.000(3) 0.007(3) C32 0.055(4) 0.052(4) 0.065(5) -0.004(3) -0.003(4) -0.002(3) C33 0.066(5) 0.080(5) 0.072(5) -0.015(4) -0.007(4) -0.014(4) C34 0.082(6) 0.082(5) 0.070(5) -0.020(4) -0.022(4) -0.001(5) C35 0.090(6) 0.090(6) 0.047(4) -0.008(4) -0.005(4) 0.013(5) C36 0.065(4) 0.065(4) 0.057(4) 0.003(3) 0.000(3) -0.004(4) C37 0.053(4) 0.053(4) 0.060(4) -0.008(3) 0.004(3) 0.006(3) C38 0.077(5) 0.079(5) 0.067(5) -0.005(4) 0.006(4) 0.014(4) C39 0.098(7) 0.114(8) 0.063(5) -0.005(5) 0.007(5) 0.021(6) C40 0.106(7) 0.093(7) 0.072(6) 0.023(5) 0.031(5) 0.030(6) C41 0.133(9) 0.070(6) 0.088(7) -0.002(5) 0.028(6) -0.017(6) C42 0.092(6) 0.069(5) 0.064(5) 0.005(4) 0.005(5) -0.001(4) C43 0.046(3) 0.042(3) 0.062(4) -0.004(3) 0.009(3) -0.004(3) C44 0.065(4) 0.066(4) 0.077(5) 0.008(4) 0.020(4) 0.013(4) C45 0.091(6) 0.084(6) 0.082(6) 0.033(5) 0.017(5) 0.020(5) C46 0.070(5) 0.049(4) 0.114(7) 0.017(4) 0.018(5) 0.014(4) C47 0.069(5) 0.054(4) 0.107(7) -0.014(5) 0.020(5) 0.015(4) C48 0.071(5) 0.061(4) 0.063(5) -0.009(4) 0.005(4) 0.006(4) _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 Co O1 1.952(4) . ? Co O2 1.970(6) . ? Co O3 2.12(5) . ? Co Se3 2.376(7) . ? Co Se2 2.4310(11) . ? Co Se1 2.4566(11) . ? Se1 P1 2.1802(16) . ? O1 P2 1.538(4) . ? P1 N1 1.576(4) . ? P1 C7 1.815(5) . ? P1 C1 1.816(6) . ? P2 N1 1.585(4) . ? P2 C19 1.801(5) . ? P2 C13 1.809(6) . ? N2 P3 1.569(5) . ? N2 P4 1.584(5) . ? Se2 O3 0.84(6) . ? Se2 P3 2.1834(17) . ? O3 P3 1.59(5) . ? P3 C31 1.800(6) . ? P3 C25 1.813(6) . ? P4 O2 1.554(6) . ? P4 C37 1.780(7) . ? P4 C43 1.803(6) . ? P4 Se3 2.051(7) . ? O2 Se3 0.781(5) . ? C1 C2 1.384(8) . ? C1 C6 1.389(9) . ? C2 C3 1.369(9) . ? C2 H2 0.95(6) . ? C3 C4 1.362(12) . ? C3 H3 0.85(5) . ? C4 C5 1.363(12) . ? C4 H4 0.84(6) . ? C5 C6 1.404(10) . ? C5 H5 1.07(9) . ? C6 H6 0.90(6) . ? C7 C8 1.358(8) . ? C7 C12 1.385(8) . ? C8 C9 1.386(9) . ? C8 H8 0.97(6) . ? C9 C10 1.357(10) . ? C9 H9 0.95(7) . ? C10 C11 1.370(10) . ? C10 H10 0.97(7) . ? C11 C12 1.365(9) . ? C11 H11 0.82(6) . ? C12 H12 0.82(6) . ? C13 C14 1.368(8) . ? C13 C18 1.382(8) . ? C14 C15 1.394(10) . ? C14 H14 0.85(6) . ? C15 C16 1.362(10) . ? C15 H15 0.99(6) . ? C16 C17 1.380(9) . ? C16 H16 0.97(6) . ? C17 C18 1.382(9) . ? C17 H17 1.01(6) . ? C18 H18 0.94(7) . ? C19 C24 1.381(8) . ? C19 C20 1.387(8) . ? C20 C21 1.387(10) . ? C20 H20 0.87(5) . ? C21 C22 1.370(11) . ? C21 H21 0.89(8) . ? C22 C23 1.374(11) . ? C22 H22 0.92(9) . ? C23 C24 1.385(9) . ? C23 H23 0.95(8) . ? C24 H24 0.83(6) . ? C25 C26 1.360(9) . ? C25 C30 1.391(9) . ? C26 C27 1.376(11) . ? C26 H26 0.92(6) . ? C27 C28 1.346(12) . ? C27 H27 0.74(7) . ? C28 C29 1.351(11) . ? C28 H28 0.93(7) . ? C29 C30 1.396(10) . ? C29 H29 0.96(7) . ? C30 H30 1.13(10) . ? C31 C32 1.364(9) . ? C31 C36 1.402(9) . ? C32 C33 1.369(10) . ? C32 H32 0.87(7) . ? C33 C34 1.369(11) . ? C33 H33 0.91(6) . ? C34 C35 1.358(12) . ? C34 H34 1.00(8) . ? C35 C36 1.383(10) . ? C35 H35 0.85(7) . ? C36 H36 1.00(6) . ? C37 C42 1.378(10) . ? C37 C38 1.397(9) . ? C38 C39 1.391(12) . ? C38 H38 1.06(8) . ? C39 C40 1.360(13) . ? C39 H39 1.03(8) . ? C40 C41 1.380(14) . ? C40 H40 0.85(8) . ? C41 C42 1.383(12) . ? C41 H41 0.77(8) . ? C42 H42 0.78(7) . ? C43 C48 1.378(9) . ? C43 C44 1.393(9) . ? C44 C45 1.394(10) . ? C44 H44 1.11(10) . ? C45 C46 1.389(12) . ? C45 H45 0.88(6) . ? C46 C47 1.356(12) . ? C46 H46 0.87(6) . ? C47 C48 1.386(10) . ? C47 H47 0.80(7) . ? C48 H48 0.83(5) . ? 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 O1 Co O2 108.0(2) . . ? O1 Co O3 117.6(12) . . ? O2 Co O3 89.5(15) . . ? O1 Co Se3 96.6(2) . . ? O2 Co Se3 17.73(18) . . ? O3 Co Se3 106.9(16) . . ? O1 Co Se2 114.58(13) . . ? O2 Co Se2 108.5(2) . . ? O3 Co Se2 19.9(16) . . ? Se3 Co Se2 126.21(16) . . ? O1 Co Se1 106.16(12) . . ? O2 Co Se1 112.50(17) . . ? O3 Co Se1 121.5(14) . . ? Se3 Co Se1 104.22(16) . . ? Se2 Co Se1 107.18(4) . . ? P1 Se1 Co 91.76(4) . . ? P2 O1 Co 126.1(2) . . ? N1 P1 C7 107.1(2) . . ? N1 P1 C1 110.7(3) . . ? C7 P1 C1 106.6(2) . . ? N1 P1 Se1 117.04(19) . . ? C7 P1 Se1 106.79(18) . . ? C1 P1 Se1 108.12(19) . . ? O1 P2 N1 118.1(2) . . ? O1 P2 C19 108.8(2) . . ? N1 P2 C19 106.5(2) . . ? O1 P2 C13 108.2(2) . . ? N1 P2 C13 108.9(3) . . ? C19 P2 C13 105.6(2) . . ? P1 N1 P2 135.7(3) . . ? P3 N2 P4 133.9(3) . . ? O3 Se2 P3 37(3) . . ? O3 Se2 Co 59(3) . . ? P3 Se2 Co 94.88(5) . . ? Se2 O3 P3 124(4) . . ? Se2 O3 Co 101(4) . . ? P3 O3 Co 132(3) . . ? N2 P3 O3 101.9(19) . . ? N2 P3 C31 107.2(3) . . ? O3 P3 C31 124.6(19) . . ? N2 P3 C25 110.4(3) . . ? O3 P3 C25 108.7(16) . . ? C31 P3 C25 103.9(3) . . ? N2 P3 Se2 117.92(19) . . ? O3 P3 Se2 19(2) . . ? C31 P3 Se2 108.2(2) . . ? C25 P3 Se2 108.32(19) . . ? O2 P4 N2 116.5(3) . . ? O2 P4 C37 108.2(3) . . ? N2 P4 C37 107.7(3) . . ? O2 P4 C43 108.7(3) . . ? N2 P4 C43 107.6(3) . . ? C37 P4 C43 107.8(3) . . ? O2 P4 Se3 19.4(2) . . ? N2 P4 Se3 133.3(3) . . ? C37 P4 Se3 91.6(3) . . ? C43 P4 Se3 106.0(3) . . ? Se3 O2 P4 119.2(8) . . ? Se3 O2 Co 112.0(7) . . ? P4 O2 Co 128.7(5) . . ? O2 Se3 P4 41.4(6) . . ? O2 Se3 Co 50.2(6) . . ? P4 Se3 Co 91.6(3) . . ? C2 C1 C6 118.8(6) . . ? C2 C1 P1 122.8(5) . . ? C6 C1 P1 118.4(5) . . ? C3 C2 C1 121.0(7) . . ? C3 C2 H2 121(4) . . ? C1 C2 H2 118(4) . . ? C4 C3 C2 120.4(8) . . ? C4 C3 H3 124(4) . . ? C2 C3 H3 115(4) . . ? C3 C4 C5 120.2(7) . . ? C3 C4 H4 119(4) . . ? C5 C4 H4 120(4) . . ? C4 C5 C6 120.4(8) . . ? C4 C5 H5 121(4) . . ? C6 C5 H5 118(5) . . ? C1 C6 C5 119.2(7) . . ? C1 C6 H6 116(4) . . ? C5 C6 H6 125(4) . . ? C8 C7 C12 118.0(5) . . ? C8 C7 P1 122.2(4) . . ? C12 C7 P1 119.8(4) . . ? C7 C8 C9 121.5(6) . . ? C7 C8 H8 119(4) . . ? C9 C8 H8 119(4) . . ? C10 C9 C8 119.8(7) . . ? C10 C9 H9 129(5) . . ? C8 C9 H9 111(5) . . ? C9 C10 C11 119.3(6) . . ? C9 C10 H10 115(4) . . ? C11 C10 H10 125(4) . . ? C12 C11 C10 120.7(7) . . ? C12 C11 H11 127(4) . . ? C10 C11 H11 112(4) . . ? C11 C12 C7 120.6(6) . . ? C11 C12 H12 124(4) . . ? C7 C12 H12 115(4) . . ? C14 C13 C18 119.2(6) . . ? C14 C13 P2 121.0(5) . . ? C18 C13 P2 119.8(4) . . ? C13 C14 C15 120.0(7) . . ? C13 C14 H14 122(4) . . ? C15 C14 H14 118(4) . . ? C16 C15 C14 120.7(6) . . ? C16 C15 H15 124(3) . . ? C14 C15 H15 115(3) . . ? C15 C16 C17 119.6(7) . . ? C15 C16 H16 126(4) . . ? C17 C16 H16 115(4) . . ? C16 C17 C18 119.8(7) . . ? C16 C17 H17 117(4) . . ? C18 C17 H17 123(4) . . ? C13 C18 C17 120.7(6) . . ? C13 C18 H18 124(4) . . ? C17 C18 H18 115(4) . . ? C24 C19 C20 118.2(6) . . ? C24 C19 P2 123.0(4) . . ? C20 C19 P2 118.8(4) . . ? C19 C20 C21 121.0(6) . . ? C19 C20 H20 109(3) . . ? C21 C20 H20 130(3) . . ? C22 C21 C20 119.5(7) . . ? C22 C21 H21 124(5) . . ? C20 C21 H21 117(5) . . ? C21 C22 C23 120.6(7) . . ? C21 C22 H22 111(6) . . ? C23 C22 H22 128(6) . . ? C22 C23 C24 119.6(7) . . ? C22 C23 H23 121(5) . . ? C24 C23 H23 119(5) . . ? C19 C24 C23 121.1(6) . . ? C19 C24 H24 125(4) . . ? C23 C24 H24 114(4) . . ? C26 C25 C30 118.6(6) . . ? C26 C25 P3 122.5(5) . . ? C30 C25 P3 119.0(5) . . ? C25 C26 C27 120.4(8) . . ? C25 C26 H26 116(4) . . ? C27 C26 H26 123(4) . . ? C28 C27 C26 121.3(9) . . ? C28 C27 H27 119(6) . . ? C26 C27 H27 120(6) . . ? C27 C28 C29 119.8(8) . . ? C27 C28 H28 123(5) . . ? C29 C28 H28 117(5) . . ? C28 C29 C30 120.1(8) . . ? C28 C29 H29 120(5) . . ? C30 C29 H29 120(5) . . ? C25 C30 C29 119.7(7) . . ? C25 C30 H30 119(5) . . ? C29 C30 H30 120(5) . . ? C32 C31 C36 117.8(6) . . ? C32 C31 P3 119.4(5) . . ? C36 C31 P3 122.6(5) . . ? C31 C32 C33 121.8(8) . . ? C31 C32 H32 121(5) . . ? C33 C32 H32 116(5) . . ? C32 C33 C34 120.5(8) . . ? C32 C33 H33 117(4) . . ? C34 C33 H33 122(4) . . ? C35 C34 C33 118.9(7) . . ? C35 C34 H34 114(5) . . ? C33 C34 H34 127(5) . . ? C34 C35 C36 121.3(8) . . ? C34 C35 H35 113(5) . . ? C36 C35 H35 125(5) . . ? C35 C36 C31 119.6(7) . . ? C35 C36 H36 128(4) . . ? C31 C36 H36 112(4) . . ? C42 C37 C38 117.7(7) . . ? C42 C37 P4 121.6(5) . . ? C38 C37 P4 120.6(6) . . ? C39 C38 C37 120.2(8) . . ? C39 C38 H38 117(4) . . ? C37 C38 H38 122(4) . . ? C40 C39 C38 120.2(9) . . ? C40 C39 H39 114(5) . . ? C38 C39 H39 125(5) . . ? C39 C40 C41 121.0(9) . . ? C39 C40 H40 124(6) . . ? C41 C40 H40 115(6) . . ? C40 C41 C42 118.3(10) . . ? C40 C41 H41 129(7) . . ? C42 C41 H41 113(7) . . ? C37 C42 C41 122.5(9) . . ? C37 C42 H42 120(6) . . ? C41 C42 H42 112(6) . . ? C48 C43 C44 118.5(6) . . ? C48 C43 P4 121.9(5) . . ? C44 C43 P4 119.5(5) . . ? C43 C44 C45 120.0(7) . . ? C43 C44 H44 120(5) . . ? C45 C44 H44 119(5) . . ? C46 C45 C44 119.7(8) . . ? C46 C45 H45 122(4) . . ? C44 C45 H45 119(4) . . ? C47 C46 C45 120.5(8) . . ? C47 C46 H46 119(4) . . ? C45 C46 H46 120(4) . . ? C46 C47 C48 119.6(8) . . ? C46 C47 H47 118(6) . . ? C48 C47 H47 122(6) . . ? C43 C48 C47 121.6(8) . . ? C43 C48 H48 124(4) . . ? C47 C48 H48 115(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.989 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.088 # start Validation Reply Form _vrf_THETM01_Complex1 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The crystals had poor diffraction ability; the data were collected in icreasing twotheta shells and the data collection was terminated when almost half of the collected shell data were unobserved. ; # end Validation Reply Form #===END data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 764425' #TrackingRef '- Ferentinos_Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 N2 Ni O2 P4 Se2' _chemical_formula_weight 1017.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.602(5) _cell_length_b 18.425(7) _cell_length_c 19.582(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.140(10) _cell_angle_gamma 90.00 _cell_volume 4476(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 11.0 _exptl_crystal_description parall _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 2.244 _exptl_absorpt_correction_type 'psi scan empirical' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Crystal Logic Dual Goniometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.5 _diffrn_reflns_number 6837 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.51 _reflns_number_total 6616 _reflns_number_gt 4956 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+8.7905P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6616 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.20223(7) 0.21268(5) 0.09041(5) 0.0446(3) Uani 1 1 d . . . Se1 Se 0.17635(6) 0.08558(4) 0.11429(4) 0.0484(2) Uani 1 1 d . . . O1 O 0.0626(4) 0.2464(3) 0.0432(2) 0.0501(12) Uani 1 1 d . . . P1 P 0.02090(13) 0.10145(8) 0.14603(9) 0.0369(4) Uani 1 1 d . . . P2 P -0.05150(13) 0.22422(9) 0.05641(9) 0.0395(4) Uani 1 1 d . . . N1 N -0.0625(4) 0.1525(3) 0.0994(3) 0.0444(13) Uani 1 1 d . . . N2 N 0.4315(5) 0.3340(3) 0.1194(3) 0.0519(15) Uani 1 1 d . . . Se2 Se 0.25361(8) 0.26856(5) 0.20246(5) 0.0463(3) Uani 0.923(4) 1 d P . . O3 O 0.280(6) 0.285(4) 0.183(4) 0.03(2) Uiso 0.077(4) 1 d P . . P3 P 0.35261(14) 0.35495(9) 0.17013(9) 0.0400(4) Uani 1 1 d . . . P4 P 0.42398(14) 0.27507(10) 0.05966(10) 0.0450(4) Uani 1 1 d . . . O2 O 0.3135(6) 0.2370(4) 0.0371(5) 0.0533(19) Uani 0.923(4) 1 d P . . Se3 Se 0.2960(11) 0.2199(7) 0.0077(7) 0.046(4) Uani 0.077(4) 1 d P . . C1 C 0.0446(6) 0.1321(3) 0.2360(3) 0.0418(16) Uani 1 1 d . . . C2 C 0.1348(6) 0.1104(4) 0.2823(4) 0.0525(18) Uani 1 1 d . . . C3 C 0.1473(9) 0.1337(5) 0.3510(4) 0.069(3) Uani 1 1 d . . . C4 C 0.0748(10) 0.1795(5) 0.3723(5) 0.078(3) Uani 1 1 d . . . C5 C -0.0132(10) 0.2019(5) 0.3266(6) 0.076(3) Uani 1 1 d . . . C6 C -0.0292(7) 0.1781(4) 0.2582(4) 0.057(2) Uani 1 1 d . . . C7 C -0.0416(5) 0.0128(3) 0.1454(3) 0.0399(15) Uani 1 1 d . . . C8 C -0.0253(8) -0.0309(4) 0.2023(4) 0.069(2) Uani 1 1 d . . . C9 C -0.0720(9) -0.1002(5) 0.1991(5) 0.080(3) Uani 1 1 d . . . C10 C -0.1344(7) -0.1237(4) 0.1410(5) 0.062(2) Uani 1 1 d . . . C11 C -0.1517(9) -0.0799(5) 0.0838(5) 0.066(3) Uani 1 1 d . . . C12 C -0.1050(7) -0.0120(4) 0.0849(4) 0.057(2) Uani 1 1 d . . . C13 C -0.1085(5) 0.2988(3) 0.0971(3) 0.0410(15) Uani 1 1 d . . . C14 C -0.0579(7) 0.3666(4) 0.1033(4) 0.0542(19) Uani 1 1 d . . . C15 C -0.1075(9) 0.4245(4) 0.1313(4) 0.064(2) Uani 1 1 d . . . C16 C -0.2037(8) 0.4154(5) 0.1540(4) 0.068(2) Uani 1 1 d . . . C17 C -0.2525(8) 0.3476(5) 0.1486(4) 0.060(2) Uani 1 1 d . . . C18 C -0.2040(6) 0.2902(4) 0.1205(4) 0.0516(18) Uani 1 1 d . . . C19 C -0.1380(5) 0.2123(3) -0.0268(3) 0.0380(14) Uani 1 1 d . . . C20 C -0.1284(7) 0.1497(4) -0.0652(4) 0.0537(19) Uani 1 1 d . . . C21 C -0.1929(8) 0.1379(5) -0.1272(4) 0.066(2) Uani 1 1 d . . . C22 C -0.2695(8) 0.1880(6) -0.1532(5) 0.072(2) Uani 1 1 d . . . C23 C -0.2812(7) 0.2506(5) -0.1181(4) 0.066(2) Uani 1 1 d . . . C24 C -0.2135(6) 0.2625(4) -0.0549(4) 0.0529(19) Uani 1 1 d . . . C25 C 0.2640(5) 0.4279(3) 0.1327(4) 0.0425(16) Uani 1 1 d . . . C26 C 0.2312(8) 0.4809(5) 0.1730(5) 0.067(2) Uani 1 1 d . . . C27 C 0.1604(9) 0.5344(5) 0.1417(7) 0.088(3) Uani 1 1 d . . . C28 C 0.1291(8) 0.5372(5) 0.0725(6) 0.077(3) Uani 1 1 d . . . C29 C 0.1606(9) 0.4848(6) 0.0339(6) 0.085(3) Uani 1 1 d . . . C30 C 0.2294(7) 0.4303(5) 0.0623(4) 0.066(2) Uani 1 1 d . . . C31 C 0.4324(5) 0.3944(3) 0.2465(4) 0.0434(16) Uani 1 1 d . . . C32 C 0.5180(6) 0.4398(4) 0.2382(4) 0.0530(18) Uani 1 1 d . . . C33 C 0.5750(8) 0.4758(5) 0.2934(5) 0.074(3) Uani 1 1 d . . . C34 C 0.5499(9) 0.4698(5) 0.3582(6) 0.080(3) Uani 1 1 d . . . C35 C 0.4663(9) 0.4260(6) 0.3680(5) 0.078(3) Uani 1 1 d . . . C36 C 0.4079(7) 0.3882(5) 0.3119(4) 0.061(2) Uani 1 1 d . . . C37 C 0.4572(5) 0.3193(4) -0.0160(4) 0.0482(17) Uani 1 1 d . . . C38 C 0.4156(7) 0.2953(6) -0.0811(5) 0.067(2) Uani 1 1 d . . . C39 C 0.4390(9) 0.3304(6) -0.1387(5) 0.081(3) Uani 1 1 d . . . C40 C 0.5044(10) 0.3895(6) -0.1315(6) 0.084(3) Uani 1 1 d . . . C41 C 0.5465(10) 0.4152(5) -0.0678(6) 0.085(3) Uani 1 1 d . . . C42 C 0.5241(8) 0.3792(5) -0.0098(5) 0.071(2) Uani 1 1 d . . . C43 C 0.5246(5) 0.2061(4) 0.0869(4) 0.0478(17) Uani 1 1 d . . . C44 C 0.5522(7) 0.1896(5) 0.1566(5) 0.069(2) Uani 1 1 d . . . C45 C 0.6262(9) 0.1343(6) 0.1783(6) 0.084(3) Uani 1 1 d . . . C46 C 0.6729(8) 0.0967(5) 0.1314(7) 0.081(3) Uani 1 1 d . . . C47 C 0.6485(8) 0.1130(5) 0.0628(6) 0.073(3) Uani 1 1 d . . . C48 C 0.5727(7) 0.1676(4) 0.0402(5) 0.062(2) Uani 1 1 d . . . H2 H 0.194(7) 0.078(4) 0.270(4) 0.07(2) Uiso 1 1 d . . . H3 H 0.205(7) 0.125(4) 0.379(4) 0.06(3) Uiso 1 1 d . . . H4 H 0.092(7) 0.198(5) 0.419(5) 0.08(3) Uiso 1 1 d . . . H5 H -0.074(9) 0.228(6) 0.340(5) 0.11(4) Uiso 1 1 d . . . H6 H -0.085(6) 0.197(4) 0.229(4) 0.05(2) Uiso 1 1 d . . . H8 H 0.015(7) -0.017(5) 0.245(5) 0.09(3) Uiso 1 1 d . . . H9 H -0.058(7) -0.127(5) 0.242(5) 0.08(3) Uiso 1 1 d . . . H10 H -0.176(7) -0.167(5) 0.138(5) 0.09(3) Uiso 1 1 d . . . H11 H -0.180(7) -0.089(5) 0.051(4) 0.06(3) Uiso 1 1 d . . . H12 H -0.116(8) 0.020(5) 0.053(5) 0.09(3) Uiso 1 1 d . . . H14 H 0.008(9) 0.374(6) 0.074(6) 0.12(4) Uiso 1 1 d . . . H15 H -0.068(7) 0.473(5) 0.131(4) 0.08(3) Uiso 1 1 d . . . H16 H -0.233(7) 0.455(5) 0.172(4) 0.07(3) Uiso 1 1 d . . . H17 H -0.312(6) 0.348(4) 0.161(4) 0.05(2) Uiso 1 1 d . . . H18 H -0.240(6) 0.246(4) 0.109(4) 0.07(2) Uiso 1 1 d . . . H20 H -0.071(5) 0.125(3) -0.041(3) 0.038(18) Uiso 1 1 d . . . H21 H -0.177(7) 0.095(5) -0.151(5) 0.08(3) Uiso 1 1 d . . . H22 H -0.315(6) 0.182(4) -0.196(4) 0.07(2) Uiso 1 1 d . . . H23 H -0.333(7) 0.287(5) -0.136(4) 0.08(3) Uiso 1 1 d . . . H24 H -0.226(5) 0.300(4) -0.036(3) 0.04(2) Uiso 1 1 d . . . H26 H 0.239(7) 0.475(5) 0.216(4) 0.07(3) Uiso 1 1 d . . . H27 H 0.144(6) 0.562(4) 0.164(4) 0.04(2) Uiso 1 1 d . . . H28 H 0.083(6) 0.574(4) 0.056(4) 0.05(2) Uiso 1 1 d . . . H29 H 0.139(7) 0.485(5) -0.010(4) 0.07(3) Uiso 1 1 d . . . H30 H 0.267(7) 0.395(5) 0.037(4) 0.08(3) Uiso 1 1 d . . . H32 H 0.537(5) 0.438(3) 0.199(3) 0.026(16) Uiso 1 1 d . . . H33 H 0.631(6) 0.502(4) 0.297(4) 0.06(2) Uiso 1 1 d . . . H34 H 0.595(6) 0.489(4) 0.402(4) 0.07(2) Uiso 1 1 d . . . H35 H 0.458(7) 0.418(4) 0.409(5) 0.07(3) Uiso 1 1 d . . . H36 H 0.346(6) 0.360(4) 0.316(4) 0.06(2) Uiso 1 1 d . . . H38 H 0.379(8) 0.255(5) -0.077(5) 0.09(3) Uiso 1 1 d . . . H39 H 0.397(6) 0.309(4) -0.179(4) 0.06(2) Uiso 1 1 d . . . H40 H 0.533(9) 0.420(6) -0.167(6) 0.13(4) Uiso 1 1 d . . . H41 H 0.586(7) 0.455(5) -0.061(4) 0.08(3) Uiso 1 1 d . . . H42 H 0.540(6) 0.398(4) 0.029(4) 0.05(2) Uiso 1 1 d . . . H44 H 0.527(6) 0.217(4) 0.191(4) 0.06(2) Uiso 1 1 d . . . H45 H 0.638(6) 0.130(4) 0.223(4) 0.06(3) Uiso 1 1 d . . . H46 H 0.737(8) 0.055(5) 0.155(5) 0.10(3) Uiso 1 1 d . . . H47 H 0.672(7) 0.083(5) 0.025(5) 0.09(3) Uiso 1 1 d . . . H48 H 0.563(8) 0.179(5) -0.008(5) 0.10(3) Uiso 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 0.0322(5) 0.0468(5) 0.0545(6) 0.0031(4) 0.0068(4) -0.0048(4) Se1 0.0444(4) 0.0453(4) 0.0575(5) 0.0040(3) 0.0145(3) 0.0060(3) O1 0.035(2) 0.065(3) 0.046(3) 0.012(2) -0.007(2) 0.007(2) P1 0.0379(9) 0.0339(8) 0.0388(9) 0.0077(7) 0.0069(7) 0.0022(7) P2 0.0326(9) 0.0395(9) 0.0440(10) 0.0125(7) 0.0000(7) -0.0015(7) N1 0.034(3) 0.046(3) 0.052(3) 0.015(3) 0.004(3) 0.002(2) N2 0.046(3) 0.053(3) 0.059(4) -0.016(3) 0.015(3) -0.007(3) Se2 0.0530(6) 0.0434(5) 0.0436(5) -0.0004(4) 0.0112(4) -0.0069(4) P3 0.0356(9) 0.0369(8) 0.0460(10) -0.0021(7) 0.0029(8) 0.0008(7) P4 0.0372(9) 0.0476(10) 0.0509(11) -0.0093(8) 0.0094(8) -0.0046(8) O2 0.041(4) 0.065(5) 0.058(5) -0.020(4) 0.019(4) -0.017(3) Se3 0.035(6) 0.058(7) 0.046(8) -0.027(6) 0.015(6) -0.032(5) C1 0.052(4) 0.028(3) 0.047(4) 0.004(3) 0.014(3) -0.004(3) C2 0.057(5) 0.054(4) 0.044(4) 0.006(3) 0.001(4) 0.001(4) C3 0.089(7) 0.074(6) 0.039(5) 0.002(4) -0.003(5) -0.030(5) C4 0.117(9) 0.061(5) 0.059(6) -0.018(5) 0.028(6) -0.029(6) C5 0.105(8) 0.052(5) 0.082(7) -0.007(5) 0.048(7) -0.002(5) C6 0.074(6) 0.050(4) 0.052(5) 0.003(4) 0.020(4) 0.010(4) C7 0.040(4) 0.039(3) 0.042(4) 0.003(3) 0.013(3) 0.004(3) C8 0.101(7) 0.052(5) 0.047(5) 0.016(4) -0.003(5) -0.023(5) C9 0.109(8) 0.058(5) 0.072(6) 0.017(5) 0.011(6) -0.017(5) C10 0.066(5) 0.043(4) 0.081(6) -0.006(4) 0.025(5) -0.014(4) C11 0.086(7) 0.064(5) 0.048(5) -0.013(4) 0.013(5) -0.017(5) C12 0.075(6) 0.044(4) 0.049(5) -0.001(4) 0.007(4) -0.005(4) C13 0.042(4) 0.042(3) 0.035(3) 0.009(3) -0.005(3) -0.002(3) C14 0.067(5) 0.046(4) 0.048(4) 0.002(3) 0.005(4) -0.014(4) C15 0.105(7) 0.042(4) 0.041(4) 0.004(3) -0.001(4) -0.005(4) C16 0.093(7) 0.052(5) 0.054(5) -0.012(4) 0.000(5) 0.006(5) C17 0.062(6) 0.064(5) 0.055(5) -0.005(4) 0.012(4) 0.008(4) C18 0.051(4) 0.042(4) 0.060(5) -0.001(3) 0.003(4) -0.002(3) C19 0.038(3) 0.037(3) 0.039(4) 0.008(3) 0.006(3) -0.004(3) C20 0.054(5) 0.050(4) 0.057(5) 0.003(4) 0.007(4) 0.011(4) C21 0.079(6) 0.070(5) 0.046(5) -0.016(4) 0.007(4) -0.001(5) C22 0.067(6) 0.091(7) 0.051(5) -0.007(5) -0.004(4) -0.008(5) C23 0.059(5) 0.081(6) 0.053(5) 0.004(4) -0.010(4) 0.015(5) C24 0.051(4) 0.051(4) 0.050(5) -0.003(4) -0.007(4) 0.012(4) C25 0.035(3) 0.038(3) 0.053(4) 0.004(3) 0.002(3) -0.001(3) C26 0.078(6) 0.062(5) 0.057(6) -0.001(4) 0.000(5) 0.032(4) C27 0.095(8) 0.063(6) 0.104(9) -0.010(6) 0.016(7) 0.037(6) C28 0.065(6) 0.057(5) 0.103(8) 0.030(6) -0.003(6) 0.014(5) C29 0.093(8) 0.092(7) 0.059(6) 0.019(6) -0.014(6) 0.013(6) C30 0.073(6) 0.070(5) 0.050(5) 0.001(4) -0.005(4) 0.012(5) C31 0.037(4) 0.042(3) 0.048(4) -0.001(3) 0.001(3) 0.007(3) C32 0.046(4) 0.057(4) 0.054(5) -0.006(4) 0.003(4) 0.001(3) C33 0.053(5) 0.079(6) 0.080(7) -0.017(5) -0.014(5) -0.013(5) C34 0.082(7) 0.076(6) 0.071(7) -0.020(5) -0.019(6) 0.009(5) C35 0.094(8) 0.087(7) 0.048(6) -0.005(5) -0.001(5) 0.012(6) C36 0.068(6) 0.066(5) 0.045(5) -0.005(4) -0.003(4) 0.000(4) C37 0.041(4) 0.048(4) 0.056(5) -0.004(3) 0.008(3) 0.003(3) C38 0.062(5) 0.083(6) 0.055(5) -0.008(5) 0.005(4) -0.006(5) C39 0.084(7) 0.100(8) 0.057(6) -0.009(6) 0.005(5) 0.014(6) C40 0.096(8) 0.087(7) 0.073(7) 0.015(6) 0.023(6) 0.020(6) C41 0.104(8) 0.064(6) 0.094(8) 0.005(5) 0.032(6) -0.018(6) C42 0.087(7) 0.070(6) 0.057(6) -0.003(5) 0.017(5) -0.018(5) C43 0.040(4) 0.046(4) 0.060(5) -0.008(3) 0.016(3) -0.014(3) C44 0.064(5) 0.069(5) 0.080(7) 0.008(5) 0.026(5) 0.014(4) C45 0.081(7) 0.093(7) 0.078(7) 0.032(6) 0.017(6) 0.014(6) C46 0.065(6) 0.052(5) 0.134(10) 0.015(6) 0.038(6) 0.008(4) C47 0.074(6) 0.057(5) 0.092(7) -0.018(5) 0.023(5) 0.008(4) C48 0.057(5) 0.059(5) 0.070(6) -0.019(4) 0.012(4) -0.001(4) _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 O1 1.940(4) . ? Ni O2 1.942(7) . ? Ni Se3 2.170(13) . ? Ni O3 2.33(7) . ? Ni Se2 2.4069(15) . ? Ni Se1 2.4212(14) . ? Se1 P1 2.177(2) . ? O1 P2 1.559(5) . ? P1 N1 1.576(5) . ? P1 C7 1.812(6) . ? P1 C1 1.824(7) . ? P2 N1 1.586(5) . ? P2 C13 1.800(7) . ? P2 C19 1.808(6) . ? N2 P3 1.572(6) . ? N2 P4 1.587(6) . ? Se2 O3 0.62(8) . ? Se2 P3 2.184(2) . ? O3 P3 1.63(8) . ? P3 C31 1.801(7) . ? P3 C25 1.818(6) . ? P4 O2 1.553(8) . ? P4 C37 1.804(7) . ? P4 C43 1.808(8) . ? P4 Se3 2.023(12) . ? O2 Se3 0.659(9) . ? C1 C2 1.382(10) . ? C1 C6 1.384(10) . ? C2 C3 1.394(11) . ? C2 H2 1.02(8) . ? C3 C4 1.363(14) . ? C3 H3 0.84(8) . ? C4 C5 1.361(14) . ? C4 H4 0.96(9) . ? C5 C6 1.390(12) . ? C5 H5 0.98(11) . ? C6 H6 0.89(7) . ? C7 C8 1.362(10) . ? C7 C12 1.384(10) . ? C8 C9 1.403(12) . ? C8 H8 0.94(9) . ? C9 C10 1.336(13) . ? C9 H9 0.97(9) . ? C10 C11 1.367(13) . ? C10 H10 0.95(9) . ? C11 C12 1.380(12) . ? C11 H11 0.70(8) . ? C12 H12 0.85(9) . ? C13 C18 1.371(10) . ? C13 C14 1.399(9) . ? C14 C15 1.395(11) . ? C14 H14 1.10(11) . ? C15 C16 1.373(13) . ? C15 H15 1.03(9) . ? C16 C17 1.388(12) . ? C16 H16 0.91(8) . ? C17 C18 1.383(11) . ? C17 H17 0.83(7) . ? C18 H18 0.94(8) . ? C19 C24 1.371(9) . ? C19 C20 1.393(10) . ? C20 C21 1.355(11) . ? C20 H20 0.91(7) . ? C21 C22 1.368(13) . ? C21 H21 0.95(9) . ? C22 C23 1.364(13) . ? C22 H22 0.93(8) . ? C23 C24 1.391(11) . ? C23 H23 0.97(9) . ? C24 H24 0.82(7) . ? C25 C26 1.365(11) . ? C25 C30 1.372(11) . ? C26 C27 1.396(12) . ? C26 H26 0.84(8) . ? C27 C28 1.345(15) . ? C27 H27 0.73(7) . ? C28 C29 1.329(14) . ? C28 H28 0.92(8) . ? C29 C30 1.378(13) . ? C29 H29 0.85(8) . ? C30 H30 0.98(9) . ? C31 C36 1.374(11) . ? C31 C32 1.396(10) . ? C32 C33 1.361(11) . ? C32 H32 0.84(6) . ? C33 C34 1.365(14) . ? C33 H33 0.85(8) . ? C34 C35 1.368(14) . ? C34 H34 1.00(8) . ? C35 C36 1.395(12) . ? C35 H35 0.84(8) . ? C36 H36 0.95(7) . ? C37 C38 1.364(11) . ? C37 C42 1.380(11) . ? C38 C39 1.376(13) . ? C38 H38 0.89(9) . ? C39 C40 1.357(15) . ? C39 H39 0.96(8) . ? C40 C41 1.352(15) . ? C40 H40 1.00(12) . ? C41 C42 1.386(13) . ? C41 H41 0.89(9) . ? C42 H42 0.82(7) . ? C43 C48 1.378(10) . ? C43 C44 1.383(11) . ? C44 C45 1.395(13) . ? C44 H44 0.95(8) . ? C45 C46 1.364(14) . ? C45 H45 0.86(8) . ? C46 C47 1.358(14) . ? C46 H46 1.15(10) . ? C47 C48 1.404(12) . ? C47 H47 1.01(9) . ? C48 H48 0.96(10) . ? 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 O1 Ni O2 110.5(3) . . ? O1 Ni Se3 101.1(4) . . ? O2 Ni Se3 17.3(3) . . ? O1 Ni O3 114.4(16) . . ? O2 Ni O3 93(2) . . ? Se3 Ni O3 110(2) . . ? O1 Ni Se2 111.90(16) . . ? O2 Ni Se2 106.7(3) . . ? Se3 Ni Se2 124.0(3) . . ? O3 Ni Se2 15(2) . . ? O1 Ni Se1 105.06(15) . . ? O2 Ni Se1 117.5(2) . . ? Se3 Ni Se1 108.2(4) . . ? O3 Ni Se1 116.9(19) . . ? Se2 Ni Se1 105.16(5) . . ? P1 Se1 Ni 94.81(5) . . ? P2 O1 Ni 128.5(3) . . ? N1 P1 C7 106.8(3) . . ? N1 P1 C1 110.7(3) . . ? C7 P1 C1 106.4(3) . . ? N1 P1 Se1 117.1(2) . . ? C7 P1 Se1 106.8(2) . . ? C1 P1 Se1 108.4(2) . . ? O1 P2 N1 118.4(3) . . ? O1 P2 C13 108.9(3) . . ? N1 P2 C13 108.8(3) . . ? O1 P2 C19 108.1(3) . . ? N1 P2 C19 106.4(3) . . ? C13 P2 C19 105.5(3) . . ? P1 N1 P2 133.9(4) . . ? P3 N2 P4 132.2(4) . . ? O3 Se2 P3 23(6) . . ? O3 Se2 Ni 75(6) . . ? P3 Se2 Ni 97.08(7) . . ? Se2 O3 P3 149(8) . . ? Se2 O3 Ni 90(7) . . ? P3 O3 Ni 120(4) . . ? N2 P3 O3 110(2) . . ? N2 P3 C31 107.5(3) . . ? O3 P3 C31 116(3) . . ? N2 P3 C25 109.8(3) . . ? O3 P3 C25 109(2) . . ? C31 P3 C25 104.5(3) . . ? N2 P3 Se2 117.5(2) . . ? O3 P3 Se2 8(3) . . ? C31 P3 Se2 108.5(2) . . ? C25 P3 Se2 108.3(2) . . ? O2 P4 N2 117.0(4) . . ? O2 P4 C37 107.3(4) . . ? N2 P4 C37 107.7(3) . . ? O2 P4 C43 108.3(4) . . ? N2 P4 C43 108.4(3) . . ? C37 P4 C43 107.9(3) . . ? O2 P4 Se3 15.0(4) . . ? N2 P4 Se3 130.8(4) . . ? C37 P4 Se3 95.4(5) . . ? C43 P4 Se3 104.5(5) . . ? Se3 O2 P4 127.6(17) . . ? Se3 O2 Ni 101.4(16) . . ? P4 O2 Ni 130.3(5) . . ? O2 Se3 P4 37.5(13) . . ? O2 Se3 Ni 61.3(15) . . ? P4 Se3 Ni 98.4(6) . . ? C2 C1 C6 119.5(7) . . ? C2 C1 P1 121.3(5) . . ? C6 C1 P1 119.2(6) . . ? C1 C2 C3 119.0(8) . . ? C1 C2 H2 124(5) . . ? C3 C2 H2 117(5) . . ? C4 C3 C2 121.2(10) . . ? C4 C3 H3 118(6) . . ? C2 C3 H3 120(6) . . ? C5 C4 C3 119.9(9) . . ? C5 C4 H4 123(5) . . ? C3 C4 H4 117(5) . . ? C4 C5 C6 120.1(9) . . ? C4 C5 H5 124(6) . . ? C6 C5 H5 115(6) . . ? C1 C6 C5 120.3(9) . . ? C1 C6 H6 122(5) . . ? C5 C6 H6 117(5) . . ? C8 C7 C12 119.0(7) . . ? C8 C7 P1 121.6(6) . . ? C12 C7 P1 119.3(5) . . ? C7 C8 C9 120.0(8) . . ? C7 C8 H8 124(6) . . ? C9 C8 H8 116(6) . . ? C10 C9 C8 120.8(9) . . ? C10 C9 H9 124(5) . . ? C8 C9 H9 115(5) . . ? C9 C10 C11 119.4(8) . . ? C9 C10 H10 124(6) . . ? C11 C10 H10 116(6) . . ? C10 C11 C12 121.0(9) . . ? C10 C11 H11 126(7) . . ? C12 C11 H11 113(7) . . ? C11 C12 C7 119.6(8) . . ? C11 C12 H12 127(7) . . ? C7 C12 H12 113(7) . . ? C18 C13 C14 119.1(7) . . ? C18 C13 P2 120.2(5) . . ? C14 C13 P2 120.7(6) . . ? C15 C14 C13 119.2(8) . . ? C15 C14 H14 123(6) . . ? C13 C14 H14 116(6) . . ? C16 C15 C14 121.1(8) . . ? C16 C15 H15 125(5) . . ? C14 C15 H15 114(5) . . ? C15 C16 C17 119.3(8) . . ? C15 C16 H16 117(5) . . ? C17 C16 H16 123(5) . . ? C18 C17 C16 119.8(9) . . ? C18 C17 H17 128(5) . . ? C16 C17 H17 112(5) . . ? C13 C18 C17 121.4(7) . . ? C13 C18 H18 116(5) . . ? C17 C18 H18 122(5) . . ? C24 C19 C20 117.6(7) . . ? C24 C19 P2 123.0(5) . . ? C20 C19 P2 119.4(5) . . ? C21 C20 C19 121.4(8) . . ? C21 C20 H20 133(4) . . ? C19 C20 H20 106(4) . . ? C20 C21 C22 119.8(8) . . ? C20 C21 H21 115(5) . . ? C22 C21 H21 125(5) . . ? C23 C22 C21 121.1(8) . . ? C23 C22 H22 117(5) . . ? C21 C22 H22 122(5) . . ? C22 C23 C24 118.5(8) . . ? C22 C23 H23 122(5) . . ? C24 C23 H23 119(5) . . ? C19 C24 C23 121.6(8) . . ? C19 C24 H24 124(5) . . ? C23 C24 H24 114(5) . . ? C26 C25 C30 119.0(7) . . ? C26 C25 P3 121.5(6) . . ? C30 C25 P3 119.5(6) . . ? C25 C26 C27 119.0(9) . . ? C25 C26 H26 119(6) . . ? C27 C26 H26 119(6) . . ? C28 C27 C26 121.4(10) . . ? C28 C27 H27 121(6) . . ? C26 C27 H27 117(6) . . ? C29 C28 C27 118.7(9) . . ? C29 C28 H28 126(5) . . ? C27 C28 H28 116(5) . . ? C28 C29 C30 122.0(10) . . ? C28 C29 H29 120(6) . . ? C30 C29 H29 118(6) . . ? C25 C30 C29 119.6(9) . . ? C25 C30 H30 113(5) . . ? C29 C30 H30 127(5) . . ? C36 C31 C32 117.5(7) . . ? C36 C31 P3 123.8(6) . . ? C32 C31 P3 118.4(6) . . ? C33 C32 C31 120.8(9) . . ? C33 C32 H32 123(4) . . ? C31 C32 H32 116(4) . . ? C32 C33 C34 121.5(10) . . ? C32 C33 H33 131(6) . . ? C34 C33 H33 108(5) . . ? C33 C34 C35 119.2(9) . . ? C33 C34 H34 125(5) . . ? C35 C34 H34 115(5) . . ? C34 C35 C36 119.8(10) . . ? C34 C35 H35 118(6) . . ? C36 C35 H35 122(6) . . ? C31 C36 C35 121.3(9) . . ? C31 C36 H36 117(5) . . ? C35 C36 H36 122(5) . . ? C38 C37 C42 118.0(8) . . ? C38 C37 P4 120.9(6) . . ? C42 C37 P4 121.0(6) . . ? C37 C38 C39 120.7(10) . . ? C37 C38 H38 107(6) . . ? C39 C38 H38 132(6) . . ? C40 C39 C38 120.4(10) . . ? C40 C39 H39 131(5) . . ? C38 C39 H39 109(5) . . ? C41 C40 C39 120.6(11) . . ? C41 C40 H40 108(7) . . ? C39 C40 H40 131(7) . . ? C40 C41 C42 119.0(10) . . ? C40 C41 H41 123(6) . . ? C42 C41 H41 118(6) . . ? C37 C42 C41 121.3(9) . . ? C37 C42 H42 118(5) . . ? C41 C42 H42 120(5) . . ? C48 C43 C44 118.5(8) . . ? C48 C43 P4 122.3(6) . . ? C44 C43 P4 119.2(6) . . ? C43 C44 C45 120.0(9) . . ? C43 C44 H44 122(5) . . ? C45 C44 H44 118(5) . . ? C46 C45 C44 120.7(10) . . ? C46 C45 H45 128(6) . . ? C44 C45 H45 111(6) . . ? C47 C46 C45 120.3(9) . . ? C47 C46 H46 124(5) . . ? C45 C46 H46 115(5) . . ? C46 C47 C48 119.5(9) . . ? C46 C47 H47 124(5) . . ? C48 C47 H47 116(5) . . ? C43 C48 C47 121.0(9) . . ? C43 C48 H48 123(6) . . ? C47 C48 H48 115(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.699 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.099 #===END data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 764426' #TrackingRef '- Ferentinos_Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H54 N4 Ni O4 P4 S2' _chemical_formula_weight 1069.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3092(2) _cell_length_b 10.3818(2) _cell_length_c 13.2729(2) _cell_angle_alpha 89.1750(10) _cell_angle_beta 85.6120(10) _cell_angle_gamma 84.5020(10) _cell_volume 1273.10(4) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parall _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24276 _diffrn_reflns_av_R_equivalents 0.0142 _diffrn_reflns_av_sigmaI/netI 0.0098 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4992 _reflns_number_gt 4753 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.6239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4992 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.0000 0.5000 0.01729(7) Uani 1 2 d S . . N N 0.55079(13) -0.11634(11) 0.76367(8) 0.0208(2) Uani 1 1 d . . . O O 0.54461(10) 0.07908(9) 0.63091(7) 0.0205(2) Uani 1 1 d . . . S S 0.36465(4) -0.17431(3) 0.58666(3) 0.02384(9) Uani 1 1 d . . . P1 P 0.46199(4) -0.21825(3) 0.71290(2) 0.01774(8) Uani 1 1 d . . . P2 P 0.57633(4) 0.02900(3) 0.73496(2) 0.01643(8) Uani 1 1 d . . . C1 C 0.58660(15) -0.36488(13) 0.69764(10) 0.0198(3) Uani 1 1 d . . . C2 C 0.69771(16) -0.38695(15) 0.76210(12) 0.0267(3) Uani 1 1 d . . . C3 C 0.78758(17) -0.50174(16) 0.75713(13) 0.0314(3) Uani 1 1 d . . . C4 C 0.76990(18) -0.59426(15) 0.68616(13) 0.0310(3) Uani 1 1 d . . . C5 C 0.66246(18) -0.57223(15) 0.62009(12) 0.0307(3) Uani 1 1 d . . . C6 C 0.57014(17) -0.45811(14) 0.62605(11) 0.0257(3) Uani 1 1 d . . . C7 C 0.32606(15) -0.26726(13) 0.80897(11) 0.0221(3) Uani 1 1 d . . . C8 C 0.18364(18) -0.27785(17) 0.78892(13) 0.0336(4) Uani 1 1 d . . . C9 C 0.08408(19) -0.3139(2) 0.86577(15) 0.0435(4) Uani 1 1 d . . . C10 C 0.1263(2) -0.34137(18) 0.96143(14) 0.0401(4) Uani 1 1 d . . . C11 C 0.2677(2) -0.33115(16) 0.98225(12) 0.0345(4) Uani 1 1 d . . . C12 C 0.36653(18) -0.29352(15) 0.90677(11) 0.0277(3) Uani 1 1 d . . . C21 C 0.76410(14) 0.04951(12) 0.75108(10) 0.0198(3) Uani 1 1 d . . . C22 C 0.86245(17) 0.03372(16) 0.66639(12) 0.0289(3) Uani 1 1 d . . . C23 C 1.00874(18) 0.04342(18) 0.67504(14) 0.0372(4) Uani 1 1 d . . . C24 C 1.05739(18) 0.07064(19) 0.76696(16) 0.0414(4) Uani 1 1 d . . . C25 C 0.96075(19) 0.08850(19) 0.85115(15) 0.0401(4) Uani 1 1 d . . . C26 C 0.81369(17) 0.07817(15) 0.84338(12) 0.0286(3) Uani 1 1 d . . . C27 C 0.46874(14) 0.13420(13) 0.82611(10) 0.0190(3) Uani 1 1 d . . . C28 C 0.39037(16) 0.08594(14) 0.90899(11) 0.0244(3) Uani 1 1 d . . . C29 C 0.30118(18) 0.16971(16) 0.97322(12) 0.0307(3) Uani 1 1 d . . . C30 C 0.29016(17) 0.30095(16) 0.95464(12) 0.0303(3) Uani 1 1 d . . . C31 C 0.3683(2) 0.35038(16) 0.87289(13) 0.0354(4) Uani 1 1 d . . . C32 C 0.45757(19) 0.26707(15) 0.80914(12) 0.0309(3) Uani 1 1 d . . . O41 O 0.30960(11) 0.12037(10) 0.50086(8) 0.0255(2) Uani 1 1 d . . . C42 C 0.29517(16) 0.21867(14) 0.55377(12) 0.0260(3) Uani 1 1 d . . . C41 C 0.1774(2) 0.42302(18) 0.61542(17) 0.0437(4) Uani 1 1 d . . . N41 N 0.18613(14) 0.30996(13) 0.55070(10) 0.0298(3) Uani 1 1 d . . . C43 C 0.0779(2) 0.3036(2) 0.47922(16) 0.0444(5) Uani 1 1 d . . . H2 H 0.712(2) -0.3265(18) 0.8081(14) 0.034(5) Uiso 1 1 d . . . H3 H 0.861(2) -0.516(2) 0.8011(16) 0.049(6) Uiso 1 1 d . . . H4 H 0.826(2) -0.6711(19) 0.6838(14) 0.037(5) Uiso 1 1 d . . . H5 H 0.650(2) -0.6310(19) 0.5704(15) 0.040(5) Uiso 1 1 d . . . H6 H 0.496(2) -0.4413(17) 0.5806(13) 0.029(4) Uiso 1 1 d . . . H8 H 0.1609(19) -0.2585(17) 0.7254(14) 0.027(4) Uiso 1 1 d . . . H9 H -0.008(3) -0.316(2) 0.8498(18) 0.059(7) Uiso 1 1 d . . . H10 H 0.057(2) -0.367(2) 1.0146(16) 0.047(6) Uiso 1 1 d . . . H11 H 0.299(2) -0.3524(19) 1.0482(16) 0.044(5) Uiso 1 1 d . . . H12 H 0.462(2) -0.2834(19) 0.9226(14) 0.039(5) Uiso 1 1 d . . . H22 H 0.828(2) 0.0205(18) 0.6037(15) 0.037(5) Uiso 1 1 d . . . H23 H 1.074(2) 0.0232(19) 0.6177(16) 0.044(5) Uiso 1 1 d . . . H24 H 1.156(3) 0.075(2) 0.7739(17) 0.055(6) Uiso 1 1 d . . . H25 H 0.990(2) 0.110(2) 0.9121(17) 0.052(6) Uiso 1 1 d . . . H26 H 0.745(2) 0.0917(18) 0.9023(14) 0.034(5) Uiso 1 1 d . . . H28 H 0.4004(19) -0.0042(18) 0.9217(13) 0.030(4) Uiso 1 1 d . . . H29 H 0.251(2) 0.1384(19) 1.0290(16) 0.043(5) Uiso 1 1 d . . . H30 H 0.230(2) 0.3574(18) 0.9973(14) 0.035(5) Uiso 1 1 d . . . H31 H 0.361(2) 0.436(2) 0.8603(16) 0.047(6) Uiso 1 1 d . . . H32 H 0.511(2) 0.2994(19) 0.7552(16) 0.043(5) Uiso 1 1 d . . . H42 H 0.367(2) 0.2342(18) 0.6013(14) 0.034(5) Uiso 1 1 d . . . H41A H 0.085(3) 0.431(2) 0.6546(17) 0.059(6) Uiso 1 1 d . . . H41B H 0.186(3) 0.500(2) 0.5728(18) 0.063(7) Uiso 1 1 d . . . H41C H 0.255(3) 0.408(2) 0.665(2) 0.072(8) Uiso 1 1 d . . . H43A H -0.013(3) 0.305(3) 0.513(2) 0.078(8) Uiso 1 1 d . . . H43B H 0.101(3) 0.231(3) 0.437(2) 0.072(8) Uiso 1 1 d . . . H43C H 0.072(3) 0.382(3) 0.435(2) 0.093(10) Uiso 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 0.01756(12) 0.01762(12) 0.01602(12) -0.00073(9) -0.00193(9) 0.00242(9) N 0.0260(6) 0.0182(6) 0.0195(6) 0.0009(4) -0.0060(5) -0.0048(5) O 0.0242(5) 0.0194(5) 0.0176(5) -0.0001(4) -0.0024(4) -0.0002(4) S 0.02625(18) 0.02525(18) 0.02117(17) 0.00152(13) -0.00640(13) -0.00492(14) P1 0.01912(17) 0.01686(16) 0.01755(16) -0.00134(12) -0.00249(13) -0.00223(13) P2 0.01744(16) 0.01594(16) 0.01596(16) -0.00077(12) -0.00144(12) -0.00165(12) C1 0.0212(6) 0.0188(6) 0.0191(6) 0.0001(5) 0.0020(5) -0.0025(5) C2 0.0274(7) 0.0260(7) 0.0265(7) -0.0049(6) -0.0035(6) 0.0000(6) C3 0.0266(8) 0.0322(8) 0.0343(8) 0.0028(7) -0.0032(6) 0.0031(6) C4 0.0304(8) 0.0202(7) 0.0394(9) 0.0023(6) 0.0098(7) 0.0026(6) C5 0.0387(9) 0.0211(7) 0.0317(8) -0.0067(6) 0.0055(7) -0.0052(6) C6 0.0296(8) 0.0226(7) 0.0253(7) -0.0031(6) -0.0007(6) -0.0045(6) C7 0.0217(7) 0.0174(6) 0.0270(7) -0.0039(5) 0.0019(5) -0.0035(5) C8 0.0276(8) 0.0426(9) 0.0313(9) 0.0004(7) -0.0029(7) -0.0075(7) C9 0.0243(8) 0.0586(12) 0.0487(11) -0.0003(9) 0.0031(8) -0.0140(8) C10 0.0391(9) 0.0438(10) 0.0367(9) -0.0019(7) 0.0138(8) -0.0133(8) C11 0.0445(10) 0.0341(9) 0.0251(8) -0.0014(6) 0.0050(7) -0.0102(7) C12 0.0302(8) 0.0284(8) 0.0250(7) -0.0015(6) 0.0003(6) -0.0074(6) C21 0.0188(6) 0.0156(6) 0.0254(7) 0.0005(5) -0.0029(5) -0.0022(5) C22 0.0243(7) 0.0329(8) 0.0296(8) -0.0043(6) 0.0005(6) -0.0039(6) C23 0.0223(8) 0.0426(10) 0.0457(10) -0.0041(8) 0.0057(7) -0.0037(7) C24 0.0201(8) 0.0472(10) 0.0580(11) -0.0024(9) -0.0079(7) -0.0053(7) C25 0.0305(9) 0.0511(11) 0.0413(10) -0.0051(8) -0.0143(7) -0.0085(8) C26 0.0265(8) 0.0324(8) 0.0278(8) -0.0013(6) -0.0048(6) -0.0048(6) C27 0.0177(6) 0.0214(7) 0.0183(6) -0.0027(5) -0.0026(5) -0.0018(5) C28 0.0284(7) 0.0233(7) 0.0215(7) 0.0011(5) -0.0007(6) -0.0031(6) C29 0.0322(8) 0.0371(9) 0.0216(7) -0.0005(6) 0.0059(6) -0.0036(7) C30 0.0294(8) 0.0347(8) 0.0251(7) -0.0086(6) 0.0005(6) 0.0062(6) C31 0.0474(10) 0.0206(8) 0.0360(9) -0.0029(6) 0.0053(7) 0.0028(7) C32 0.0390(9) 0.0226(7) 0.0292(8) -0.0003(6) 0.0101(7) -0.0038(6) O41 0.0220(5) 0.0250(5) 0.0283(5) -0.0010(4) -0.0030(4) 0.0046(4) C42 0.0214(7) 0.0248(7) 0.0304(8) 0.0014(6) 0.0002(6) 0.0032(6) C41 0.0394(10) 0.0315(9) 0.0564(12) -0.0071(8) 0.0030(9) 0.0121(8) N41 0.0254(6) 0.0274(7) 0.0337(7) 0.0021(5) 0.0013(5) 0.0084(5) C43 0.0332(9) 0.0524(12) 0.0436(10) 0.0023(9) -0.0075(8) 0.0193(9) _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 O 2.0205(9) . ? Ni O 2.0205(9) 2_656 ? Ni O41 2.0679(10) 2_656 ? Ni O41 2.0679(10) . ? Ni S 2.5181(4) . ? Ni S 2.5181(4) 2_656 ? N P2 1.5864(11) . ? N P1 1.5907(11) . ? O P2 1.5090(10) . ? S P1 1.9919(5) . ? P1 C1 1.8272(14) . ? P1 C7 1.8287(14) . ? P2 C21 1.8101(14) . ? P2 C27 1.8174(13) . ? C1 C2 1.392(2) . ? C1 C6 1.393(2) . ? C2 C3 1.388(2) . ? C2 H2 0.906(19) . ? C3 C4 1.385(2) . ? C3 H3 0.93(2) . ? C4 C5 1.381(2) . ? C4 H4 0.91(2) . ? C5 C6 1.395(2) . ? C5 H5 0.93(2) . ? C6 H6 0.951(18) . ? C7 C8 1.387(2) . ? C7 C12 1.395(2) . ? C8 C9 1.397(2) . ? C8 H8 0.900(18) . ? C9 C10 1.376(3) . ? C9 H9 0.90(2) . ? C10 C11 1.380(3) . ? C10 H10 0.97(2) . ? C11 C12 1.385(2) . ? C11 H11 0.96(2) . ? C12 H12 0.94(2) . ? C21 C26 1.388(2) . ? C21 C22 1.396(2) . ? C22 C23 1.389(2) . ? C22 H22 0.93(2) . ? C23 C24 1.376(3) . ? C23 H23 0.95(2) . ? C24 C25 1.383(3) . ? C24 H24 0.93(2) . ? C25 C26 1.395(2) . ? C25 H25 0.91(2) . ? C26 H26 0.976(19) . ? C27 C28 1.387(2) . ? C27 C32 1.390(2) . ? C28 C29 1.395(2) . ? C28 H28 0.946(18) . ? C29 C30 1.377(2) . ? C29 H29 0.92(2) . ? C30 C31 1.380(2) . ? C30 H30 0.936(19) . ? C31 C32 1.389(2) . ? C31 H31 0.90(2) . ? C32 H32 0.92(2) . ? O41 C42 1.2380(18) . ? C42 N41 1.3233(19) . ? C42 H42 0.979(19) . ? C41 N41 1.457(2) . ? C41 H41A 0.97(2) . ? C41 H41B 0.98(3) . ? C41 H41C 1.02(3) . ? N41 C43 1.442(2) . ? C43 H43A 0.93(3) . ? C43 H43B 0.94(3) . ? C43 H43C 1.00(3) . ? 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 O Ni O 180.0 . 2_656 ? O Ni O41 90.22(4) . 2_656 ? O Ni O41 89.78(4) 2_656 2_656 ? O Ni O41 89.78(4) . . ? O Ni O41 90.22(4) 2_656 . ? O41 Ni O41 180.0 2_656 . ? O Ni S 93.88(3) . . ? O Ni S 86.12(3) 2_656 . ? O41 Ni S 90.05(3) 2_656 . ? O41 Ni S 89.95(3) . . ? O Ni S 86.12(3) . 2_656 ? O Ni S 93.88(3) 2_656 2_656 ? O41 Ni S 89.95(3) 2_656 2_656 ? O41 Ni S 90.05(3) . 2_656 ? S Ni S 180.000(11) . 2_656 ? P2 N P1 131.64(8) . . ? P2 O Ni 135.76(6) . . ? P1 S Ni 105.922(17) . . ? N P1 C1 105.20(6) . . ? N P1 C7 107.27(6) . . ? C1 P1 C7 102.39(6) . . ? N P1 S 120.86(5) . . ? C1 P1 S 111.31(5) . . ? C7 P1 S 108.22(5) . . ? O P2 N 118.99(6) . . ? O P2 C21 107.29(6) . . ? N P2 C21 107.62(6) . . ? O P2 C27 107.44(6) . . ? N P2 C27 108.20(6) . . ? C21 P2 C27 106.68(6) . . ? C2 C1 C6 118.87(13) . . ? C2 C1 P1 119.19(11) . . ? C6 C1 P1 121.89(11) . . ? C3 C2 C1 120.48(14) . . ? C3 C2 H2 119.4(12) . . ? C1 C2 H2 120.2(12) . . ? C4 C3 C2 120.26(15) . . ? C4 C3 H3 119.8(13) . . ? C2 C3 H3 119.9(13) . . ? C5 C4 C3 119.85(15) . . ? C5 C4 H4 119.1(12) . . ? C3 C4 H4 121.1(12) . . ? C4 C5 C6 120.10(15) . . ? C4 C5 H5 121.7(12) . . ? C6 C5 H5 118.2(12) . . ? C1 C6 C5 120.41(15) . . ? C1 C6 H6 118.6(11) . . ? C5 C6 H6 121.0(11) . . ? C8 C7 C12 118.56(14) . . ? C8 C7 P1 122.66(12) . . ? C12 C7 P1 118.78(11) . . ? C7 C8 C9 120.08(16) . . ? C7 C8 H8 116.1(11) . . ? C9 C8 H8 123.8(11) . . ? C10 C9 C8 120.61(17) . . ? C10 C9 H9 122.6(15) . . ? C8 C9 H9 116.8(15) . . ? C9 C10 C11 119.79(16) . . ? C9 C10 H10 120.3(12) . . ? C11 C10 H10 119.9(12) . . ? C10 C11 C12 119.90(16) . . ? C10 C11 H11 120.7(12) . . ? C12 C11 H11 119.3(12) . . ? C11 C12 C7 121.03(15) . . ? C11 C12 H12 119.1(12) . . ? C7 C12 H12 119.8(12) . . ? C26 C21 C22 119.23(13) . . ? C26 C21 P2 122.99(11) . . ? C22 C21 P2 117.77(11) . . ? C23 C22 C21 120.30(15) . . ? C23 C22 H22 120.4(12) . . ? C21 C22 H22 119.2(12) . . ? C24 C23 C22 120.16(16) . . ? C24 C23 H23 121.2(13) . . ? C22 C23 H23 118.4(13) . . ? C23 C24 C25 120.11(16) . . ? C23 C24 H24 120.8(14) . . ? C25 C24 H24 119.1(14) . . ? C24 C25 C26 120.17(16) . . ? C24 C25 H25 121.6(14) . . ? C26 C25 H25 118.2(14) . . ? C21 C26 C25 120.00(15) . . ? C21 C26 H26 119.3(11) . . ? C25 C26 H26 120.7(11) . . ? C28 C27 C32 118.74(13) . . ? C28 C27 P2 122.18(11) . . ? C32 C27 P2 118.97(11) . . ? C27 C28 C29 120.31(14) . . ? C27 C28 H28 118.7(11) . . ? C29 C28 H28 121.0(11) . . ? C30 C29 C28 120.18(14) . . ? C30 C29 H29 119.2(13) . . ? C28 C29 H29 120.6(13) . . ? C29 C30 C31 120.13(14) . . ? C29 C30 H30 120.4(12) . . ? C31 C30 H30 119.5(12) . . ? C30 C31 C32 119.72(15) . . ? C30 C31 H31 120.4(14) . . ? C32 C31 H31 119.8(14) . . ? C27 C32 C31 120.92(14) . . ? C27 C32 H32 118.9(13) . . ? C31 C32 H32 120.2(13) . . ? C42 O41 Ni 119.21(10) . . ? O41 C42 N41 124.10(15) . . ? O41 C42 H42 120.9(11) . . ? N41 C42 H42 115.0(11) . . ? N41 C41 H41A 109.2(14) . . ? N41 C41 H41B 108.7(14) . . ? H41A C41 H41B 109.7(19) . . ? N41 C41 H41C 108.1(14) . . ? H41A C41 H41C 107(2) . . ? H41B C41 H41C 114(2) . . ? C42 N41 C43 120.81(14) . . ? C42 N41 C41 120.67(15) . . ? C43 N41 C41 118.43(15) . . ? N41 C43 H43A 110.4(17) . . ? N41 C43 H43B 110.1(16) . . ? H43A C43 H43B 113(2) . . ? N41 C43 H43C 111.5(17) . . ? H43A C43 H43C 104(2) . . ? H43B C43 H43C 107(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.399 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.045 #===END data_Complex4 _database_code_depnum_ccdc_archive 'CCDC 764427' #TrackingRef '- Ferentinos_Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H54 N4 Ni O4 P4 Se2' _chemical_formula_weight 1163.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.326(4) _cell_length_b 10.505(5) _cell_length_c 13.500(6) _cell_angle_alpha 88.890(10) _cell_angle_beta 86.330(10) _cell_angle_gamma 85.300(10) _cell_volume 1315.3(10) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 11.0 _exptl_crystal_description parall _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 1.923 _exptl_absorpt_correction_type 'psi scan empirical' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Crystal Logic Dual Goniometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.1 _diffrn_reflns_number 4765 _diffrn_reflns_av_R_equivalents 0.0083 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4453 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.5464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4453 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.0000 0.5000 0.03177(15) Uani 1 2 d S . . Se Se 0.34556(3) -0.17626(3) 0.58383(2) 0.04246(13) Uani 1 1 d . . . P1 P 0.43193(8) -0.02878(7) 0.26587(5) 0.03010(18) Uani 1 1 d . . . P2 P 0.45648(8) -0.21980(7) 0.71665(5) 0.03237(18) Uani 1 1 d . . . O1 O 0.4643(2) -0.07721(19) 0.36848(14) 0.0365(5) Uani 1 1 d . . . N1 N 0.5457(3) -0.1157(2) 0.76324(18) 0.0376(6) Uani 1 1 d . . . C1 C 0.5397(3) -0.1304(3) 0.1774(2) 0.0342(6) Uani 1 1 d . . . C2 C 0.5566(5) -0.2604(3) 0.1964(3) 0.0554(9) Uani 1 1 d . . . C3 C 0.6428(5) -0.3415(4) 0.1326(3) 0.0640(11) Uani 1 1 d . . . C4 C 0.7123(4) -0.2930(4) 0.0506(3) 0.0561(9) Uani 1 1 d . . . C5 C 0.6970(4) -0.1643(4) 0.0301(3) 0.0561(9) Uani 1 1 d . . . C6 C 0.6111(4) -0.0829(3) 0.0934(2) 0.0437(7) Uani 1 1 d . . . C7 C 0.2455(3) -0.0529(3) 0.2474(2) 0.0360(6) Uani 1 1 d . . . C8 C 0.1971(4) -0.0825(4) 0.1563(3) 0.0515(8) Uani 1 1 d . . . C9 C 0.0519(5) -0.0942(5) 0.1466(4) 0.0729(12) Uani 1 1 d . . . C10 C -0.0456(5) -0.0778(5) 0.2272(4) 0.0706(12) Uani 1 1 d . . . C11 C 0.0010(5) -0.0507(4) 0.3176(4) 0.0681(11) Uani 1 1 d . . . C12 C 0.1455(4) -0.0393(4) 0.3284(3) 0.0508(8) Uani 1 1 d . . . C13 C 0.5816(3) -0.3620(3) 0.7006(2) 0.0359(6) Uani 1 1 d . . . C14 C 0.6974(4) -0.3807(4) 0.7594(3) 0.0523(9) Uani 1 1 d . . . C15 C 0.7872(5) -0.4927(4) 0.7545(3) 0.0638(10) Uani 1 1 d . . . C16 C 0.7647(5) -0.5854(4) 0.6882(3) 0.0603(11) Uani 1 1 d . . . C17 C 0.6525(5) -0.5671(3) 0.6271(3) 0.0584(10) Uani 1 1 d . . . C18 C 0.5602(4) -0.4571(3) 0.6331(3) 0.0474(8) Uani 1 1 d . . . C19 C 0.3270(3) -0.2717(3) 0.8135(2) 0.0388(7) Uani 1 1 d . . . C20 C 0.3740(4) -0.3027(4) 0.9073(2) 0.0500(8) Uani 1 1 d . . . C21 C 0.2799(5) -0.3414(4) 0.9830(3) 0.0630(11) Uani 1 1 d . . . C22 C 0.1366(5) -0.3459(5) 0.9677(3) 0.0709(12) Uani 1 1 d . . . C23 C 0.0885(6) -0.3150(6) 0.8773(4) 0.0836(15) Uani 1 1 d . . . C24 C 0.1831(4) -0.2787(5) 0.7990(3) 0.0632(10) Uani 1 1 d . . . O2 O 0.3124(2) 0.1193(2) 0.49242(16) 0.0441(5) Uani 1 1 d . . . N2 N 0.1812(3) 0.3005(3) 0.5398(2) 0.0547(8) Uani 1 1 d . . . C25 C 0.2940(4) 0.2165(3) 0.5424(3) 0.0459(8) Uani 1 1 d . . . C26 C 0.0695(5) 0.2828(5) 0.4731(4) 0.0860(15) Uani 1 1 d . . . H26A H -0.0188 0.2693 0.5109 0.143(15) Uiso 1 1 calc R . . H26B H 0.0976 0.2100 0.4324 0.143(15) Uiso 1 1 calc R . . H26C H 0.0556 0.3576 0.4316 0.143(15) Uiso 1 1 calc R . . C27 C 0.1686(5) 0.4141(4) 0.6012(4) 0.0833(15) Uani 1 1 d . . . H27A H 0.0780 0.4188 0.6394 0.112(11) Uiso 1 1 calc R . . H27B H 0.1737 0.4888 0.5594 0.112(11) Uiso 1 1 calc R . . H27C H 0.2459 0.4095 0.6451 0.112(11) Uiso 1 1 calc R . . H2 H 0.502(5) -0.293(4) 0.250(3) 0.073(13) Uiso 1 1 d . . . H3 H 0.650(5) -0.422(4) 0.147(3) 0.074(13) Uiso 1 1 d . . . H4 H 0.776(5) -0.350(4) 0.015(3) 0.062(11) Uiso 1 1 d . . . H5 H 0.747(5) -0.130(4) -0.022(4) 0.072(13) Uiso 1 1 d . . . H6 H 0.596(4) 0.000(4) 0.077(3) 0.046(9) Uiso 1 1 d . . . H8 H 0.277(5) -0.097(4) 0.101(3) 0.059(11) Uiso 1 1 d . . . H9 H 0.023(6) -0.110(5) 0.089(4) 0.084(15) Uiso 1 1 d . . . H10 H -0.147(6) -0.080(5) 0.222(4) 0.092(16) Uiso 1 1 d . . . H11 H -0.062(6) -0.033(4) 0.377(4) 0.079(14) Uiso 1 1 d . . . H12 H 0.179(5) -0.020(4) 0.389(3) 0.075(13) Uiso 1 1 d . . . H14 H 0.714(4) -0.328(4) 0.797(3) 0.052(11) Uiso 1 1 d . . . H15 H 0.862(5) -0.504(4) 0.792(3) 0.068(13) Uiso 1 1 d . . . H16 H 0.828(5) -0.654(4) 0.683(3) 0.065(12) Uiso 1 1 d . . . H17 H 0.633(5) -0.632(4) 0.581(3) 0.069(12) Uiso 1 1 d . . . H18 H 0.477(4) -0.442(3) 0.593(3) 0.051(10) Uiso 1 1 d . . . H20 H 0.475(5) -0.299(4) 0.917(3) 0.072(13) Uiso 1 1 d . . . H21 H 0.311(5) -0.375(4) 1.041(4) 0.074(13) Uiso 1 1 d . . . H22 H 0.074(6) -0.377(5) 1.022(4) 0.090(15) Uiso 1 1 d . . . H23 H 0.000(6) -0.305(4) 0.864(3) 0.071(14) Uiso 1 1 d . . . H24 H 0.145(6) -0.259(5) 0.737(4) 0.093(16) Uiso 1 1 d . . . H25 H 0.359(5) 0.234(4) 0.588(4) 0.077(14) Uiso 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 0.0315(3) 0.0330(3) 0.0299(3) -0.00287(19) -0.00423(19) 0.0056(2) Se 0.0436(2) 0.0465(2) 0.03916(19) -0.00031(13) -0.01050(13) -0.00868(14) P1 0.0317(4) 0.0289(4) 0.0300(3) -0.0027(3) -0.0029(3) -0.0031(3) P2 0.0350(4) 0.0302(4) 0.0324(4) -0.0028(3) -0.0027(3) -0.0045(3) O1 0.0410(12) 0.0363(11) 0.0319(10) -0.0030(8) -0.0032(8) -0.0009(9) N1 0.0443(15) 0.0340(13) 0.0361(12) 0.0003(10) -0.0103(11) -0.0068(11) C1 0.0342(16) 0.0358(15) 0.0334(14) -0.0038(11) -0.0029(11) -0.0056(12) C2 0.072(3) 0.0411(18) 0.0504(19) -0.0015(15) 0.0177(18) -0.0054(17) C3 0.089(3) 0.038(2) 0.062(2) -0.0082(17) 0.012(2) 0.0058(19) C4 0.050(2) 0.066(2) 0.0494(19) -0.0151(17) 0.0046(16) 0.0092(18) C5 0.059(2) 0.067(2) 0.0405(18) -0.0024(16) 0.0114(16) -0.0053(18) C6 0.049(2) 0.0437(18) 0.0382(16) 0.0014(13) -0.0011(13) -0.0031(15) C7 0.0351(17) 0.0294(14) 0.0434(16) -0.0008(12) -0.0027(12) -0.0006(12) C8 0.045(2) 0.060(2) 0.0513(19) -0.0053(16) -0.0117(16) -0.0082(16) C9 0.055(3) 0.094(3) 0.074(3) -0.012(2) -0.025(2) -0.012(2) C10 0.037(2) 0.080(3) 0.097(3) -0.006(2) -0.016(2) -0.0074(19) C11 0.043(2) 0.077(3) 0.083(3) -0.010(2) 0.010(2) -0.008(2) C12 0.036(2) 0.062(2) 0.055(2) -0.0115(16) 0.0002(15) -0.0058(16) C13 0.0378(17) 0.0318(14) 0.0376(14) -0.0010(11) 0.0036(12) -0.0051(12) C14 0.052(2) 0.049(2) 0.056(2) -0.0138(17) -0.0095(16) 0.0039(16) C15 0.054(2) 0.059(2) 0.076(3) 0.000(2) -0.009(2) 0.0101(19) C16 0.062(3) 0.0366(18) 0.078(3) 0.0023(17) 0.020(2) 0.0070(17) C17 0.073(3) 0.0371(18) 0.063(2) -0.0121(16) 0.016(2) -0.0067(17) C18 0.057(2) 0.0376(17) 0.0484(18) -0.0075(14) 0.0010(16) -0.0090(15) C19 0.0395(18) 0.0344(15) 0.0427(16) -0.0069(12) 0.0025(13) -0.0075(13) C20 0.050(2) 0.060(2) 0.0416(17) -0.0015(15) -0.0002(15) -0.0147(17) C21 0.080(3) 0.066(2) 0.045(2) 0.0006(18) 0.0064(19) -0.018(2) C22 0.070(3) 0.083(3) 0.059(2) -0.003(2) 0.023(2) -0.025(2) C23 0.044(3) 0.126(5) 0.082(3) 0.005(3) 0.011(2) -0.026(3) C24 0.050(2) 0.086(3) 0.055(2) 0.003(2) -0.0002(17) -0.014(2) O2 0.0362(12) 0.0438(12) 0.0505(12) -0.0026(10) -0.0067(9) 0.0100(10) N2 0.0432(17) 0.0476(16) 0.0692(19) 0.0033(14) 0.0041(14) 0.0154(13) C25 0.0353(18) 0.0413(18) 0.059(2) 0.0013(15) -0.0001(15) 0.0068(14) C26 0.062(3) 0.101(4) 0.089(3) 0.004(3) -0.016(2) 0.036(3) C27 0.068(3) 0.053(2) 0.122(4) -0.015(3) 0.012(3) 0.022(2) _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 O1 2.024(2) . ? Ni O1 2.024(2) 2_656 ? Ni O2 2.074(2) 2_656 ? Ni O2 2.074(2) . ? Ni Se 2.6326(9) . ? Ni Se 2.6326(9) 2_656 ? Se P2 2.1501(11) . ? P1 O1 1.507(2) . ? P1 N1 1.588(3) 2_656 ? P1 C7 1.811(3) . ? P1 C1 1.816(3) . ? P2 N1 1.589(3) . ? P2 C13 1.826(3) . ? P2 C19 1.828(3) . ? N1 P1 1.588(3) 2_656 ? C1 C6 1.383(4) . ? C1 C2 1.383(5) . ? C2 C3 1.393(5) . ? C2 H2 0.93(5) . ? C3 C4 1.359(6) . ? C3 H3 0.87(5) . ? C4 C5 1.372(6) . ? C4 H4 0.93(4) . ? C5 C6 1.390(5) . ? C5 H5 0.91(5) . ? C6 H6 0.90(4) . ? C7 C8 1.387(5) . ? C7 C12 1.392(5) . ? C8 C9 1.385(6) . ? C8 H8 1.03(4) . ? C9 C10 1.376(7) . ? C9 H9 0.86(5) . ? C10 C11 1.364(7) . ? C10 H10 0.96(6) . ? C11 C12 1.380(6) . ? C11 H11 0.97(5) . ? C12 H12 0.93(5) . ? C13 C14 1.380(5) . ? C13 C18 1.399(4) . ? C14 C15 1.387(5) . ? C14 H14 0.79(4) . ? C15 C16 1.373(6) . ? C15 H15 0.88(5) . ? C16 C17 1.373(6) . ? C16 H16 0.90(4) . ? C17 C18 1.384(5) . ? C17 H17 0.97(4) . ? C18 H18 0.98(4) . ? C19 C24 1.376(5) . ? C19 C20 1.391(5) . ? C20 C21 1.382(5) . ? C20 H20 0.96(5) . ? C21 C22 1.370(7) . ? C21 H21 0.91(5) . ? C22 C23 1.352(7) . ? C22 H22 0.97(5) . ? C23 C24 1.400(6) . ? C23 H23 0.85(5) . ? C24 H24 0.95(5) . ? O2 C25 1.229(4) . ? N2 C25 1.319(4) . ? N2 C26 1.445(6) . ? N2 C27 1.459(5) . ? C25 H25 0.93(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? 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 O1 Ni O1 180.000(1) . 2_656 ? O1 Ni O2 89.85(9) . 2_656 ? O1 Ni O2 90.15(9) 2_656 2_656 ? O1 Ni O2 90.15(9) . . ? O1 Ni O2 89.85(9) 2_656 . ? O2 Ni O2 180.0 2_656 . ? O1 Ni Se 86.73(6) . . ? O1 Ni Se 93.27(6) 2_656 . ? O2 Ni Se 91.22(7) 2_656 . ? O2 Ni Se 88.78(7) . . ? O1 Ni Se 93.27(6) . 2_656 ? O1 Ni Se 86.73(6) 2_656 2_656 ? O2 Ni Se 88.78(7) 2_656 2_656 ? O2 Ni Se 91.22(7) . 2_656 ? Se Ni Se 180.0 . 2_656 ? P2 Se Ni 101.40(3) . . ? O1 P1 N1 119.26(12) . 2_656 ? O1 P1 C7 107.89(13) . . ? N1 P1 C7 106.89(13) 2_656 . ? O1 P1 C1 107.61(13) . . ? N1 P1 C1 108.24(14) 2_656 . ? C7 P1 C1 106.26(13) . . ? N1 P2 C13 105.67(14) . . ? N1 P2 C19 107.67(14) . . ? C13 P2 C19 102.15(14) . . ? N1 P2 Se 120.21(10) . . ? C13 P2 Se 110.92(10) . . ? C19 P2 Se 108.70(11) . . ? P1 O1 Ni 136.76(13) . . ? P1 N1 P2 132.55(16) 2_656 . ? C6 C1 C2 118.2(3) . . ? C6 C1 P1 122.8(2) . . ? C2 C1 P1 118.9(2) . . ? C1 C2 C3 120.9(3) . . ? C1 C2 H2 118(3) . . ? C3 C2 H2 121(3) . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 122(3) . . ? C2 C3 H3 118(3) . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 116(3) . . ? C5 C4 H4 123(3) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 121(3) . . ? C6 C5 H5 119(3) . . ? C1 C6 C5 120.6(3) . . ? C1 C6 H6 120(2) . . ? C5 C6 H6 120(2) . . ? C8 C7 C12 118.4(3) . . ? C8 C7 P1 123.2(3) . . ? C12 C7 P1 118.4(2) . . ? C9 C8 C7 120.1(4) . . ? C9 C8 H8 125(2) . . ? C7 C8 H8 115(2) . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 120(4) . . ? C8 C9 H9 119(4) . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10 118(3) . . ? C9 C10 H10 122(3) . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 125(3) . . ? C12 C11 H11 115(3) . . ? C11 C12 C7 120.9(4) . . ? C11 C12 H12 121(3) . . ? C7 C12 H12 118(3) . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P2 119.8(2) . . ? C18 C13 P2 121.9(3) . . ? C13 C14 C15 120.9(4) . . ? C13 C14 H14 120(3) . . ? C15 C14 H14 119(3) . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119(3) . . ? C14 C15 H15 121(3) . . ? C15 C16 C17 119.7(4) . . ? C15 C16 H16 119(3) . . ? C17 C16 H16 121(3) . . ? C16 C17 C18 120.5(4) . . ? C16 C17 H17 121(3) . . ? C18 C17 H17 118(3) . . ? C17 C18 C13 120.3(4) . . ? C17 C18 H18 123(2) . . ? C13 C18 H18 117(2) . . ? C24 C19 C20 117.8(3) . . ? C24 C19 P2 123.2(3) . . ? C20 C19 P2 119.0(3) . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20 121(3) . . ? C19 C20 H20 117(3) . . ? C22 C21 C20 120.3(4) . . ? C22 C21 H21 117(3) . . ? C20 C21 H21 122(3) . . ? C23 C22 C21 119.5(4) . . ? C23 C22 H22 122(3) . . ? C21 C22 H22 118(3) . . ? C22 C23 C24 120.9(5) . . ? C22 C23 H23 125(3) . . ? C24 C23 H23 114(3) . . ? C19 C24 C23 120.4(4) . . ? C19 C24 H24 122(3) . . ? C23 C24 H24 118(3) . . ? C25 O2 Ni 120.3(2) . . ? C25 N2 C26 120.0(3) . . ? C25 N2 C27 121.1(4) . . ? C26 N2 C27 118.9(3) . . ? O2 C25 N2 124.7(4) . . ? O2 C25 H25 121(3) . . ? N2 C25 H25 114(3) . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.633 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.083 #===END