# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Weerakanya Maneeprakorn' _publ_contact_author_email WEERAKANYA.MANEEPRAKORN@POSTGRAD.MANCHESTER.AC.UK _publ_section_title ; Synthesis of the Nickel Selenophosphinates [Ni(R2PSe2)2] (R = iPr, tBu and Ph) and their use as Single Source Precursors for the Deposition of Nickel Phosphide or Nickel Selenide Nanoparticles ; loop_ _publ_author_name "Paul O'Brien" 'Mohammad Azad Malik' 'Weerakanya Maneeprakorn' 'Chinh Q. Nguyen' 'James Raftery' # Attachment '[Ni_tBu2PSe2_2]s2392na.cif' data_s2392na _database_code_depnum_ccdc_archive 'CCDC 692535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 Ni P2 Se4' _chemical_formula_weight 664.94 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' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.8391(8) _cell_length_b 16.2638(7) _cell_length_c 33.5402(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.1650(10) _cell_angle_gamma 90.00 _cell_volume 9705.4(7) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8039 _cell_measurement_theta_min 2.4275 _cell_measurement_theta_max 27.002 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5216 _exptl_absorpt_coefficient_mu 6.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1505 _exptl_absorpt_correction_T_max 0.4229 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83345 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 28.33 _reflns_number_total 23010 _reflns_number_gt 15871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0373P)^2^+27.3838P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23010 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 C1 C -0.0295(4) 0.9659(4) 0.59444(18) 0.0291(15) Uani 1 1 d . . . C2 C -0.0458(4) 0.8846(4) 0.6145(2) 0.0395(18) Uani 1 1 d . . . H2A H -0.0522 0.8941 0.6429 0.059 Uiso 1 1 calc R . . H2B H -0.0037 0.8468 0.6118 0.059 Uiso 1 1 calc R . . H2C H -0.0919 0.8607 0.6018 0.059 Uiso 1 1 calc R . . C3 C -0.0971(4) 1.0231(5) 0.5989(3) 0.052(2) Uani 1 1 d . . . H3A H -0.1410 1.0018 0.5828 0.079 Uiso 1 1 calc R . . H3B H -0.0851 1.0784 0.5896 0.079 Uiso 1 1 calc R . . H3C H -0.1083 1.0255 0.6270 0.079 Uiso 1 1 calc R . . C4 C -0.0181(5) 0.9524(7) 0.5505(2) 0.075(3) Uani 1 1 d . . . H4A H 0.0231 0.9134 0.5479 0.113 Uiso 1 1 calc R . . H4B H -0.0058 1.0048 0.5382 0.113 Uiso 1 1 calc R . . H4C H -0.0643 0.9302 0.5370 0.113 Uiso 1 1 calc R . . C5 C 0.0953(4) 1.1014(4) 0.59540(18) 0.0273(14) Uani 1 1 d . . . C6 C 0.1552(5) 1.1421(6) 0.6245(3) 0.067(3) Uani 1 1 d . . . H6A H 0.1952 1.1025 0.6318 0.101 Uiso 1 1 calc R . . H6B H 0.1319 1.1599 0.6487 0.101 Uiso 1 1 calc R . . H6C H 0.1765 1.1899 0.6116 0.101 Uiso 1 1 calc R . . C7 C 0.1327(6) 1.0765(5) 0.5581(2) 0.071(3) Uani 1 1 d . . . H7A H 0.1605 1.1234 0.5482 0.106 Uiso 1 1 calc R . . H7B H 0.0942 1.0591 0.5374 0.106 Uiso 1 1 calc R . . H7C H 0.1674 1.0309 0.5644 0.106 Uiso 1 1 calc R . . C8 C 0.0344(4) 1.1663(4) 0.5854(3) 0.054(2) Uani 1 1 d . . . H8A H 0.0571 1.2145 0.5735 0.082 Uiso 1 1 calc R . . H8B H 0.0116 1.1826 0.6099 0.082 Uiso 1 1 calc R . . H8C H -0.0043 1.1433 0.5664 0.082 Uiso 1 1 calc R . . C9 C 0.2775(3) 0.8683(3) 0.80140(16) 0.0183(12) Uani 1 1 d . . . C10 C 0.2684(4) 0.9212(4) 0.83878(18) 0.0287(14) Uani 1 1 d . . . H10A H 0.2428 0.8891 0.8585 0.043 Uiso 1 1 calc R . . H10B H 0.2386 0.9702 0.8313 0.043 Uiso 1 1 calc R . . H10C H 0.3180 0.9380 0.8504 0.043 Uiso 1 1 calc R . . C11 C 0.3242(4) 0.7914(4) 0.8118(2) 0.0302(15) Uani 1 1 d . . . H11A H 0.3256 0.7565 0.7881 0.045 Uiso 1 1 calc R . . H11B H 0.3014 0.7608 0.8330 0.045 Uiso 1 1 calc R . . H11C H 0.3755 0.8075 0.8211 0.045 Uiso 1 1 calc R . . C12 C 0.3200(3) 0.9199(4) 0.7720(2) 0.0317(15) Uani 1 1 d . . . H12A H 0.3675 0.9391 0.7852 0.048 Uiso 1 1 calc R . . H12B H 0.2892 0.9672 0.7631 0.048 Uiso 1 1 calc R . . H12C H 0.3303 0.8861 0.7488 0.048 Uiso 1 1 calc R . . C13 C 0.1315(3) 0.7631(4) 0.80208(19) 0.0255(14) Uani 1 1 d . . . C14 C 0.1656(4) 0.6778(4) 0.7959(2) 0.0375(17) Uani 1 1 d . . . H14A H 0.2143 0.6737 0.8113 0.056 Uiso 1 1 calc R . . H14B H 0.1727 0.6697 0.7674 0.056 Uiso 1 1 calc R . . H14C H 0.1316 0.6354 0.8049 0.056 Uiso 1 1 calc R . . C15 C 0.1308(4) 0.7829(4) 0.84689(19) 0.0352(16) Uani 1 1 d . . . H15A H 0.1168 0.8407 0.8502 0.053 Uiso 1 1 calc R . . H15B H 0.1809 0.7733 0.8600 0.053 Uiso 1 1 calc R . . H15C H 0.0942 0.7475 0.8590 0.053 Uiso 1 1 calc R . . C16 C 0.0505(3) 0.7623(4) 0.7829(2) 0.0330(16) Uani 1 1 d . . . H16A H 0.0225 0.7172 0.7943 0.050 Uiso 1 1 calc R . . H16B H 0.0513 0.7546 0.7540 0.050 Uiso 1 1 calc R . . H16C H 0.0260 0.8147 0.7883 0.050 Uiso 1 1 calc R . . C17 C 0.5067(3) 0.5717(4) 0.63180(17) 0.0224(13) Uani 1 1 d . . . C18 C 0.5263(4) 0.4891(4) 0.61346(19) 0.0315(15) Uani 1 1 d . . . H18A H 0.5701 0.4959 0.5977 0.047 Uiso 1 1 calc R . . H18B H 0.4835 0.4695 0.5961 0.047 Uiso 1 1 calc R . . H18C H 0.5380 0.4490 0.6348 0.047 Uiso 1 1 calc R . . C19 C 0.5760(3) 0.6045(4) 0.6562(2) 0.0327(16) Uani 1 1 d . . . H19A H 0.5867 0.5697 0.6798 0.049 Uiso 1 1 calc R . . H19B H 0.5665 0.6610 0.6647 0.049 Uiso 1 1 calc R . . H19C H 0.6192 0.6039 0.6398 0.049 Uiso 1 1 calc R . . C20 C 0.4833(4) 0.6315(5) 0.5973(2) 0.046(2) Uani 1 1 d . . . H20A H 0.5236 0.6350 0.5790 0.070 Uiso 1 1 calc R . . H20B H 0.4741 0.6862 0.6082 0.070 Uiso 1 1 calc R . . H20C H 0.4373 0.6114 0.5827 0.070 Uiso 1 1 calc R . . C21 C 0.3852(3) 0.6486(3) 0.68335(16) 0.0191(12) Uani 1 1 d . . . C22 C 0.4450(4) 0.7058(4) 0.70346(18) 0.0271(14) Uani 1 1 d . . . H22A H 0.4204 0.7515 0.7163 0.041 Uiso 1 1 calc R . . H22B H 0.4768 0.7274 0.6833 0.041 Uiso 1 1 calc R . . H22C H 0.4761 0.6750 0.7236 0.041 Uiso 1 1 calc R . . C23 C 0.3405(3) 0.6941(4) 0.64865(18) 0.0272(14) Uani 1 1 d . . . H23A H 0.3033 0.6567 0.6356 0.041 Uiso 1 1 calc R . . H23B H 0.3751 0.7128 0.6292 0.041 Uiso 1 1 calc R . . H23C H 0.3147 0.7417 0.6593 0.041 Uiso 1 1 calc R . . C24 C 0.3306(4) 0.6227(4) 0.71445(18) 0.0289(15) Uani 1 1 d . . . H24A H 0.3055 0.6715 0.7242 0.043 Uiso 1 1 calc R . . H24B H 0.3586 0.5952 0.7369 0.043 Uiso 1 1 calc R . . H24C H 0.2930 0.5849 0.7021 0.043 Uiso 1 1 calc R . . C25 C 0.2050(4) 0.3915(4) 0.78284(19) 0.0262(14) Uani 1 1 d . . . C26 C 0.2342(4) 0.4765(4) 0.7713(2) 0.0442(19) Uani 1 1 d . . . H26A H 0.2142 0.5185 0.7886 0.066 Uiso 1 1 calc R . . H26B H 0.2179 0.4883 0.7434 0.066 Uiso 1 1 calc R . . H26C H 0.2893 0.4770 0.7747 0.066 Uiso 1 1 calc R . . C27 C 0.1204(4) 0.3905(4) 0.7733(2) 0.0372(17) Uani 1 1 d . . . H27A H 0.0990 0.3414 0.7850 0.056 Uiso 1 1 calc R . . H27B H 0.1094 0.3897 0.7442 0.056 Uiso 1 1 calc R . . H27C H 0.0982 0.4398 0.7844 0.056 Uiso 1 1 calc R . . C28 C 0.2264(4) 0.3778(5) 0.8273(2) 0.0428(19) Uani 1 1 d . . . H28A H 0.2117 0.4259 0.8425 0.064 Uiso 1 1 calc R . . H28B H 0.2808 0.3696 0.8315 0.064 Uiso 1 1 calc R . . H28C H 0.2003 0.3290 0.8365 0.064 Uiso 1 1 calc R . . C29 C 0.2224(3) 0.2056(3) 0.76067(18) 0.0227(13) Uani 1 1 d . . . C30 C 0.1393(4) 0.1948(4) 0.7487(3) 0.051(2) Uani 1 1 d . . . H30A H 0.1272 0.2201 0.7225 0.076 Uiso 1 1 calc R . . H30B H 0.1097 0.2212 0.7687 0.076 Uiso 1 1 calc R . . H30C H 0.1272 0.1360 0.7473 0.076 Uiso 1 1 calc R . . C31 C 0.2402(5) 0.1794(4) 0.8038(2) 0.046(2) Uani 1 1 d . . . H31A H 0.2310 0.1203 0.8064 0.069 Uiso 1 1 calc R . . H31B H 0.2080 0.2097 0.8212 0.069 Uiso 1 1 calc R . . H31C H 0.2930 0.1913 0.8118 0.069 Uiso 1 1 calc R . . C32 C 0.2665(5) 0.1519(4) 0.7336(2) 0.046(2) Uani 1 1 d . . . H32A H 0.2470 0.0956 0.7338 0.070 Uiso 1 1 calc R . . H32B H 0.3197 0.1519 0.7432 0.070 Uiso 1 1 calc R . . H32C H 0.2612 0.1736 0.7063 0.070 Uiso 1 1 calc R . . C33 C 0.4474(4) -0.0437(4) 0.63718(18) 0.0289(15) Uani 1 1 d . . . C34 C 0.4954(4) -0.1143(4) 0.6239(2) 0.0397(19) Uani 1 1 d . . . H34A H 0.4725 -0.1666 0.6309 0.060 Uiso 1 1 calc R . . H34B H 0.5459 -0.1103 0.6373 0.060 Uiso 1 1 calc R . . H34C H 0.4987 -0.1116 0.5949 0.060 Uiso 1 1 calc R . . C35 C 0.4414(4) -0.0490(4) 0.68261(18) 0.0337(16) Uani 1 1 d . . . H35A H 0.4199 -0.1022 0.6893 0.051 Uiso 1 1 calc R . . H35B H 0.4089 -0.0047 0.6911 0.051 Uiso 1 1 calc R . . H35C H 0.4915 -0.0433 0.6963 0.051 Uiso 1 1 calc R . . C36 C 0.3691(4) -0.0518(4) 0.6150(2) 0.0384(17) Uani 1 1 d . . . H36A H 0.3737 -0.0474 0.5861 0.058 Uiso 1 1 calc R . . H36B H 0.3364 -0.0079 0.6236 0.058 Uiso 1 1 calc R . . H36C H 0.3474 -0.1053 0.6211 0.058 Uiso 1 1 calc R . . C37 C 0.4557(4) 0.1482(4) 0.64593(17) 0.0244(13) Uani 1 1 d . . . C38 C 0.4821(4) 0.1523(4) 0.69034(18) 0.0319(15) Uani 1 1 d . . . H38A H 0.4617 0.2018 0.7022 0.048 Uiso 1 1 calc R . . H38B H 0.5371 0.1541 0.6932 0.048 Uiso 1 1 calc R . . H38C H 0.4644 0.1035 0.7040 0.048 Uiso 1 1 calc R . . C39 C 0.3701(4) 0.1496(4) 0.6402(2) 0.0335(16) Uani 1 1 d . . . H39A H 0.3494 0.1070 0.6569 0.050 Uiso 1 1 calc R . . H39B H 0.3543 0.1393 0.6121 0.050 Uiso 1 1 calc R . . H39C H 0.3516 0.2036 0.6481 0.050 Uiso 1 1 calc R . . C40 C 0.4875(4) 0.2234(4) 0.62513(19) 0.0302(15) Uani 1 1 d . . . H40A H 0.4723 0.2737 0.6385 0.045 Uiso 1 1 calc R . . H40B H 0.4680 0.2245 0.5971 0.045 Uiso 1 1 calc R . . H40C H 0.5425 0.2200 0.6266 0.045 Uiso 1 1 calc R . . C41 C 0.7916(3) 0.2031(4) 0.49018(17) 0.0220(13) Uani 1 1 d . . . C42 C 0.7971(4) 0.1097(4) 0.4821(2) 0.0343(16) Uani 1 1 d . . . H42A H 0.7514 0.0911 0.4668 0.051 Uiso 1 1 calc R . . H42B H 0.8027 0.0801 0.5076 0.051 Uiso 1 1 calc R . . H42C H 0.8408 0.0987 0.4668 0.051 Uiso 1 1 calc R . . C43 C 0.8655(3) 0.2317(4) 0.5119(2) 0.0336(16) Uani 1 1 d . . . H43A H 0.9079 0.2116 0.4976 0.050 Uiso 1 1 calc R . . H43B H 0.8693 0.2099 0.5392 0.050 Uiso 1 1 calc R . . H43C H 0.8666 0.2919 0.5128 0.050 Uiso 1 1 calc R . . C44 C 0.7782(4) 0.2474(4) 0.4500(2) 0.0392(18) Uani 1 1 d . . . H44A H 0.7810 0.3069 0.4542 0.059 Uiso 1 1 calc R . . H44B H 0.7283 0.2329 0.4378 0.059 Uiso 1 1 calc R . . H44C H 0.8166 0.2306 0.4322 0.059 Uiso 1 1 calc R . . C45 C 0.6851(4) 0.3264(4) 0.53030(19) 0.0315(16) Uani 1 1 d . . . C46 C 0.7518(4) 0.3784(4) 0.5440(2) 0.0399(18) Uani 1 1 d . . . H46A H 0.7344 0.4319 0.5531 0.060 Uiso 1 1 calc R . . H46B H 0.7838 0.3863 0.5218 0.060 Uiso 1 1 calc R . . H46C H 0.7806 0.3507 0.5661 0.060 Uiso 1 1 calc R . . C47 C 0.6455(4) 0.3611(4) 0.4910(2) 0.0402(18) Uani 1 1 d . . . H47A H 0.6289 0.4175 0.4955 0.060 Uiso 1 1 calc R . . H47B H 0.6019 0.3268 0.4828 0.060 Uiso 1 1 calc R . . H47C H 0.6808 0.3608 0.4700 0.060 Uiso 1 1 calc R . . C48 C 0.6269(4) 0.3276(4) 0.5618(2) 0.0403(18) Uani 1 1 d . . . H48A H 0.6512 0.3123 0.5878 0.060 Uiso 1 1 calc R . . H48B H 0.5866 0.2884 0.5542 0.060 Uiso 1 1 calc R . . H48C H 0.6057 0.3830 0.5634 0.060 Uiso 1 1 calc R . . C49 C 0.6759(4) 0.6669(4) 0.48246(17) 0.0269(14) Uani 1 1 d . . . C50 C 0.7178(6) 0.5866(4) 0.4784(2) 0.069(3) Uani 1 1 d . . . H50A H 0.6950 0.5556 0.4556 0.104 Uiso 1 1 calc R . . H50B H 0.7150 0.5542 0.5029 0.104 Uiso 1 1 calc R . . H50C H 0.7706 0.5981 0.4742 0.104 Uiso 1 1 calc R . . C51 C 0.5965(5) 0.6453(9) 0.4911(3) 0.118(6) Uani 1 1 d . . . H51A H 0.5677 0.6958 0.4942 0.177 Uiso 1 1 calc R . . H51B H 0.5972 0.6130 0.5158 0.177 Uiso 1 1 calc R . . H51C H 0.5731 0.6130 0.4689 0.177 Uiso 1 1 calc R . . C52 C 0.6784(5) 0.7130(5) 0.4443(2) 0.061(3) Uani 1 1 d . . . H52A H 0.7304 0.7282 0.4403 0.091 Uiso 1 1 calc R . . H52B H 0.6478 0.7628 0.4454 0.091 Uiso 1 1 calc R . . H52C H 0.6585 0.6783 0.4221 0.091 Uiso 1 1 calc R . . C53 C 0.6837(4) 0.8268(4) 0.5342(2) 0.0391(18) Uani 1 1 d . . . C54 C 0.6991(4) 0.8876(4) 0.5019(3) 0.054(2) Uani 1 1 d . . . H54A H 0.6792 0.9416 0.5088 0.080 Uiso 1 1 calc R . . H54B H 0.6746 0.8691 0.4764 0.080 Uiso 1 1 calc R . . H54C H 0.7534 0.8917 0.4996 0.080 Uiso 1 1 calc R . . C55 C 0.7198(9) 0.8576(7) 0.5738(4) 0.179(9) Uani 1 1 d . . . H55A H 0.6907 0.9040 0.5831 0.268 Uiso 1 1 calc R . . H55B H 0.7714 0.8754 0.5702 0.268 Uiso 1 1 calc R . . H55C H 0.7205 0.8132 0.5935 0.268 Uiso 1 1 calc R . . C56 C 0.5991(5) 0.8239(5) 0.5376(3) 0.080(4) Uani 1 1 d . . . H56A H 0.5873 0.7813 0.5568 0.121 Uiso 1 1 calc R . . H56B H 0.5738 0.8112 0.5114 0.121 Uiso 1 1 calc R . . H56C H 0.5818 0.8774 0.5468 0.121 Uiso 1 1 calc R . . C57 C 1.0583(3) 0.6067(4) 0.65008(18) 0.0258(14) Uani 1 1 d . . . C58 C 1.0228(6) 0.6902(5) 0.6553(3) 0.081(3) Uani 1 1 d . . . H58A H 0.9716 0.6832 0.6636 0.121 Uiso 1 1 calc R . . H58B H 1.0211 0.7202 0.6299 0.121 Uiso 1 1 calc R . . H58C H 1.0528 0.7213 0.6758 0.121 Uiso 1 1 calc R . . C59 C 1.0547(6) 0.5583(6) 0.6877(3) 0.083(4) Uani 1 1 d . . . H59A H 1.0858 0.5088 0.6862 0.125 Uiso 1 1 calc R . . H59B H 1.0025 0.5424 0.6909 0.125 Uiso 1 1 calc R . . H59C H 1.0735 0.5919 0.7105 0.125 Uiso 1 1 calc R . . C60 C 1.1399(4) 0.6159(6) 0.6414(3) 0.063(3) Uani 1 1 d . . . H60A H 1.1667 0.6471 0.6630 0.094 Uiso 1 1 calc R . . H60B H 1.1431 0.6452 0.6160 0.094 Uiso 1 1 calc R . . H60C H 1.1628 0.5614 0.6395 0.094 Uiso 1 1 calc R . . C61 C 1.0419(5) 0.4545(5) 0.5924(3) 0.065(3) Uani 1 1 d . . . C62 C 1.0497(7) 0.3981(5) 0.6292(4) 0.107(5) Uani 1 1 d . . . H62A H 1.0492 0.3405 0.6205 0.161 Uiso 1 1 calc R . . H62B H 1.0078 0.4079 0.6459 0.161 Uiso 1 1 calc R . . H62C H 1.0973 0.4098 0.6447 0.161 Uiso 1 1 calc R . . C63 C 0.9821(7) 0.4164(6) 0.5621(4) 0.109(5) Uani 1 1 d . . . H63A H 0.9971 0.3603 0.5555 0.163 Uiso 1 1 calc R . . H63B H 0.9779 0.4498 0.5377 0.163 Uiso 1 1 calc R . . H63C H 0.9334 0.4150 0.5739 0.163 Uiso 1 1 calc R . . C64 C 1.1134(6) 0.4646(8) 0.5727(4) 0.132(6) Uani 1 1 d . . . H64A H 1.1536 0.4804 0.5927 0.198 Uiso 1 1 calc R . . H64B H 1.1072 0.5076 0.5522 0.198 Uiso 1 1 calc R . . H64C H 1.1265 0.4126 0.5602 0.198 Uiso 1 1 calc R . . Ni1 Ni 0.12229(4) 0.93075(4) 0.69883(2) 0.01683(16) Uani 1 1 d . . . Ni2 Ni 0.35595(4) 0.40334(4) 0.69943(2) 0.01641(15) Uani 1 1 d . . . Ni3 Ni 0.61346(4) 0.10238(4) 0.56770(2) 0.01753(16) Uani 1 1 d . . . Ni4 Ni 0.86400(4) 0.64167(5) 0.56735(2) 0.01897(16) Uani 1 1 d . . . P1 P 0.05707(9) 1.01046(10) 0.62092(4) 0.0202(3) Uani 1 1 d . . . P2 P 0.18375(8) 0.84399(9) 0.77608(4) 0.0163(3) Uani 1 1 d . . . P3 P 0.42912(8) 0.55262(9) 0.66485(4) 0.0168(3) Uani 1 1 d . . . P4 P 0.25205(8) 0.31365(9) 0.75177(4) 0.0176(3) Uani 1 1 d . . . P5 P 0.49372(9) 0.05346(9) 0.62251(4) 0.0194(3) Uani 1 1 d . . . P6 P 0.71131(8) 0.21631(9) 0.52232(4) 0.0171(3) Uani 1 1 d . . . P7 P 0.72593(9) 0.72468(10) 0.52511(5) 0.0218(3) Uani 1 1 d . . . P8 P 1.00298(9) 0.55641(10) 0.60706(5) 0.0254(4) Uani 1 1 d . . . Se1 Se 0.14534(3) 0.91845(4) 0.631038(17) 0.02455(14) Uani 1 1 d . . . Se2 Se 0.03580(3) 1.03692(4) 0.682736(17) 0.02168(13) Uani 1 1 d . . . Se3 Se 0.19162(4) 0.81099(4) 0.713582(17) 0.02385(14) Uani 1 1 d . . . Se4 Se 0.11746(3) 0.95592(3) 0.767486(16) 0.01858(12) Uani 1 1 d . . . Se5 Se 0.34111(3) 0.47356(4) 0.637541(17) 0.02291(13) Uani 1 1 d . . . Se6 Se 0.46889(3) 0.47427(4) 0.714428(17) 0.02065(13) Uani 1 1 d . . . Se7 Se 0.37357(3) 0.32892(4) 0.759860(18) 0.02395(14) Uani 1 1 d . . . Se8 Se 0.23585(3) 0.34503(4) 0.688518(17) 0.02362(14) Uani 1 1 d . . . Se9 Se 0.61563(3) 0.05336(4) 0.633882(18) 0.02514(14) Uani 1 1 d . . . Se10 Se 0.48774(3) 0.06136(4) 0.557561(17) 0.02480(14) Uani 1 1 d . . . Se11 Se 0.61238(3) 0.14696(4) 0.500618(17) 0.02449(14) Uani 1 1 d . . . Se12 Se 0.73572(3) 0.15501(4) 0.579556(17) 0.02202(13) Uani 1 1 d . . . Se13 Se 0.73525(4) 0.64814(5) 0.578602(18) 0.03176(16) Uani 1 1 d . . . Se14 Se 0.84446(4) 0.73651(4) 0.51555(2) 0.03589(18) Uani 1 1 d . . . Se15 Se 0.99157(4) 0.63693(5) 0.55552(2) 0.04056(19) Uani 1 1 d . . . Se16 Se 0.88560(4) 0.54659(5) 0.61931(2) 0.0441(2) 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 C1 0.025(3) 0.041(4) 0.021(3) 0.005(3) 0.001(3) 0.003(3) C2 0.045(5) 0.023(4) 0.049(5) -0.002(3) -0.008(4) 0.003(3) C3 0.022(4) 0.050(5) 0.084(6) 0.027(4) -0.007(4) 0.001(3) C4 0.047(5) 0.154(10) 0.024(4) -0.019(5) 0.004(4) -0.046(6) C5 0.032(4) 0.026(3) 0.024(3) 0.007(3) 0.006(3) 0.006(3) C6 0.055(6) 0.079(7) 0.067(6) 0.026(5) 0.000(5) -0.033(5) C7 0.143(10) 0.027(4) 0.050(5) 0.006(4) 0.055(6) -0.003(5) C8 0.046(5) 0.020(4) 0.099(7) 0.015(4) 0.017(5) 0.007(3) C9 0.014(3) 0.023(3) 0.017(3) 0.002(2) 0.001(2) 0.000(2) C10 0.024(3) 0.033(4) 0.028(3) -0.006(3) -0.003(3) -0.004(3) C11 0.026(4) 0.025(3) 0.037(4) -0.003(3) -0.009(3) 0.007(3) C12 0.020(3) 0.038(4) 0.038(4) 0.008(3) 0.008(3) -0.006(3) C13 0.021(3) 0.021(3) 0.033(4) 0.011(3) -0.003(3) -0.003(2) C14 0.036(4) 0.020(3) 0.055(5) 0.014(3) -0.004(3) -0.002(3) C15 0.038(4) 0.042(4) 0.026(4) 0.012(3) 0.005(3) -0.008(3) C16 0.018(3) 0.035(4) 0.046(4) 0.009(3) -0.003(3) -0.010(3) C17 0.022(3) 0.027(3) 0.019(3) 0.000(2) 0.007(2) 0.005(3) C18 0.029(4) 0.036(4) 0.031(4) -0.006(3) 0.008(3) 0.011(3) C19 0.023(4) 0.039(4) 0.038(4) 0.004(3) 0.014(3) 0.001(3) C20 0.047(5) 0.059(5) 0.037(4) 0.022(4) 0.028(4) 0.018(4) C21 0.023(3) 0.018(3) 0.017(3) 0.003(2) 0.007(2) 0.007(2) C22 0.030(4) 0.023(3) 0.028(3) -0.004(3) 0.002(3) 0.002(3) C23 0.022(3) 0.031(4) 0.030(3) 0.010(3) 0.005(3) 0.006(3) C24 0.030(4) 0.033(4) 0.025(3) 0.002(3) 0.013(3) 0.005(3) C25 0.028(4) 0.020(3) 0.031(4) -0.002(3) 0.005(3) 0.004(3) C26 0.057(5) 0.022(4) 0.056(5) -0.004(3) 0.021(4) -0.006(3) C27 0.026(4) 0.039(4) 0.048(4) -0.003(3) 0.009(3) 0.009(3) C28 0.050(5) 0.048(5) 0.030(4) -0.017(3) 0.003(3) 0.010(4) C29 0.026(3) 0.015(3) 0.028(3) 0.003(2) 0.003(3) 0.001(2) C30 0.032(4) 0.022(4) 0.095(7) 0.005(4) -0.008(4) -0.010(3) C31 0.071(6) 0.028(4) 0.038(4) 0.010(3) 0.005(4) -0.005(4) C32 0.066(5) 0.021(4) 0.058(5) -0.003(3) 0.034(4) 0.006(3) C33 0.037(4) 0.029(4) 0.022(3) 0.001(3) 0.010(3) -0.006(3) C34 0.063(5) 0.021(3) 0.039(4) -0.004(3) 0.026(4) -0.005(3) C35 0.053(5) 0.026(4) 0.024(3) -0.001(3) 0.013(3) -0.005(3) C36 0.039(4) 0.044(4) 0.033(4) -0.008(3) 0.011(3) -0.020(3) C37 0.035(4) 0.021(3) 0.016(3) 0.001(2) 0.001(3) 0.007(3) C38 0.039(4) 0.033(4) 0.024(3) -0.009(3) 0.000(3) 0.006(3) C39 0.031(4) 0.036(4) 0.033(4) 0.007(3) 0.005(3) 0.012(3) C40 0.035(4) 0.022(3) 0.033(4) 0.002(3) 0.001(3) -0.001(3) C41 0.022(3) 0.023(3) 0.022(3) 0.003(2) 0.007(3) 0.000(2) C42 0.033(4) 0.032(4) 0.039(4) -0.004(3) 0.016(3) 0.002(3) C43 0.021(3) 0.042(4) 0.038(4) -0.003(3) 0.006(3) -0.004(3) C44 0.044(4) 0.046(4) 0.030(4) 0.003(3) 0.016(3) 0.009(4) C45 0.048(4) 0.021(3) 0.024(3) -0.003(3) -0.002(3) 0.010(3) C46 0.053(5) 0.021(4) 0.044(4) -0.009(3) -0.008(4) 0.001(3) C47 0.048(5) 0.031(4) 0.041(4) 0.005(3) -0.007(3) 0.013(3) C48 0.052(5) 0.035(4) 0.034(4) -0.006(3) 0.003(3) 0.020(3) C49 0.029(4) 0.034(4) 0.017(3) -0.008(3) 0.002(3) -0.004(3) C50 0.131(9) 0.026(4) 0.044(5) -0.017(4) -0.033(5) 0.011(5) C51 0.046(6) 0.257(17) 0.054(6) -0.075(8) 0.011(5) -0.061(8) C52 0.098(7) 0.045(5) 0.032(4) 0.013(4) -0.035(4) -0.017(5) C53 0.051(5) 0.030(4) 0.033(4) -0.011(3) -0.016(3) 0.019(3) C54 0.045(5) 0.015(3) 0.106(7) 0.003(4) 0.036(5) 0.006(3) C55 0.280(19) 0.096(9) 0.136(11) -0.102(9) -0.160(13) 0.119(11) C56 0.090(7) 0.054(6) 0.107(8) 0.048(5) 0.080(7) 0.045(5) C57 0.024(3) 0.026(3) 0.026(3) 0.005(3) -0.006(3) -0.002(3) C58 0.089(8) 0.055(6) 0.090(8) -0.047(5) -0.039(6) 0.029(5) C59 0.103(8) 0.094(8) 0.046(5) 0.032(5) -0.032(5) -0.057(7) C60 0.035(5) 0.088(7) 0.064(6) -0.023(5) -0.004(4) -0.024(5) C61 0.059(6) 0.031(4) 0.100(8) -0.033(5) -0.037(5) 0.012(4) C62 0.127(10) 0.021(5) 0.159(12) 0.013(6) -0.090(9) 0.014(5) C63 0.125(10) 0.058(7) 0.130(10) -0.041(7) -0.083(9) 0.018(7) C64 0.076(9) 0.110(10) 0.209(16) -0.097(10) -0.002(9) 0.043(8) Ni1 0.0188(4) 0.0188(4) 0.0128(3) 0.0016(3) 0.0006(3) 0.0053(3) Ni2 0.0168(4) 0.0149(4) 0.0173(4) 0.0008(3) -0.0001(3) 0.0002(3) Ni3 0.0190(4) 0.0199(4) 0.0137(3) 0.0000(3) 0.0015(3) 0.0014(3) Ni4 0.0158(4) 0.0239(4) 0.0169(4) 0.0049(3) -0.0008(3) 0.0017(3) P1 0.0201(8) 0.0261(8) 0.0150(7) 0.0051(6) 0.0039(6) 0.0071(6) P2 0.0171(8) 0.0153(7) 0.0161(7) 0.0028(6) -0.0016(6) 0.0011(6) P3 0.0152(7) 0.0196(8) 0.0156(7) 0.0009(6) 0.0007(6) 0.0009(6) P4 0.0181(8) 0.0163(7) 0.0182(7) 0.0019(6) -0.0001(6) 0.0003(6) P5 0.0217(8) 0.0221(8) 0.0143(7) 0.0011(6) 0.0006(6) -0.0013(6) P6 0.0190(8) 0.0179(7) 0.0140(7) -0.0009(6) -0.0012(6) 0.0013(6) P7 0.0213(8) 0.0236(8) 0.0195(8) -0.0021(6) -0.0047(6) 0.0069(6) P8 0.0200(8) 0.0206(8) 0.0343(9) 0.0048(7) -0.0077(7) 0.0006(6) Se1 0.0249(3) 0.0344(4) 0.0147(3) 0.0025(2) 0.0039(2) 0.0142(3) Se2 0.0253(3) 0.0255(3) 0.0146(3) 0.0028(2) 0.0036(2) 0.0108(3) Se3 0.0317(4) 0.0216(3) 0.0176(3) -0.0028(2) -0.0032(3) 0.0118(3) Se4 0.0239(3) 0.0174(3) 0.0143(3) 0.0003(2) 0.0000(2) 0.0060(2) Se5 0.0260(3) 0.0254(3) 0.0164(3) 0.0015(2) -0.0044(2) -0.0052(3) Se6 0.0178(3) 0.0224(3) 0.0211(3) 0.0057(2) -0.0035(2) -0.0008(2) Se7 0.0155(3) 0.0320(3) 0.0239(3) 0.0100(3) -0.0022(2) -0.0009(2) Se8 0.0230(3) 0.0259(3) 0.0209(3) 0.0050(2) -0.0057(2) -0.0064(3) Se9 0.0212(3) 0.0354(4) 0.0187(3) 0.0079(3) 0.0002(2) 0.0055(3) Se10 0.0252(3) 0.0348(4) 0.0141(3) 0.0024(3) 0.0000(2) -0.0083(3) Se11 0.0220(3) 0.0376(4) 0.0135(3) 0.0013(3) -0.0015(2) -0.0082(3) Se12 0.0212(3) 0.0269(3) 0.0172(3) 0.0037(2) -0.0035(2) -0.0011(2) Se13 0.0180(3) 0.0586(5) 0.0188(3) 0.0085(3) 0.0021(2) 0.0049(3) Se14 0.0204(3) 0.0431(4) 0.0433(4) 0.0285(3) -0.0037(3) -0.0014(3) Se15 0.0184(3) 0.0679(5) 0.0359(4) 0.0261(4) 0.0054(3) 0.0064(3) Se16 0.0205(4) 0.0642(5) 0.0457(4) 0.0384(4) -0.0104(3) -0.0117(3) _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 C1 C4 1.519(9) . ? C1 C2 1.521(9) . ? C1 C3 1.538(9) . ? C1 P1 1.871(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.516(9) . ? C5 C8 1.534(9) . ? C5 C6 1.543(10) . ? C5 P1 1.863(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.530(8) . ? C9 C12 1.536(8) . ? C9 C10 1.539(8) . ? C9 P2 1.863(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.535(9) . ? C13 C15 1.538(9) . ? C13 C16 1.539(8) . ? C13 P2 1.865(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.528(9) . ? C17 C18 1.529(8) . ? C17 C20 1.547(9) . ? C17 P3 1.861(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.534(8) . ? C21 C24 1.537(8) . ? C21 C23 1.551(8) . ? C21 P3 1.873(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.521(9) . ? C25 C28 1.529(9) . ? C25 C26 1.538(9) . ? C25 P4 1.876(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.518(9) . ? C29 C32 1.520(8) . ? C29 C31 1.521(9) . ? C29 P4 1.865(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.518(9) . ? C33 C35 1.538(8) . ? C33 C36 1.540(9) . ? C33 P5 1.865(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.525(9) . ? C37 C38 1.531(8) . ? C37 C40 1.537(8) . ? C37 P5 1.879(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.532(8) . ? C41 C44 1.533(8) . ? C41 C42 1.547(8) . ? C41 P6 1.867(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.504(9) . ? C45 C48 1.533(9) . ? C45 C47 1.555(9) . ? C45 P6 1.874(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C52 1.486(9) . ? C49 C51 1.508(10) . ? C49 C50 1.515(10) . ? C49 P7 1.881(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.505(10) . ? C53 C55 1.518(10) . ? C53 C56 1.524(11) . ? C53 P7 1.857(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C59 1.491(9) . ? C57 C58 1.514(10) . ? C57 C60 1.514(10) . ? C57 P8 1.875(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C64 1.487(15) . ? C61 C62 1.537(14) . ? C61 C63 1.548(11) . ? C61 P8 1.876(8) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? Ni1 Se3 2.3408(9) . ? Ni1 Se4 2.3467(9) . ? Ni1 Se1 2.3482(9) . ? Ni1 Se2 2.3520(9) . ? Ni2 Se6 2.3442(9) . ? Ni2 Se8 2.3473(9) . ? Ni2 Se7 2.3621(9) . ? Ni2 Se5 2.3671(9) . ? Ni3 Se10 2.3408(9) . ? Ni3 Se12 2.3499(9) . ? Ni3 Se9 2.3563(9) . ? Ni3 Se11 2.3626(9) . ? Ni4 Se14 2.3305(9) . ? Ni4 Se15 2.3396(10) . ? Ni4 Se16 2.3409(10) . ? Ni4 Se13 2.3568(9) . ? P1 Se2 2.1777(16) . ? P1 Se1 2.1809(16) . ? P2 Se3 2.1782(15) . ? P2 Se4 2.1785(15) . ? P3 Se6 2.1725(15) . ? P3 Se5 2.1792(16) . ? P4 Se7 2.1792(16) . ? P4 Se8 2.1807(16) . ? P5 Se10 2.1770(16) . ? P5 Se9 2.1806(16) . ? P6 Se11 2.1749(16) . ? P6 Se12 2.1789(15) . ? P7 Se14 2.1703(17) . ? P7 Se13 2.1800(17) . ? P8 Se15 2.1663(18) . ? P8 Se16 2.1690(18) . ? 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 C4 C1 C2 110.3(6) . . ? C4 C1 C3 110.1(6) . . ? C2 C1 C3 107.8(6) . . ? C4 C1 P1 110.6(5) . . ? C2 C1 P1 107.7(4) . . ? C3 C1 P1 110.2(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C8 110.5(6) . . ? C7 C5 C6 108.2(7) . . ? C8 C5 C6 106.8(6) . . ? C7 C5 P1 111.4(5) . . ? C8 C5 P1 111.7(5) . . ? C6 C5 P1 108.0(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C12 107.9(5) . . ? C11 C9 C10 111.0(5) . . ? C12 C9 C10 107.8(5) . . ? C11 C9 P2 112.7(4) . . ? C12 C9 P2 106.9(4) . . ? C10 C9 P2 110.2(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 110.7(5) . . ? C14 C13 C16 107.8(5) . . ? C15 C13 C16 109.6(5) . . ? C14 C13 P2 111.0(4) . . ? C15 C13 P2 110.4(4) . . ? C16 C13 P2 107.3(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 108.8(5) . . ? C19 C17 C20 110.2(6) . . ? C18 C17 C20 108.0(5) . . ? C19 C17 P3 110.3(4) . . ? C18 C17 P3 107.2(4) . . ? C20 C17 P3 112.3(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C24 108.8(5) . . ? C22 C21 C23 110.1(5) . . ? C24 C21 C23 108.9(5) . . ? C22 C21 P3 110.9(4) . . ? C24 C21 P3 107.3(4) . . ? C23 C21 P3 110.7(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 112.2(6) . . ? C27 C25 C26 107.8(6) . . ? C28 C25 C26 108.1(6) . . ? C27 C25 P4 110.7(4) . . ? C28 C25 P4 110.7(4) . . ? C26 C25 P4 107.1(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C32 108.3(6) . . ? C30 C29 C31 110.5(6) . . ? C32 C29 C31 109.1(6) . . ? C30 C29 P4 110.5(4) . . ? C32 C29 P4 106.3(4) . . ? C31 C29 P4 112.0(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 109.3(5) . . ? C34 C33 C36 107.7(6) . . ? C35 C33 C36 110.3(5) . . ? C34 C33 P5 107.1(4) . . ? C35 C33 P5 111.9(4) . . ? C36 C33 P5 110.4(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 110.8(5) . . ? C39 C37 C40 109.3(5) . . ? C38 C37 C40 108.1(5) . . ? C39 C37 P5 110.4(4) . . ? C38 C37 P5 110.3(4) . . ? C40 C37 P5 107.9(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 110.5(5) . . ? C43 C41 C42 108.5(5) . . ? C44 C41 C42 108.4(5) . . ? C43 C41 P6 111.1(4) . . ? C44 C41 P6 112.1(4) . . ? C42 C41 P6 106.0(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C48 110.0(6) . . ? C46 C45 C47 110.8(6) . . ? C48 C45 C47 106.8(6) . . ? C46 C45 P6 112.4(5) . . ? C48 C45 P6 107.4(5) . . ? C47 C45 P6 109.2(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C49 C51 111.7(7) . . ? C52 C49 C50 108.2(6) . . ? C51 C49 C50 107.0(8) . . ? C52 C49 P7 111.2(5) . . ? C51 C49 P7 111.7(5) . . ? C50 C49 P7 106.8(5) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C55 108.9(9) . . ? C54 C53 C56 107.9(6) . . ? C55 C53 C56 107.6(9) . . ? C54 C53 P7 111.9(5) . . ? C55 C53 P7 106.7(5) . . ? C56 C53 P7 113.6(6) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C59 C57 C58 109.4(8) . . ? C59 C57 C60 108.4(7) . . ? C58 C57 C60 110.4(7) . . ? C59 C57 P8 111.6(5) . . ? C58 C57 P8 106.2(5) . . ? C60 C57 P8 110.7(5) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C64 C61 C62 113.1(9) . . ? C64 C61 C63 109.0(10) . . ? C62 C61 C63 107.8(8) . . ? C64 C61 P8 111.4(7) . . ? C62 C61 P8 109.3(7) . . ? C63 C61 P8 106.0(6) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Se3 Ni1 Se4 89.66(3) . . ? Se3 Ni1 Se1 90.39(3) . . ? Se4 Ni1 Se1 170.57(4) . . ? Se3 Ni1 Se2 170.77(4) . . ? Se4 Ni1 Se2 91.54(3) . . ? Se1 Ni1 Se2 89.91(3) . . ? Se6 Ni2 Se8 173.10(4) . . ? Se6 Ni2 Se7 90.53(3) . . ? Se8 Ni2 Se7 89.42(3) . . ? Se6 Ni2 Se5 89.45(3) . . ? Se8 Ni2 Se5 90.89(3) . . ? Se7 Ni2 Se5 177.60(4) . . ? Se10 Ni3 Se12 174.92(4) . . ? Se10 Ni3 Se9 89.45(3) . . ? Se12 Ni3 Se9 90.70(3) . . ? Se10 Ni3 Se11 90.44(3) . . ? Se12 Ni3 Se11 89.58(3) . . ? Se9 Ni3 Se11 178.03(4) . . ? Se14 Ni4 Se15 89.43(3) . . ? Se14 Ni4 Se16 179.13(4) . . ? Se15 Ni4 Se16 89.71(3) . . ? Se14 Ni4 Se13 89.72(3) . . ? Se15 Ni4 Se13 179.14(4) . . ? Se16 Ni4 Se13 91.14(3) . . ? C5 P1 C1 114.0(3) . . ? C5 P1 Se2 112.1(2) . . ? C1 P1 Se2 109.5(2) . . ? C5 P1 Se1 109.4(2) . . ? C1 P1 Se1 111.7(2) . . ? Se2 P1 Se1 99.28(6) . . ? C9 P2 C13 113.5(3) . . ? C9 P2 Se3 111.88(18) . . ? C13 P2 Se3 110.2(2) . . ? C9 P2 Se4 110.10(19) . . ? C13 P2 Se4 111.5(2) . . ? Se3 P2 Se4 98.67(6) . . ? C17 P3 C21 113.9(3) . . ? C17 P3 Se6 109.76(19) . . ? C21 P3 Se6 110.89(18) . . ? C17 P3 Se5 113.1(2) . . ? C21 P3 Se5 108.97(19) . . ? Se6 P3 Se5 99.26(6) . . ? C29 P4 C25 113.8(3) . . ? C29 P4 Se7 112.2(2) . . ? C25 P4 Se7 109.6(2) . . ? C29 P4 Se8 110.9(2) . . ? C25 P4 Se8 110.5(2) . . ? Se7 P4 Se8 98.91(6) . . ? C33 P5 C37 113.9(3) . . ? C33 P5 Se10 108.9(2) . . ? C37 P5 Se10 112.15(19) . . ? C33 P5 Se9 114.1(2) . . ? C37 P5 Se9 108.2(2) . . ? Se10 P5 Se9 98.67(6) . . ? C41 P6 C45 113.7(3) . . ? C41 P6 Se11 112.6(2) . . ? C45 P6 Se11 109.8(2) . . ? C41 P6 Se12 110.08(19) . . ? C45 P6 Se12 110.3(2) . . ? Se11 P6 Se12 99.38(6) . . ? C53 P7 C49 113.3(3) . . ? C53 P7 Se14 110.8(3) . . ? C49 P7 Se14 110.2(2) . . ? C53 P7 Se13 112.6(2) . . ? C49 P7 Se13 110.1(2) . . ? Se14 P7 Se13 98.94(6) . . ? C57 P8 C61 113.8(3) . . ? C57 P8 Se15 111.4(2) . . ? C61 P8 Se15 109.9(3) . . ? C57 P8 Se16 110.3(2) . . ? C61 P8 Se16 111.4(3) . . ? Se15 P8 Se16 99.19(7) . . ? P1 Se1 Ni1 85.24(5) . . ? P1 Se2 Ni1 85.22(5) . . ? P2 Se3 Ni1 85.90(4) . . ? P2 Se4 Ni1 85.75(5) . . ? P3 Se5 Ni2 83.38(5) . . ? P3 Se6 Ni2 84.07(5) . . ? P4 Se7 Ni2 83.25(5) . . ? P4 Se8 Ni2 83.56(5) . . ? P5 Se9 Ni3 83.51(5) . . ? P5 Se10 Ni3 83.96(5) . . ? P6 Se11 Ni3 83.70(5) . . ? P6 Se12 Ni3 83.91(5) . . ? P7 Se13 Ni4 84.88(5) . . ? P7 Se14 Ni4 85.74(5) . . ? P8 Se15 Ni4 85.46(5) . . ? P8 Se16 Ni4 85.37(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C5 P1 C1 -73.1(6) . . . . ? C8 C5 P1 C1 51.0(6) . . . . ? C6 C5 P1 C1 168.2(5) . . . . ? C7 C5 P1 Se2 161.8(5) . . . . ? C8 C5 P1 Se2 -74.1(5) . . . . ? C6 C5 P1 Se2 43.1(6) . . . . ? C7 C5 P1 Se1 52.8(6) . . . . ? C8 C5 P1 Se1 176.8(5) . . . . ? C6 C5 P1 Se1 -66.0(5) . . . . ? C4 C1 P1 C5 49.6(7) . . . . ? C2 C1 P1 C5 170.3(4) . . . . ? C3 C1 P1 C5 -72.3(5) . . . . ? C4 C1 P1 Se2 176.0(5) . . . . ? C2 C1 P1 Se2 -63.3(5) . . . . ? C3 C1 P1 Se2 54.1(5) . . . . ? C4 C1 P1 Se1 -75.0(6) . . . . ? C2 C1 P1 Se1 45.6(5) . . . . ? C3 C1 P1 Se1 163.0(4) . . . . ? C11 C9 P2 C13 48.9(5) . . . . ? C12 C9 P2 C13 167.3(4) . . . . ? C10 C9 P2 C13 -75.8(5) . . . . ? C11 C9 P2 Se3 -76.7(4) . . . . ? C12 C9 P2 Se3 41.8(4) . . . . ? C10 C9 P2 Se3 158.7(3) . . . . ? C11 C9 P2 Se4 174.7(4) . . . . ? C12 C9 P2 Se4 -66.9(4) . . . . ? C10 C9 P2 Se4 50.0(4) . . . . ? C14 C13 P2 C9 -73.7(5) . . . . ? C15 C13 P2 C9 49.5(5) . . . . ? C16 C13 P2 C9 168.8(4) . . . . ? C14 C13 P2 Se3 52.7(5) . . . . ? C15 C13 P2 Se3 175.9(4) . . . . ? C16 C13 P2 Se3 -64.8(5) . . . . ? C14 C13 P2 Se4 161.2(4) . . . . ? C15 C13 P2 Se4 -75.6(4) . . . . ? C16 C13 P2 Se4 43.7(5) . . . . ? C19 C17 P3 C21 71.8(5) . . . . ? C18 C17 P3 C21 -169.9(4) . . . . ? C20 C17 P3 C21 -51.4(6) . . . . ? C19 C17 P3 Se6 -53.2(4) . . . . ? C18 C17 P3 Se6 65.1(4) . . . . ? C20 C17 P3 Se6 -176.5(4) . . . . ? C19 C17 P3 Se5 -163.0(4) . . . . ? C18 C17 P3 Se5 -44.7(4) . . . . ? C20 C17 P3 Se5 73.7(5) . . . . ? C22 C21 P3 C17 -53.5(5) . . . . ? C24 C21 P3 C17 -172.3(4) . . . . ? C23 C21 P3 C17 69.0(5) . . . . ? C22 C21 P3 Se6 70.9(4) . . . . ? C24 C21 P3 Se6 -47.9(4) . . . . ? C23 C21 P3 Se6 -166.5(3) . . . . ? C22 C21 P3 Se5 179.1(3) . . . . ? C24 C21 P3 Se5 60.4(4) . . . . ? C23 C21 P3 Se5 -58.3(4) . . . . ? C30 C29 P4 C25 63.4(6) . . . . ? C32 C29 P4 C25 -179.4(5) . . . . ? C31 C29 P4 C25 -60.3(5) . . . . ? C30 C29 P4 Se7 -171.5(4) . . . . ? C32 C29 P4 Se7 -54.2(5) . . . . ? C31 C29 P4 Se7 64.8(5) . . . . ? C30 C29 P4 Se8 -61.9(5) . . . . ? C32 C29 P4 Se8 55.4(5) . . . . ? C31 C29 P4 Se8 174.4(4) . . . . ? C27 C25 P4 C29 -61.6(5) . . . . ? C28 C25 P4 C29 63.4(5) . . . . ? C26 C25 P4 C29 -178.9(5) . . . . ? C27 C25 P4 Se7 171.9(4) . . . . ? C28 C25 P4 Se7 -63.1(5) . . . . ? C26 C25 P4 Se7 54.6(5) . . . . ? C27 C25 P4 Se8 63.9(5) . . . . ? C28 C25 P4 Se8 -171.1(4) . . . . ? C26 C25 P4 Se8 -53.4(5) . . . . ? C34 C33 P5 C37 -167.3(4) . . . . ? C35 C33 P5 C37 -47.6(6) . . . . ? C36 C33 P5 C37 75.8(5) . . . . ? C34 C33 P5 Se10 66.8(5) . . . . ? C35 C33 P5 Se10 -173.5(4) . . . . ? C36 C33 P5 Se10 -50.1(5) . . . . ? C34 C33 P5 Se9 -42.3(5) . . . . ? C35 C33 P5 Se9 77.4(5) . . . . ? C36 C33 P5 Se9 -159.3(4) . . . . ? C39 C37 P5 C33 -49.8(5) . . . . ? C38 C37 P5 C33 73.1(5) . . . . ? C40 C37 P5 C33 -169.1(4) . . . . ? C39 C37 P5 Se10 74.4(4) . . . . ? C38 C37 P5 Se10 -162.8(4) . . . . ? C40 C37 P5 Se10 -44.9(5) . . . . ? C39 C37 P5 Se9 -177.8(4) . . . . ? C38 C37 P5 Se9 -55.0(5) . . . . ? C40 C37 P5 Se9 62.9(4) . . . . ? C43 C41 P6 C45 70.3(5) . . . . ? C44 C41 P6 C45 -53.9(5) . . . . ? C42 C41 P6 C45 -172.0(4) . . . . ? C43 C41 P6 Se11 -164.0(4) . . . . ? C44 C41 P6 Se11 71.8(5) . . . . ? C42 C41 P6 Se11 -46.3(5) . . . . ? C43 C41 P6 Se12 -54.1(5) . . . . ? C44 C41 P6 Se12 -178.3(4) . . . . ? C42 C41 P6 Se12 63.6(4) . . . . ? C46 C45 P6 C41 -50.8(6) . . . . ? C48 C45 P6 C41 -171.9(4) . . . . ? C47 C45 P6 C41 72.5(6) . . . . ? C46 C45 P6 Se11 -178.0(4) . . . . ? C48 C45 P6 Se11 60.8(5) . . . . ? C47 C45 P6 Se11 -54.7(5) . . . . ? C46 C45 P6 Se12 73.4(5) . . . . ? C48 C45 P6 Se12 -47.7(5) . . . . ? C47 C45 P6 Se12 -163.2(4) . . . . ? C54 C53 P7 C49 -71.9(6) . . . . ? C55 C53 P7 C49 169.1(9) . . . . ? C56 C53 P7 C49 50.6(7) . . . . ? C54 C53 P7 Se14 52.6(6) . . . . ? C55 C53 P7 Se14 -66.5(9) . . . . ? C56 C53 P7 Se14 175.1(5) . . . . ? C54 C53 P7 Se13 162.3(5) . . . . ? C55 C53 P7 Se13 43.3(9) . . . . ? C56 C53 P7 Se13 -75.2(6) . . . . ? C52 C49 P7 C53 61.0(6) . . . . ? C51 C49 P7 C53 -64.5(8) . . . . ? C50 C49 P7 C53 178.8(6) . . . . ? C52 C49 P7 Se14 -63.8(6) . . . . ? C51 C49 P7 Se14 170.7(7) . . . . ? C50 C49 P7 Se14 54.0(6) . . . . ? C52 C49 P7 Se13 -171.9(5) . . . . ? C51 C49 P7 Se13 62.5(8) . . . . ? C50 C49 P7 Se13 -54.1(5) . . . . ? C59 C57 P8 C61 -65.5(8) . . . . ? C58 C57 P8 C61 175.4(7) . . . . ? C60 C57 P8 C61 55.5(7) . . . . ? C59 C57 P8 Se15 169.7(6) . . . . ? C58 C57 P8 Se15 50.6(6) . . . . ? C60 C57 P8 Se15 -69.4(5) . . . . ? C59 C57 P8 Se16 60.6(6) . . . . ? C58 C57 P8 Se16 -58.5(6) . . . . ? C60 C57 P8 Se16 -178.5(5) . . . . ? C64 C61 P8 C57 -71.3(9) . . . . ? C62 C61 P8 C57 54.4(8) . . . . ? C63 C61 P8 C57 170.3(7) . . . . ? C64 C61 P8 Se15 54.3(8) . . . . ? C62 C61 P8 Se15 180.0(6) . . . . ? C63 C61 P8 Se15 -64.0(8) . . . . ? C64 C61 P8 Se16 163.2(7) . . . . ? C62 C61 P8 Se16 -71.1(6) . . . . ? C63 C61 P8 Se16 44.9(9) . . . . ? C5 P1 Se1 Ni1 122.2(2) . . . . ? C1 P1 Se1 Ni1 -110.7(2) . . . . ? Se2 P1 Se1 Ni1 4.73(6) . . . . ? Se3 Ni1 Se1 P1 166.46(5) . . . . ? Se4 Ni1 Se1 P1 -103.2(2) . . . . ? Se2 Ni1 Se1 P1 -4.32(5) . . . . ? C5 P1 Se2 Ni1 -120.1(2) . . . . ? C1 P1 Se2 Ni1 112.4(2) . . . . ? Se1 P1 Se2 Ni1 -4.72(6) . . . . ? Se3 Ni1 Se2 P1 -87.6(2) . . . . ? Se4 Ni1 Se2 P1 175.01(5) . . . . ? Se1 Ni1 Se2 P1 4.33(5) . . . . ? C9 P2 Se3 Ni1 -114.9(2) . . . . ? C13 P2 Se3 Ni1 117.8(2) . . . . ? Se4 P2 Se3 Ni1 0.96(5) . . . . ? Se4 Ni1 Se3 P2 -0.88(5) . . . . ? Se1 Ni1 Se3 P2 169.69(5) . . . . ? Se2 Ni1 Se3 P2 -98.4(2) . . . . ? C9 P2 Se4 Ni1 116.25(19) . . . . ? C13 P2 Se4 Ni1 -116.8(2) . . . . ? Se3 P2 Se4 Ni1 -0.96(5) . . . . ? Se3 Ni1 Se4 P2 0.88(5) . . . . ? Se1 Ni1 Se4 P2 -89.5(2) . . . . ? Se2 Ni1 Se4 P2 171.73(5) . . . . ? C17 P3 Se5 Ni2 131.7(2) . . . . ? C21 P3 Se5 Ni2 -100.55(18) . . . . ? Se6 P3 Se5 Ni2 15.43(5) . . . . ? Se6 Ni2 Se5 P3 -14.09(5) . . . . ? Se8 Ni2 Se5 P3 159.02(5) . . . . ? Se7 Ni2 Se5 P3 -103.8(10) . . . . ? C17 P3 Se6 Ni2 -134.3(2) . . . . ? C21 P3 Se6 Ni2 98.9(2) . . . . ? Se5 P3 Se6 Ni2 -15.56(5) . . . . ? Se8 Ni2 Se6 P3 -78.7(3) . . . . ? Se7 Ni2 Se6 P3 -168.29(5) . . . . ? Se5 Ni2 Se6 P3 14.11(5) . . . . ? C29 P4 Se7 Ni2 134.4(2) . . . . ? C25 P4 Se7 Ni2 -98.2(2) . . . . ? Se8 P4 Se7 Ni2 17.35(5) . . . . ? Se6 Ni2 Se7 P4 157.21(5) . . . . ? Se8 Ni2 Se7 P4 -15.88(5) . . . . ? Se5 Ni2 Se7 P4 -113.1(10) . . . . ? C29 P4 Se8 Ni2 -135.5(2) . . . . ? C25 P4 Se8 Ni2 97.4(2) . . . . ? Se7 P4 Se8 Ni2 -17.45(5) . . . . ? Se6 Ni2 Se8 P4 -73.8(3) . . . . ? Se7 Ni2 Se8 P4 15.86(5) . . . . ? Se5 Ni2 Se8 P4 -166.52(5) . . . . ? C33 P5 Se9 Ni3 131.8(2) . . . . ? C37 P5 Se9 Ni3 -100.4(2) . . . . ? Se10 P5 Se9 Ni3 16.48(5) . . . . ? Se10 Ni3 Se9 P5 -15.12(5) . . . . ? Se12 Ni3 Se9 P5 159.80(5) . . . . ? Se11 Ni3 Se9 P5 -102.1(12) . . . . ? C33 P5 Se10 Ni3 -135.8(2) . . . . ? C37 P5 Se10 Ni3 97.2(2) . . . . ? Se9 P5 Se10 Ni3 -16.58(5) . . . . ? Se12 Ni3 Se10 P5 -76.6(5) . . . . ? Se9 Ni3 Se10 P5 15.14(5) . . . . ? Se11 Ni3 Se10 P5 -166.83(5) . . . . ? C41 P6 Se11 Ni3 131.1(2) . . . . ? C45 P6 Se11 Ni3 -101.0(2) . . . . ? Se12 P6 Se11 Ni3 14.64(5) . . . . ? Se10 Ni3 Se11 P6 161.56(5) . . . . ? Se12 Ni3 Se11 P6 -13.37(5) . . . . ? Se9 Ni3 Se11 P6 -111.5(12) . . . . ? C41 P6 Se12 Ni3 -133.1(2) . . . . ? C45 P6 Se12 Ni3 100.5(2) . . . . ? Se11 P6 Se12 Ni3 -14.71(5) . . . . ? Se10 Ni3 Se12 P6 -76.9(5) . . . . ? Se9 Ni3 Se12 P6 -168.61(5) . . . . ? Se11 Ni3 Se12 P6 13.33(5) . . . . ? C53 P7 Se13 Ni4 -123.8(3) . . . . ? C49 P7 Se13 Ni4 108.7(2) . . . . ? Se14 P7 Se13 Ni4 -6.71(6) . . . . ? Se14 Ni4 Se13 P7 6.17(5) . . . . ? Se15 Ni4 Se13 P7 16(4) . . . . ? Se16 Ni4 Se13 P7 -173.97(5) . . . . ? C53 P7 Se14 Ni4 125.2(2) . . . . ? C49 P7 Se14 Ni4 -108.6(2) . . . . ? Se13 P7 Se14 Ni4 6.78(6) . . . . ? Se15 Ni4 Se14 P7 173.95(5) . . . . ? Se16 Ni4 Se14 P7 -177(100) . . . . ? Se13 Ni4 Se14 P7 -6.19(5) . . . . ? C57 P8 Se15 Ni4 -112.0(2) . . . . ? C61 P8 Se15 Ni4 121.0(3) . . . . ? Se16 P8 Se15 Ni4 4.18(6) . . . . ? Se14 Ni4 Se15 P8 176.04(6) . . . . ? Se16 Ni4 Se15 P8 -3.82(6) . . . . ? Se13 Ni4 Se15 P8 166(30) . . . . ? C57 P8 Se16 Ni4 112.8(2) . . . . ? C61 P8 Se16 Ni4 -119.8(3) . . . . ? Se15 P8 Se16 Ni4 -4.17(6) . . . . ? Se14 Ni4 Se16 P8 -5(3) . . . . ? Se15 Ni4 Se16 P8 3.81(6) . . . . ? Se13 Ni4 Se16 P8 -176.04(6) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.562 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.162 # Attachment '[Ni_iPr2PSe2_2]s2519abs.cif' data_z:\s2519\work\s2519abs _database_code_depnum_ccdc_archive 'CCDC 692536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Ni P2 Se4' _chemical_formula_weight 608.83 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' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2865(9) _cell_length_b 10.9349(10) _cell_length_c 10.1364(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.904(2) _cell_angle_gamma 90.00 _cell_volume 1019.54(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3486 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 8.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0929 _exptl_absorpt_correction_T_max 0.1045 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5643 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2067 _reflns_number_gt 1933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0217P)^2^+0.4516P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2067 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Se1 Se 0.07909(2) 0.19667(2) 0.07323(2) 0.01232(7) Uani 1 1 d . . . Se2 Se 0.03748(3) -0.06966(2) 0.22209(2) 0.01356(8) Uani 1 1 d . . . Ni1 Ni 0.0000 0.0000 0.0000 0.01018(10) Uani 1 2 d S . . P1 P 0.08459(6) 0.12079(5) 0.27171(5) 0.00992(13) Uani 1 1 d . . . C1 C 0.2609(2) 0.1377(2) 0.3746(2) 0.0118(5) Uani 1 1 d . . . H1 H 0.2759 0.2263 0.3973 0.014 Uiso 1 1 calc R . . C2 C 0.2633(3) 0.0660(2) 0.5043(2) 0.0172(5) Uani 1 1 d . . . H2A H 0.2517 -0.0214 0.4842 0.026 Uiso 1 1 calc R . . H2B H 0.1836 0.0938 0.5509 0.026 Uiso 1 1 calc R . . H2C H 0.3562 0.0797 0.5610 0.026 Uiso 1 1 calc R . . C3 C 0.3836(3) 0.0961(2) 0.2993(2) 0.0181(5) Uani 1 1 d . . . H3A H 0.4769 0.1054 0.3564 0.027 Uiso 1 1 calc R . . H3B H 0.3834 0.1460 0.2190 0.027 Uiso 1 1 calc R . . H3C H 0.3691 0.0100 0.2740 0.027 Uiso 1 1 calc R . . C4 C -0.0539(3) 0.1882(2) 0.3622(2) 0.0142(5) Uani 1 1 d . . . H4 H -0.0545 0.1405 0.4463 0.017 Uiso 1 1 calc R . . C5 C -0.0191(3) 0.3215(2) 0.4009(3) 0.0245(6) Uani 1 1 d . . . H5A H -0.0130 0.3698 0.3204 0.037 Uiso 1 1 calc R . . H5B H 0.0741 0.3253 0.4593 0.037 Uiso 1 1 calc R . . H5C H -0.0960 0.3546 0.4477 0.037 Uiso 1 1 calc R . . C6 C -0.2044(3) 0.1771(2) 0.2816(3) 0.0195(5) Uani 1 1 d . . . H6A H -0.2776 0.2070 0.3348 0.029 Uiso 1 1 calc R . . H6B H -0.2240 0.0912 0.2580 0.029 Uiso 1 1 calc R . . H6C H -0.2083 0.2260 0.2002 0.029 Uiso 1 1 calc R . . 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 Se1 0.01653(13) 0.01215(13) 0.00802(12) 0.00098(8) 0.00074(9) -0.00214(9) Se2 0.02005(14) 0.01120(13) 0.00878(12) -0.00008(8) -0.00035(9) -0.00322(9) Ni1 0.0116(2) 0.0115(2) 0.0072(2) -0.00059(14) 0.00027(15) -0.00113(15) P1 0.0103(3) 0.0114(3) 0.0079(3) -0.0001(2) 0.0006(2) -0.0008(2) C1 0.0116(11) 0.0142(11) 0.0095(11) -0.0001(8) 0.0007(9) -0.0019(9) C2 0.0168(12) 0.0228(13) 0.0104(12) 0.0033(9) -0.0038(9) -0.0028(10) C3 0.0122(11) 0.0212(13) 0.0209(13) -0.0008(10) 0.0023(10) 0.0017(10) C4 0.0139(12) 0.0177(12) 0.0123(11) 0.0012(9) 0.0062(9) 0.0004(9) C5 0.0263(15) 0.0180(13) 0.0321(15) -0.0074(11) 0.0146(12) 0.0004(11) C6 0.0128(12) 0.0250(14) 0.0212(13) 0.0069(10) 0.0045(10) 0.0027(10) _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 Se1 P1 2.1703(6) . ? Se1 Ni1 2.3591(3) . ? Se2 P1 2.1728(6) . ? Se2 Ni1 2.3566(3) . ? Ni1 Se2 2.3566(3) 3 ? Ni1 Se1 2.3591(3) 3 ? P1 C1 1.826(2) . ? P1 C4 1.834(2) . ? C1 C3 1.525(3) . ? C1 C2 1.528(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.523(3) . ? C4 C5 1.533(3) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 P1 Se1 Ni1 84.823(17) . . ? P1 Se2 Ni1 84.830(17) . . ? Se2 Ni1 Se2 180.0 . 3 ? Se2 Ni1 Se1 90.263(9) . 3 ? Se2 Ni1 Se1 89.736(9) 3 3 ? Se2 Ni1 Se1 89.737(9) . . ? Se2 Ni1 Se1 90.264(9) 3 . ? Se1 Ni1 Se1 180.0 3 . ? C1 P1 C4 108.00(11) . . ? C1 P1 Se1 113.31(7) . . ? C4 P1 Se1 112.41(8) . . ? C1 P1 Se2 111.46(8) . . ? C4 P1 Se2 111.60(8) . . ? Se1 P1 Se2 99.99(2) . . ? C3 C1 C2 110.72(19) . . ? C3 C1 P1 110.86(15) . . ? C2 C1 P1 110.18(15) . . ? C3 C1 H1 108.3 . . ? C2 C1 H1 108.3 . . ? P1 C1 H1 108.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 111.0(2) . . ? C6 C4 P1 110.77(17) . . ? C5 C4 P1 111.85(17) . . ? C6 C4 H4 107.7 . . ? C5 C4 H4 107.7 . . ? P1 C4 H4 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Se2 Ni1 Se2 116(2) . . . 3 ? P1 Se2 Ni1 Se1 -174.340(17) . . . 3 ? P1 Se2 Ni1 Se1 5.661(17) . . . . ? P1 Se1 Ni1 Se2 -5.667(17) . . . . ? P1 Se1 Ni1 Se2 174.334(17) . . . 3 ? P1 Se1 Ni1 Se1 -80.1(18) . . . 3 ? Ni1 Se1 P1 C1 124.95(8) . . . . ? Ni1 Se1 P1 C4 -112.25(9) . . . . ? Ni1 Se1 P1 Se2 6.243(19) . . . . ? Ni1 Se2 P1 C1 -126.31(8) . . . . ? Ni1 Se2 P1 C4 112.84(8) . . . . ? Ni1 Se2 P1 Se1 -6.250(18) . . . . ? C4 P1 C1 C3 -173.87(16) . . . . ? Se1 P1 C1 C3 -48.66(18) . . . . ? Se2 P1 C1 C3 63.20(17) . . . . ? C4 P1 C1 C2 63.21(18) . . . . ? Se1 P1 C1 C2 -171.58(14) . . . . ? Se2 P1 C1 C2 -59.72(17) . . . . ? C1 P1 C4 C6 180.00(16) . . . . ? Se1 P1 C4 C6 54.26(18) . . . . ? Se2 P1 C4 C6 -57.16(17) . . . . ? C1 P1 C4 C5 55.6(2) . . . . ? Se1 P1 C4 C5 -70.17(18) . . . . ? Se2 P1 C4 C5 178.41(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.543 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.088