# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Tristram Chivers' 'Mohammad Afzaal' 'Javeed Akhtar' "Paul O'Brien" 'Stuart D. Robertson' _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; Nickel(II) complexes of heterodichalcogenido PNP ligands [(EPiPr2)(TeiPr2)N]- (E = S, Se) and monochalcogenido PNP ligands [(PiPr2)(EiPr2)N]- (E = Se, Te): AACVD synthesis of nickel ditelluride ; # Attachment 'combined_cif_files.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 698665' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 Ni P4 S2 Te2' _chemical_formula_sum 'C24 H56 N2 Ni P4 S2 Te2' _chemical_formula_weight 874.62 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' P P 0.1023 0.0942 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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 8.3894(5) _cell_length_b 9.5766(4) _cell_length_c 12.7480(8) _cell_angle_alpha 106.053(3) _cell_angle_beta 98.788(3) _cell_angle_gamma 110.508(3) _cell_volume 885.72(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30318 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 438 _exptl_absorpt_coefficient_mu 2.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_T_max 0.787 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15755 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3124 _reflns_number_gt 2796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0594P)^2^+0.6786P] 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 3124 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _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 Ni1 Ni 0.0000 0.0000 1.0000 0.01999(18) Uani 1 2 d S . . Te1 Te 0.12940(3) 0.27678(3) 0.99436(2) 0.02494(13) Uani 1 1 d . . . P1 P 0.18623(13) 0.26121(11) 0.81002(9) 0.0198(2) Uani 1 1 d . . . C10 C 0.1532(5) 0.4261(5) 0.7775(4) 0.0242(9) Uani 1 1 d . . . H10A H 0.1835 0.4259 0.7046 0.029 Uiso 1 1 calc R . . C11 C 0.2748(6) 0.5886(5) 0.8686(4) 0.0330(10) Uani 1 1 d . . . H11A H 0.2531 0.6728 0.8477 0.050 Uiso 1 1 calc R . . H11B H 0.3986 0.6059 0.8748 0.050 Uiso 1 1 calc R . . H11C H 0.2505 0.5914 0.9418 0.050 Uiso 1 1 calc R . . C12 C -0.0398(6) 0.3998(5) 0.7592(4) 0.0320(10) Uani 1 1 d . . . H12A H -0.0560 0.4862 0.7385 0.048 Uiso 1 1 calc R . . H12B H -0.0737 0.3988 0.8293 0.048 Uiso 1 1 calc R . . H12C H -0.1142 0.2975 0.6978 0.048 Uiso 1 1 calc R . . C20 C 0.4210(5) 0.3037(5) 0.8250(4) 0.0252(9) Uani 1 1 d . . . H20A H 0.4928 0.4043 0.8918 0.030 Uiso 1 1 calc R . . C21 C 0.4728(6) 0.3294(6) 0.7196(4) 0.0388(11) Uani 1 1 d . . . H21A H 0.5974 0.3479 0.7282 0.058 Uiso 1 1 calc R . . H21B H 0.4560 0.4222 0.7109 0.058 Uiso 1 1 calc R . . H21C H 0.3983 0.2345 0.6523 0.058 Uiso 1 1 calc R . . C22 C 0.4611(6) 0.1689(5) 0.8480(4) 0.0331(10) Uani 1 1 d . . . H22A H 0.5879 0.1953 0.8593 0.050 Uiso 1 1 calc R . . H22B H 0.3929 0.0692 0.7830 0.050 Uiso 1 1 calc R . . H22C H 0.4282 0.1560 0.9163 0.050 Uiso 1 1 calc R . . S1 S 0.02470(13) -0.13593(11) 0.83459(8) 0.0225(2) Uani 1 1 d . . . N1 N 0.0653(4) 0.0994(4) 0.7030(3) 0.0228(7) Uani 1 1 d . . . P2 P -0.06369(13) -0.06641(12) 0.70811(8) 0.0199(2) Uani 1 1 d . . . C30 C -0.2789(5) -0.0589(5) 0.7120(4) 0.0244(9) Uani 1 1 d . . . H30A H -0.2509 0.0453 0.7724 0.029 Uiso 1 1 calc R . . C31 C -0.3679(6) -0.0498(6) 0.6013(4) 0.0325(10) Uani 1 1 d . . . H31A H -0.4569 -0.0075 0.6143 0.049 Uiso 1 1 calc R . . H31B H -0.4254 -0.1567 0.5427 0.049 Uiso 1 1 calc R . . H31C H -0.2785 0.0208 0.5762 0.049 Uiso 1 1 calc R . . C32 C -0.4068(6) -0.1857(6) 0.7453(4) 0.0344(10) Uani 1 1 d . . . H32A H -0.5068 -0.1590 0.7575 0.052 Uiso 1 1 calc R . . H32B H -0.3453 -0.1899 0.8154 0.052 Uiso 1 1 calc R . . H32C H -0.4507 -0.2898 0.6843 0.052 Uiso 1 1 calc R . . C40 C -0.0868(5) -0.2168(5) 0.5748(3) 0.0249(9) Uani 1 1 d . . . H40A H -0.1187 -0.1793 0.5121 0.030 Uiso 1 1 calc R . . C41 C 0.0919(6) -0.2267(6) 0.5733(4) 0.0381(11) Uani 1 1 d . . . H41A H 0.0802 -0.3024 0.4998 0.057 Uiso 1 1 calc R . . H41B H 0.1277 -0.2630 0.6341 0.057 Uiso 1 1 calc R . . H41C H 0.1818 -0.1211 0.5853 0.057 Uiso 1 1 calc R . . C42 C -0.2337(6) -0.3814(5) 0.5496(4) 0.0356(10) Uani 1 1 d . . . H42A H -0.2308 -0.4583 0.4815 0.053 Uiso 1 1 calc R . . H42B H -0.3489 -0.3754 0.5367 0.053 Uiso 1 1 calc R . . H42C H -0.2153 -0.4158 0.6143 0.053 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 Ni1 0.0228(4) 0.0190(4) 0.0187(4) 0.0059(3) 0.0075(3) 0.0092(3) Te1 0.03215(19) 0.01986(18) 0.02206(18) 0.00642(12) 0.01110(12) 0.00925(13) P1 0.0183(5) 0.0189(5) 0.0216(6) 0.0064(4) 0.0070(4) 0.0073(4) C10 0.026(2) 0.024(2) 0.025(2) 0.0095(18) 0.0118(17) 0.0103(17) C11 0.033(2) 0.023(2) 0.042(3) 0.011(2) 0.011(2) 0.0099(19) C12 0.030(2) 0.033(2) 0.039(3) 0.015(2) 0.0087(19) 0.019(2) C20 0.0153(19) 0.028(2) 0.027(2) 0.0036(18) 0.0059(16) 0.0076(16) C21 0.029(2) 0.053(3) 0.042(3) 0.019(2) 0.021(2) 0.019(2) C22 0.022(2) 0.033(2) 0.041(3) 0.008(2) 0.0049(19) 0.0136(19) S1 0.0288(5) 0.0226(5) 0.0186(5) 0.0072(4) 0.0082(4) 0.0130(4) N1 0.0258(17) 0.0231(17) 0.0185(17) 0.0066(14) 0.0074(14) 0.0091(14) P2 0.0198(5) 0.0194(5) 0.0194(5) 0.0053(4) 0.0064(4) 0.0078(4) C30 0.019(2) 0.027(2) 0.026(2) 0.0061(18) 0.0083(16) 0.0110(17) C31 0.028(2) 0.041(3) 0.034(3) 0.017(2) 0.0085(19) 0.016(2) C32 0.026(2) 0.038(3) 0.043(3) 0.018(2) 0.012(2) 0.012(2) C40 0.028(2) 0.024(2) 0.021(2) 0.0077(17) 0.0073(16) 0.0093(17) C41 0.038(3) 0.041(3) 0.031(3) 0.002(2) 0.015(2) 0.018(2) C42 0.041(3) 0.026(2) 0.030(3) 0.002(2) 0.007(2) 0.010(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 Ni1 S1 2.2335(12) 2_557 ? Ni1 S1 2.2335(12) . ? Ni1 Te1 2.5145(8) . ? Ni1 Te1 2.5145(8) 2_557 ? Te1 P1 2.4434(11) . ? P1 N1 1.612(4) . ? P1 C20 1.833(4) . ? P1 C10 1.837(4) . ? C10 C12 1.518(6) . ? C10 C11 1.529(6) . ? C20 C21 1.529(6) . ? C20 C22 1.533(6) . ? S1 P2 2.0413(15) . ? N1 P2 1.603(3) . ? P2 C40 1.830(4) . ? P2 C30 1.839(4) . ? C30 C32 1.523(6) . ? C30 C31 1.532(6) . ? C40 C42 1.531(6) . ? C40 C41 1.538(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S1 180.0 2_557 . ? S1 Ni1 Te1 80.78(4) 2_557 . ? S1 Ni1 Te1 99.22(4) . . ? S1 Ni1 Te1 99.22(4) 2_557 2_557 ? S1 Ni1 Te1 80.78(4) . 2_557 ? Te1 Ni1 Te1 180.0 . 2_557 ? P1 Te1 Ni1 109.19(4) . . ? N1 P1 C20 109.77(19) . . ? N1 P1 C10 107.56(18) . . ? C20 P1 C10 106.14(19) . . ? N1 P1 Te1 117.69(13) . . ? C20 P1 Te1 108.63(14) . . ? C10 P1 Te1 106.41(14) . . ? C12 C10 C11 111.1(4) . . ? C12 C10 P1 110.6(3) . . ? C11 C10 P1 112.3(3) . . ? C21 C20 C22 111.2(4) . . ? C21 C20 P1 110.9(3) . . ? C22 C20 P1 110.3(3) . . ? P2 S1 Ni1 110.72(5) . . ? P2 N1 P1 126.3(2) . . ? N1 P2 C40 104.47(18) . . ? N1 P2 C30 108.00(18) . . ? C40 P2 C30 110.10(19) . . ? N1 P2 S1 117.25(14) . . ? C40 P2 S1 105.93(14) . . ? C30 P2 S1 110.77(14) . . ? C32 C30 C31 111.5(3) . . ? C32 C30 P2 116.8(3) . . ? C31 C30 P2 110.9(3) . . ? C42 C40 C41 111.2(4) . . ? C42 C40 P2 113.8(3) . . ? C41 C40 P2 110.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.167 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.155 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 698666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 Ni P4 Se2 Te2' _chemical_formula_sum 'C24 H56 N2 Ni P4 Se2 Te2' _chemical_formula_weight 968.42 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' 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' Te Te -0.5308 1.6751 '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 9.7452(5) _cell_length_b 9.7701(5) _cell_length_c 9.9532(6) _cell_angle_alpha 82.164(3) _cell_angle_beta 89.853(3) _cell_angle_gamma 76.153(3) _cell_volume 911.08(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14165 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 474 _exptl_absorpt_coefficient_mu 4.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9506 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3075 _reflns_number_gt 2737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0236P)^2^+1.6628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 3075 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.01982(15) Uani 1 2 d S . . Te1 Te 0.32687(3) 0.44839(3) 0.33990(3) 0.02712(10) Uani 1 1 d . . . P1 P 0.19026(10) 0.66957(11) 0.21195(10) 0.0233(2) Uani 1 1 d . . . C10 C 0.2461(5) 0.6778(5) 0.0352(4) 0.0344(10) Uani 1 1 d . . . H10A H 0.1857 0.7662 -0.0172 0.041 Uiso 1 1 calc R . . C11 C 0.2232(6) 0.5504(5) -0.0290(5) 0.0478(12) Uani 1 1 d . . . H11A H 0.2637 0.5517 -0.1192 0.072 Uiso 1 1 calc R . . H11B H 0.1216 0.5564 -0.0371 0.072 Uiso 1 1 calc R . . H11C H 0.2695 0.4617 0.0285 0.072 Uiso 1 1 calc R . . C12 C 0.3993(5) 0.6886(5) 0.0255(5) 0.0421(11) Uani 1 1 d . . . H12A H 0.4250 0.6984 -0.0700 0.063 Uiso 1 1 calc R . . H12B H 0.4612 0.6024 0.0750 0.063 Uiso 1 1 calc R . . H12C H 0.4103 0.7719 0.0652 0.063 Uiso 1 1 calc R . . C20 C 0.0057(4) 0.6561(5) 0.2047(4) 0.0328(10) Uani 1 1 d . . . H20A H 0.0048 0.5638 0.1724 0.039 Uiso 1 1 calc R . . C21 C -0.0846(5) 0.7762(6) 0.1042(5) 0.0497(13) Uani 1 1 d . . . H21A H -0.1832 0.7689 0.1065 0.075 Uiso 1 1 calc R . . H21B H -0.0496 0.7683 0.0125 0.075 Uiso 1 1 calc R . . H21C H -0.0789 0.8683 0.1293 0.075 Uiso 1 1 calc R . . C22 C -0.0578(5) 0.6547(6) 0.3436(5) 0.0511(13) Uani 1 1 d . . . H22A H -0.1540 0.6414 0.3376 0.077 Uiso 1 1 calc R . . H22B H -0.0607 0.7454 0.3766 0.077 Uiso 1 1 calc R . . H22C H 0.0002 0.5765 0.4065 0.077 Uiso 1 1 calc R . . Se1 Se 0.48655(4) 0.27296(4) 0.60651(4) 0.02372(11) Uani 1 1 d . . . N1 N 0.8105(3) 0.1860(3) 0.7292(3) 0.0244(7) Uani 1 1 d . . . P2 P 0.70554(10) 0.14338(10) 0.62876(10) 0.0215(2) Uani 1 1 d . . . C30 C 0.7826(4) 0.1335(4) 0.4603(4) 0.0284(9) Uani 1 1 d . . . H30A H 0.8804 0.0710 0.4746 0.034 Uiso 1 1 calc R . . C31 C 0.7964(4) 0.2771(5) 0.3912(4) 0.0345(10) Uani 1 1 d . . . H31A H 0.8510 0.2648 0.3090 0.052 Uiso 1 1 calc R . . H31B H 0.8451 0.3211 0.4530 0.052 Uiso 1 1 calc R . . H31C H 0.7022 0.3384 0.3667 0.052 Uiso 1 1 calc R . . C32 C 0.7022(5) 0.0657(5) 0.3662(5) 0.0446(12) Uani 1 1 d . . . H32A H 0.7508 0.0586 0.2802 0.067 Uiso 1 1 calc R . . H32B H 0.6057 0.1247 0.3489 0.067 Uiso 1 1 calc R . . H32C H 0.6987 -0.0297 0.4094 0.067 Uiso 1 1 calc R . . C40 C 0.6968(4) -0.0380(4) 0.6943(4) 0.0265(8) Uani 1 1 d . . . H40A H 0.6383 -0.0709 0.6288 0.032 Uiso 1 1 calc R . . C41 C 0.6272(5) -0.0449(5) 0.8315(4) 0.0357(10) Uani 1 1 d . . . H41A H 0.6194 -0.1424 0.8614 0.054 Uiso 1 1 calc R . . H41B H 0.5327 0.0196 0.8232 0.054 Uiso 1 1 calc R . . H41C H 0.6848 -0.0162 0.8980 0.054 Uiso 1 1 calc R . . C42 C 0.8454(4) -0.1368(4) 0.7037(5) 0.0342(10) Uani 1 1 d . . . H42A H 0.8414 -0.2319 0.7474 0.051 Uiso 1 1 calc R . . H42B H 0.9081 -0.0988 0.7574 0.051 Uiso 1 1 calc R . . H42C H 0.8819 -0.1430 0.6123 0.051 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 Ni1 0.0176(3) 0.0162(3) 0.0246(3) -0.0012(3) -0.0014(3) -0.0030(3) Te1 0.02798(15) 0.02152(15) 0.03174(16) -0.00267(11) -0.00633(11) -0.00621(11) P1 0.0243(5) 0.0230(5) 0.0229(5) 0.0001(4) -0.0032(4) -0.0081(4) C10 0.045(3) 0.034(2) 0.025(2) -0.0006(18) 0.0005(18) -0.013(2) C11 0.062(3) 0.054(3) 0.033(2) -0.014(2) 0.000(2) -0.020(3) C12 0.051(3) 0.047(3) 0.034(2) -0.012(2) 0.018(2) -0.019(2) C20 0.027(2) 0.031(2) 0.042(2) 0.0003(19) -0.0111(18) -0.0117(18) C21 0.035(3) 0.060(3) 0.047(3) 0.008(2) -0.017(2) -0.008(2) C22 0.027(2) 0.072(4) 0.049(3) 0.014(3) 0.000(2) -0.016(2) Se1 0.01789(19) 0.0181(2) 0.0329(2) 0.00125(16) -0.00143(15) -0.00270(15) N1 0.0241(16) 0.0200(16) 0.0279(17) -0.0001(13) -0.0063(13) -0.0047(13) P2 0.0184(5) 0.0186(5) 0.0264(5) -0.0012(4) -0.0022(4) -0.0035(4) C30 0.025(2) 0.028(2) 0.029(2) -0.0039(17) 0.0003(16) 0.0012(16) C31 0.029(2) 0.039(2) 0.030(2) 0.0043(18) 0.0066(17) -0.0026(19) C32 0.051(3) 0.050(3) 0.037(3) -0.018(2) -0.001(2) -0.014(2) C40 0.027(2) 0.0167(19) 0.036(2) -0.0011(16) -0.0065(16) -0.0072(16) C41 0.037(2) 0.027(2) 0.040(2) 0.0081(18) -0.0004(19) -0.0098(19) C42 0.034(2) 0.021(2) 0.046(3) -0.0004(18) -0.0048(19) -0.0041(17) _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 Ni1 Se1 2.3577(8) 2_666 ? Ni1 Se1 2.3577(8) . ? Ni1 Te1 2.5060(7) . ? Ni1 Te1 2.5060(7) 2_666 ? Te1 P1 2.4383(14) . ? P1 N1 1.598(3) 2_666 ? P1 C10 1.837(4) . ? P1 C20 1.837(4) . ? C10 C12 1.524(6) . ? C10 C11 1.535(6) . ? C20 C22 1.512(6) . ? C20 C21 1.530(6) . ? Se1 P2 2.1997(12) . ? N1 P2 1.595(3) . ? N1 P1 1.598(3) 2_666 ? P2 C40 1.825(4) . ? P2 C30 1.840(4) . ? C30 C31 1.512(6) . ? C30 C32 1.534(6) . ? C40 C41 1.524(6) . ? C40 C42 1.531(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 Se1 Ni1 Se1 180.000(8) 2_666 . ? Se1 Ni1 Te1 99.42(3) 2_666 . ? Se1 Ni1 Te1 80.58(3) . . ? Se1 Ni1 Te1 80.58(3) 2_666 2_666 ? Se1 Ni1 Te1 99.42(3) . 2_666 ? Te1 Ni1 Te1 180.000(1) . 2_666 ? P1 Te1 Ni1 110.13(3) . . ? N1 P1 C10 111.34(18) 2_666 . ? N1 P1 C20 106.78(19) 2_666 . ? C10 P1 C20 105.0(2) . . ? N1 P1 Te1 117.29(12) 2_666 . ? C10 P1 Te1 108.45(15) . . ? C20 P1 Te1 107.16(14) . . ? C12 C10 C11 111.2(4) . . ? C12 C10 P1 110.9(3) . . ? C11 C10 P1 111.4(3) . . ? C22 C20 C21 110.3(4) . . ? C22 C20 P1 111.3(3) . . ? C21 C20 P1 111.6(3) . . ? P2 Se1 Ni1 105.96(4) . . ? P2 N1 P1 132.9(2) . 2_666 ? N1 P2 C40 106.33(17) . . ? N1 P2 C30 110.09(18) . . ? C40 P2 C30 105.63(19) . . ? N1 P2 Se1 117.63(13) . . ? C40 P2 Se1 106.86(13) . . ? C30 P2 Se1 109.55(13) . . ? C31 C30 C32 110.0(4) . . ? C31 C30 P2 112.3(3) . . ? C32 C30 P2 113.2(3) . . ? C41 C40 C42 110.9(3) . . ? C41 C40 P2 111.5(3) . . ? C42 C40 P2 109.8(3) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.510 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.109 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 698667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 Ni P4 Se2' _chemical_formula_sum 'C24 H56 N2 Ni P4 Se2' _chemical_formula_weight 713.22 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' 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 8.9748(2) _cell_length_b 19.7569(4) _cell_length_c 9.3534(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.61(3) _cell_angle_gamma 90.00 _cell_volume 1604.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20328 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 3.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25896 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.42 _reflns_number_total 3644 _reflns_number_gt 3339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0443P)^2^+0.5052P] 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 3644 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Ni1 Ni 0.5000 0.0000 1.0000 0.01770(9) Uani 1 2 d S . . Se1 Se 0.60228(2) 0.063793(9) 0.84158(2) 0.02395(8) Uani 1 1 d . . . P1 P 0.65686(5) 0.15668(2) 0.97651(5) 0.01959(11) Uani 1 1 d . . . C10 C 0.5181(2) 0.22284(10) 0.8925(2) 0.0276(4) Uani 1 1 d . . . H10A H 0.5317 0.2321 0.7914 0.033 Uiso 1 1 calc R . . C11 C 0.3520(3) 0.20026(13) 0.8754(3) 0.0495(7) Uani 1 1 d . . . H11A H 0.2819 0.2355 0.8239 0.074 Uiso 1 1 calc R . . H11B H 0.3341 0.1925 0.9732 0.074 Uiso 1 1 calc R . . H11C H 0.3333 0.1582 0.8179 0.074 Uiso 1 1 calc R . . C12 C 0.5490(3) 0.28900(11) 0.9806(3) 0.0419(5) Uani 1 1 d . . . H12A H 0.4667 0.3215 0.9399 0.063 Uiso 1 1 calc R . . H12B H 0.6480 0.3079 0.9737 0.063 Uiso 1 1 calc R . . H12C H 0.5522 0.2800 1.0843 0.063 Uiso 1 1 calc R . . C20 C 0.8420(2) 0.19109(10) 0.9592(2) 0.0270(4) Uani 1 1 d . . . H20A H 0.8507 0.2382 0.9995 0.032 Uiso 1 1 calc R . . C21 C 0.9777(2) 0.15123(13) 1.0501(3) 0.0388(5) Uani 1 1 d . . . H21A H 1.0738 0.1744 1.0484 0.058 Uiso 1 1 calc R . . H21B H 0.9777 0.1057 1.0083 0.058 Uiso 1 1 calc R . . H21C H 0.9692 0.1478 1.1522 0.058 Uiso 1 1 calc R . . C22 C 0.8501(3) 0.19582(13) 0.7986(3) 0.0399(5) Uani 1 1 d . . . H22A H 0.9474 0.2172 0.7940 0.060 Uiso 1 1 calc R . . H22B H 0.7637 0.2230 0.7424 0.060 Uiso 1 1 calc R . . H22C H 0.8444 0.1503 0.7560 0.060 Uiso 1 1 calc R . . N1 N 0.65991(18) 0.14215(8) 1.14447(17) 0.0224(3) Uani 1 1 d . . . P2 P 0.61246(5) 0.06601(2) 1.19139(5) 0.01850(11) Uani 1 1 d . . . C30 C 0.5031(2) 0.08398(10) 1.3303(2) 0.0245(4) Uani 1 1 d . . . H30A H 0.4913 0.0406 1.3814 0.029 Uiso 1 1 calc R . . C31 C 0.3425(3) 0.11007(11) 1.2547(3) 0.0341(5) Uani 1 1 d . . . H31A H 0.2841 0.1174 1.3289 0.051 Uiso 1 1 calc R . . H31B H 0.2891 0.0767 1.1822 0.051 Uiso 1 1 calc R . . H31C H 0.3513 0.1529 1.2045 0.051 Uiso 1 1 calc R . . C32 C 0.5875(3) 0.13423(11) 1.4469(2) 0.0331(5) Uani 1 1 d . . . H32A H 0.5284 0.1411 1.5206 0.050 Uiso 1 1 calc R . . H32B H 0.5988 0.1775 1.3994 0.050 Uiso 1 1 calc R . . H32C H 0.6896 0.1163 1.4954 0.050 Uiso 1 1 calc R . . C40 C 0.7935(2) 0.02643(9) 1.3025(2) 0.0251(4) Uani 1 1 d . . . H40A H 0.8628 0.0641 1.3503 0.030 Uiso 1 1 calc R . . C41 C 0.7741(3) -0.02097(11) 1.4265(2) 0.0351(5) Uani 1 1 d . . . H41A H 0.8736 -0.0415 1.4743 0.053 Uiso 1 1 calc R . . H41B H 0.6999 -0.0566 1.3848 0.053 Uiso 1 1 calc R . . H41C H 0.7364 0.0050 1.4996 0.053 Uiso 1 1 calc R . . C42 C 0.8756(3) -0.01071(12) 1.2006(3) 0.0364(5) Uani 1 1 d . . . H42A H 0.9801 -0.0229 1.2562 0.055 Uiso 1 1 calc R . . H42B H 0.8811 0.0188 1.1179 0.055 Uiso 1 1 calc R . . H42C H 0.8183 -0.0519 1.1625 0.055 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 Ni1 0.01900(16) 0.01534(16) 0.01697(17) 0.00009(11) 0.00122(12) -0.00333(11) Se1 0.03114(12) 0.02078(12) 0.01970(12) -0.00179(7) 0.00599(8) -0.00841(7) P1 0.0207(2) 0.0168(2) 0.0200(2) 0.00077(17) 0.00282(17) -0.00277(16) C10 0.0328(10) 0.0239(9) 0.0251(10) 0.0066(8) 0.0056(8) 0.0041(8) C11 0.0256(11) 0.0440(14) 0.0709(19) 0.0133(13) -0.0031(11) 0.0070(10) C12 0.0488(14) 0.0279(11) 0.0500(14) -0.0019(10) 0.0140(11) 0.0086(10) C20 0.0244(9) 0.0244(9) 0.0326(11) -0.0047(8) 0.0080(8) -0.0078(7) C21 0.0239(10) 0.0507(14) 0.0412(13) -0.0004(11) 0.0069(9) -0.0027(9) C22 0.0409(12) 0.0447(13) 0.0370(13) 0.0024(10) 0.0150(10) -0.0164(10) N1 0.0269(8) 0.0189(7) 0.0198(8) -0.0013(6) 0.0028(6) -0.0047(6) P2 0.0191(2) 0.0169(2) 0.0173(2) 0.00050(16) 0.00038(18) -0.00168(16) C30 0.0297(10) 0.0235(9) 0.0201(9) 0.0008(7) 0.0059(7) -0.0022(8) C31 0.0326(11) 0.0331(11) 0.0370(12) -0.0024(9) 0.0097(9) 0.0073(9) C32 0.0454(13) 0.0331(11) 0.0215(10) -0.0050(8) 0.0093(9) -0.0059(9) C40 0.0214(9) 0.0215(9) 0.0275(10) 0.0011(7) -0.0030(7) -0.0015(7) C41 0.0330(11) 0.0316(11) 0.0330(11) 0.0103(9) -0.0060(9) -0.0009(9) C42 0.0292(11) 0.0326(11) 0.0438(13) 0.0005(10) 0.0026(9) 0.0099(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 Ni1 P2 2.2388(7) 3_657 ? Ni1 P2 2.2388(7) . ? Ni1 Se1 2.3051(5) 3_657 ? Ni1 Se1 2.3051(4) . ? Se1 P1 2.2109(6) . ? P1 N1 1.5905(17) . ? P1 C10 1.839(2) . ? P1 C20 1.8402(19) . ? C10 C11 1.526(3) . ? C10 C12 1.533(3) . ? C20 C21 1.518(3) . ? C20 C22 1.525(3) . ? N1 P2 1.6527(16) . ? P2 C30 1.850(2) . ? P2 C40 1.866(2) . ? C30 C31 1.526(3) . ? C30 C32 1.527(3) . ? C40 C42 1.531(3) . ? C40 C41 1.534(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 P2 Ni1 P2 180.0 3_657 . ? P2 Ni1 Se1 91.329(19) 3_657 3_657 ? P2 Ni1 Se1 88.67(2) . 3_657 ? P2 Ni1 Se1 88.671(19) 3_657 . ? P2 Ni1 Se1 91.329(19) . . ? Se1 Ni1 Se1 180.0 3_657 . ? P1 Se1 Ni1 98.84(2) . . ? N1 P1 C10 113.04(9) . . ? N1 P1 C20 111.28(9) . . ? C10 P1 C20 103.22(9) . . ? N1 P1 Se1 111.11(6) . . ? C10 P1 Se1 108.51(7) . . ? C20 P1 Se1 109.35(7) . . ? C11 C10 C12 110.2(2) . . ? C11 C10 P1 112.05(15) . . ? C12 C10 P1 111.44(16) . . ? C21 C20 C22 110.66(19) . . ? C21 C20 P1 111.93(15) . . ? C22 C20 P1 112.21(14) . . ? P1 N1 P2 119.02(10) . . ? N1 P2 C30 103.29(9) . . ? N1 P2 C40 106.44(9) . . ? C30 P2 C40 103.35(9) . . ? N1 P2 Ni1 114.35(6) . . ? C30 P2 Ni1 117.48(7) . . ? C40 P2 Ni1 110.79(7) . . ? C31 C30 C32 110.59(18) . . ? C31 C30 P2 110.22(14) . . ? C32 C30 P2 111.75(14) . . ? C42 C40 C41 110.03(17) . . ? C42 C40 P2 110.02(14) . . ? C41 C40 P2 115.33(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.550 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.112 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 698668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 Ni P4 Te2' _chemical_formula_sum 'C24 H56 N2 Ni P4 Te2' _chemical_formula_weight 810.50 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' 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' Te Te -0.5308 1.6751 '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 8.8985(4) _cell_length_b 10.3031(4) _cell_length_c 10.6062(6) _cell_angle_alpha 107.612(2) _cell_angle_beta 110.266(2) _cell_angle_gamma 97.466(3) _cell_volume 838.95(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 406 _exptl_absorpt_coefficient_mu 2.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12947 _diffrn_reflns_av_R_equivalents 0.1309 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2968 _reflns_number_gt 2310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0278P)^2^+3.2173P] 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 2968 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _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 Ni1 Ni 0.5000 1.0000 0.0000 0.0163(3) Uani 1 2 d S . . Te1 Te 0.37366(5) 0.80116(5) 0.04938(4) 0.02547(16) Uani 1 1 d . . . P1 P 0.26049(19) 0.63556(17) -0.20164(16) 0.0203(4) Uani 1 1 d . . . C10 C 0.3821(9) 0.5064(8) -0.2192(8) 0.0349(17) Uani 1 1 d . . . H10A H 0.3603 0.4447 -0.1672 0.042 Uiso 1 1 calc R . . C11 C 0.3247(13) 0.4124(9) -0.3788(9) 0.062(3) Uani 1 1 d . . . H11A H 0.3879 0.3414 -0.3866 0.094 Uiso 1 1 calc R . . H11B H 0.3434 0.4705 -0.4328 0.094 Uiso 1 1 calc R . . H11C H 0.2062 0.3652 -0.4191 0.094 Uiso 1 1 calc R . . C12 C 0.5671(11) 0.5750(10) -0.1510(11) 0.059(3) Uani 1 1 d . . . H12A H 0.6272 0.5018 -0.1584 0.088 Uiso 1 1 calc R . . H12B H 0.6013 0.6335 -0.0487 0.088 Uiso 1 1 calc R . . H12C H 0.5925 0.6342 -0.2018 0.088 Uiso 1 1 calc R . . C20 C 0.0502(8) 0.5309(7) -0.2531(7) 0.0314(16) Uani 1 1 d . . . H20A H 0.0088 0.4657 -0.3565 0.038 Uiso 1 1 calc R . . C21 C 0.0466(9) 0.4405(8) -0.1638(8) 0.043(2) Uani 1 1 d . . . H21A H -0.0684 0.3901 -0.1926 0.064 Uiso 1 1 calc R . . H21B H 0.0946 0.5010 -0.0608 0.064 Uiso 1 1 calc R . . H21C H 0.1114 0.3722 -0.1806 0.064 Uiso 1 1 calc R . . C22 C -0.0665(8) 0.6258(10) -0.2449(9) 0.055(2) Uani 1 1 d . . . H22A H -0.1811 0.5675 -0.2884 0.082 Uiso 1 1 calc R . . H22B H -0.0564 0.6874 -0.2977 0.082 Uiso 1 1 calc R . . H22C H -0.0372 0.6835 -0.1433 0.082 Uiso 1 1 calc R . . N1 N 0.2596(6) 0.7203(6) -0.3031(5) 0.0227(12) Uani 1 1 d . . . P2 P 0.34153(19) 0.89197(17) -0.23945(16) 0.0179(3) Uani 1 1 d . . . C30 C 0.1621(7) 0.9687(7) -0.2905(7) 0.0263(15) Uani 1 1 d . . . H30A H 0.0692 0.8916 -0.3747 0.032 Uiso 1 1 calc R . . C31 C 0.1866(9) 1.0930(8) -0.3384(7) 0.0377(18) Uani 1 1 d . . . H31A H 0.0850 1.1252 -0.3617 0.057 Uiso 1 1 calc R . . H31B H 0.2112 1.0629 -0.4244 0.057 Uiso 1 1 calc R . . H31C H 0.2792 1.1704 -0.2599 0.057 Uiso 1 1 calc R . . C32 C 0.1021(9) 1.0115(9) -0.1681(8) 0.044(2) Uani 1 1 d . . . H32A H -0.0043 1.0346 -0.2038 0.066 Uiso 1 1 calc R . . H32B H 0.1843 1.0941 -0.0868 0.066 Uiso 1 1 calc R . . H32C H 0.0879 0.9330 -0.1355 0.066 Uiso 1 1 calc R . . C40 C 0.4386(8) 0.9062(7) -0.3654(6) 0.0254(15) Uani 1 1 d . . . H40A H 0.4665 1.0075 -0.3539 0.031 Uiso 1 1 calc R . . C41 C 0.6000(9) 0.8598(8) -0.3276(8) 0.0386(18) Uani 1 1 d . . . H41A H 0.6561 0.8781 -0.3877 0.058 Uiso 1 1 calc R . . H41B H 0.5745 0.7587 -0.3458 0.058 Uiso 1 1 calc R . . H41C H 0.6726 0.9130 -0.2251 0.058 Uiso 1 1 calc R . . C42 C 0.3195(9) 0.8193(8) -0.5238(7) 0.0364(17) Uani 1 1 d . . . H42A H 0.3740 0.8298 -0.5875 0.055 Uiso 1 1 calc R . . H42B H 0.2191 0.8530 -0.5478 0.055 Uiso 1 1 calc R . . H42C H 0.2894 0.7196 -0.5373 0.055 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 Ni1 0.0160(5) 0.0141(6) 0.0140(5) 0.0028(5) 0.0034(4) 0.0016(4) Te1 0.0316(3) 0.0201(3) 0.0166(2) 0.00397(18) 0.00642(18) -0.00252(18) P1 0.0231(8) 0.0158(9) 0.0182(8) 0.0026(7) 0.0090(7) 0.0007(7) C10 0.053(5) 0.027(4) 0.044(4) 0.019(4) 0.035(4) 0.018(4) C11 0.119(8) 0.032(5) 0.050(5) 0.006(4) 0.054(6) 0.027(5) C12 0.065(6) 0.064(7) 0.098(7) 0.055(6) 0.059(6) 0.046(5) C20 0.032(4) 0.024(4) 0.023(3) -0.004(3) 0.012(3) -0.014(3) C21 0.047(5) 0.040(5) 0.032(4) 0.006(4) 0.019(4) -0.010(4) C22 0.017(4) 0.073(7) 0.064(6) 0.028(5) 0.009(4) -0.006(4) N1 0.028(3) 0.019(3) 0.016(3) 0.002(2) 0.007(2) 0.004(2) P2 0.0190(8) 0.0168(9) 0.0139(7) 0.0039(7) 0.0041(6) 0.0039(6) C30 0.018(3) 0.028(4) 0.023(3) 0.010(3) -0.004(3) 0.005(3) C31 0.040(4) 0.032(5) 0.027(4) 0.011(3) -0.003(3) 0.013(3) C32 0.031(4) 0.046(5) 0.052(5) 0.016(4) 0.011(4) 0.023(4) C40 0.036(4) 0.018(4) 0.016(3) 0.001(3) 0.010(3) -0.001(3) C41 0.041(4) 0.042(5) 0.037(4) 0.012(4) 0.024(4) 0.011(4) C42 0.046(4) 0.039(5) 0.022(3) 0.013(3) 0.013(3) 0.001(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 Ni1 P2 2.2534(19) . ? Ni1 P2 2.2534(19) 2_675 ? Ni1 Te1 2.4888(8) 2_675 ? Ni1 Te1 2.4888(8) . ? Te1 P1 2.441(2) . ? P1 N1 1.577(5) . ? P1 C10 1.828(7) . ? P1 C20 1.837(6) . ? C10 C12 1.516(11) . ? C10 C11 1.531(10) . ? C20 C21 1.521(10) . ? C20 C22 1.522(11) . ? N1 P2 1.648(5) . ? P2 C40 1.854(6) . ? P2 C30 1.859(6) . ? C30 C31 1.531(9) . ? C30 C32 1.536(9) . ? C40 C41 1.532(9) . ? C40 C42 1.535(9) . ? 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 P2 Ni1 P2 180.000(1) . 2_675 ? P2 Ni1 Te1 88.63(5) . 2_675 ? P2 Ni1 Te1 91.37(5) 2_675 2_675 ? P2 Ni1 Te1 91.37(5) . . ? P2 Ni1 Te1 88.63(5) 2_675 . ? Te1 Ni1 Te1 180.000(16) 2_675 . ? P1 Te1 Ni1 94.55(5) . . ? N1 P1 C10 111.9(3) . . ? N1 P1 C20 110.9(3) . . ? C10 P1 C20 104.8(3) . . ? N1 P1 Te1 109.1(2) . . ? C10 P1 Te1 109.7(2) . . ? C20 P1 Te1 110.3(2) . . ? C12 C10 C11 110.9(6) . . ? C12 C10 P1 112.4(5) . . ? C11 C10 P1 110.2(5) . . ? C21 C20 C22 111.0(6) . . ? C21 C20 P1 112.7(5) . . ? C22 C20 P1 110.6(5) . . ? P1 N1 P2 122.6(3) . . ? N1 P2 C40 101.2(3) . . ? N1 P2 C30 105.1(3) . . ? C40 P2 C30 104.0(3) . . ? N1 P2 Ni1 117.67(18) . . ? C40 P2 Ni1 117.6(2) . . ? C30 P2 Ni1 109.8(2) . . ? C31 C30 C32 108.9(6) . . ? C31 C30 P2 116.6(5) . . ? C32 C30 P2 111.0(4) . . ? C41 C40 C42 110.4(6) . . ? C41 C40 P2 110.5(4) . . ? C42 C40 P2 111.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.737 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.201 #===END