data_global _publ_contact_author_email CBIANCHINI@ICCOM.CNR.IT _publ_contact_author_name 'Dr Claudio Bianchini' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; ICCOM CNR Area di Ricerca CNR di Firenze Via Madonna del Piano Sesto Fiorentino Firenze 50019 ITALY ; _publ_section_title ; Schulz-Flory oligomerisation of ethylene by the binuclear nickel(II) complex Ni2Cl4[cis, trans, cis-1,2,3,4-tetrakis-(diphenylphosphino)cyclobutane] ; loop_ _publ_author_name '' 'Claudio Bianchini' 'Peter Bruggeller' 'Luca Gonsalvi' 'Rene Gutmann' 'Werner Oberhauser' ; D.Semeril ; data_david _database_code_CSD 215914 _audit_creation_date 2003-09-01T10:20:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H28 Cl2 Ni1 P2' _chemical_formula_sum 'C31.50 H32 Cl2 Ni P2' _chemical_formula_weight 602.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 8.495(5) _cell_length_b 16.8561(15) _cell_length_c 20.561(6) _cell_angle_alpha 90 _cell_angle_beta 94.34(4) _cell_angle_gamma 90 _cell_volume 2936(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown-reddish _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_factor_muR 0.145 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.8643 _exptl_absorpt_correction_T_ave 0.8361 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.02841 _diffrn_orient_matrix_ub_12 -0.002569 _diffrn_orient_matrix_ub_13 0.04628 _diffrn_orient_matrix_ub_21 -0.008219 _diffrn_orient_matrix_ub_22 0.059174 _diffrn_orient_matrix_ub_23 0.001116 _diffrn_orient_matrix_ub_31 -0.114193 _diffrn_orient_matrix_ub_32 -0.003739 _diffrn_orient_matrix_ub_33 -0.015368 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.039 _diffrn_standards_decay_corr_min 0.979 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 -7 -2 2 5 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_number 5303 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 5155 _reflns_number_gt 4019 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0613P)^2^+2.1897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5155 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 0.94 _refine_ls_restrained_S_all 0.94 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 0.382 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 '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' 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 1.11550(4) 0.27306(2) 0.466517(17) 0.03552(12) Uani 1 1 d . . . P2 P 0.91827(8) 0.24354(4) 0.52115(3) 0.03534(18) Uani 1 1 d . . . P1 P 0.94758(8) 0.26988(4) 0.38190(3) 0.03496(18) Uani 1 1 d . . . Cl1 Cl 1.30365(9) 0.30792(6) 0.40393(4) 0.0589(2) Uani 1 1 d . . . Cl2 Cl 1.26573(10) 0.28038(7) 0.55724(4) 0.0691(3) Uani 1 1 d . . . C1 C 0.7528(3) 0.23132(18) 0.40423(14) 0.0399(7) Uani 1 1 d . . . H1 H 0.6907 0.278 0.4147 0.041(6) Uiso 1 1 calc R . . C2 C 0.7796(3) 0.18394(17) 0.46787(14) 0.0406(7) Uani 1 1 d . . . H2 H 0.6791 0.1804 0.4882 0.041(6) Uiso 1 1 calc R . . C3 C 0.6559(4) 0.1880(2) 0.34912(16) 0.0599(9) Uani 1 1 d . . . H3A H 0.7148 0.1434 0.335 0.074(5) Uiso 1 1 calc R . . H3B H 0.6337 0.2237 0.3132 0.074(5) Uiso 1 1 calc R . . H3C H 0.5585 0.1698 0.3647 0.074(5) Uiso 1 1 calc R . . C4 C 0.8434(4) 0.10038(14) 0.46005(15) 0.0571(9) Uani 1 1 d . . . H4A H 0.7692 0.0699 0.4328 0.074(5) Uiso 1 1 calc R . . H4B H 0.8591 0.0756 0.5021 0.074(5) Uiso 1 1 calc R . . H4C H 0.9422 0.1029 0.4403 0.074(5) Uiso 1 1 calc R . . C2*1 C 0.9973(4) 0.39712(15) 0.29933(16) 0.0616(9) Uani 1 1 d R . . H2*1 H 1.0753 0.3658 0.2829 0.074 Uiso 1 1 calc R . . C3*1 C 0.9709(5) 0.4741(2) 0.2762(2) 0.0757(12) Uani 1 1 d . . . H3*1 H 1.0304 0.4936 0.2435 0.091 Uiso 1 1 calc R . . C4*1 C 0.8592(5) 0.5213(2) 0.3006(2) 0.0732(11) Uani 1 1 d . . . H4*1 H 0.8429 0.5725 0.2847 0.088 Uiso 1 1 calc R . . C5*1 C 0.7713(5) 0.4931(2) 0.34851(19) 0.0656(10) Uani 1 1 d . . . H5*1 H 0.696 0.5255 0.3657 0.079 Uiso 1 1 calc R . . C6*1 C 0.7938(4) 0.4171(2) 0.37145(16) 0.0531(8) Uani 1 1 d . . . H6*1 H 0.7327 0.3984 0.4039 0.064 Uiso 1 1 calc R . . C1*1 C 0.9061(3) 0.36765(17) 0.34712(14) 0.0408(7) Uani 1 1 d . . . C2*2 C 1.1219(4) 0.1502(2) 0.33084(16) 0.0570(9) Uani 1 1 d . . . H2*2 H 1.1663 0.1451 0.3734 0.068 Uiso 1 1 calc R . . C3*2 C 1.1680(5) 0.1001(3) 0.28341(18) 0.0777(12) Uani 1 1 d . . . H3*2 H 1.2415 0.0604 0.2941 0.093 Uiso 1 1 calc R . . C4*2 C 1.1065(5) 0.1081(2) 0.22028(18) 0.0711(11) Uani 1 1 d . . . H4*2 H 1.1394 0.0745 0.1881 0.085 Uiso 1 1 calc R . . C5*2 C 0.9970(4) 0.1653(2) 0.20463(16) 0.0595(9) Uani 1 1 d . . . H5*2 H 0.9561 0.1711 0.1616 0.071 Uiso 1 1 calc R . . C6*2 C 0.9464(4) 0.21487(19) 0.25229(14) 0.0478(7) Uani 1 1 d . . . H6*2 H 0.8693 0.2528 0.2415 0.057 Uiso 1 1 calc R . . C1*2 C 1.0101(3) 0.20823(17) 0.31604(13) 0.0396(6) Uani 1 1 d . . . C2*3 C 0.9081(4) 0.40366(19) 0.54919(15) 0.0470(7) Uani 1 1 d . . . H2*3 H 1.0176 0.4008 0.5502 0.056 Uiso 1 1 calc R . . C3*3 C 0.8366(4) 0.47482(19) 0.56028(16) 0.0541(8) Uani 1 1 d . . . H3*3 H 0.898 0.5197 0.5693 0.065 Uiso 1 1 calc R . . C4*3 C 0.6737(4) 0.4802(2) 0.55813(15) 0.0513(8) Uani 1 1 d . . . H4*3 H 0.6253 0.5286 0.5653 0.062 Uiso 1 1 calc R . . C5*3 C 0.5844(4) 0.41356(19) 0.54538(14) 0.0464(7) Uani 1 1 d . . . H5*3 H 0.4749 0.4171 0.5439 0.056 Uiso 1 1 calc R . . C6*3 C 0.6536(3) 0.34147(18) 0.53470(13) 0.0408(7) Uani 1 1 d . . . H6*3 H 0.5914 0.2967 0.5264 0.049 Uiso 1 1 calc R . . C1*3 C 0.8184(3) 0.33574(17) 0.53647(12) 0.0357(6) Uani 1 1 d . . . C2*4 C 0.8685(4) 0.2214(2) 0.65232(16) 0.0597(9) Uani 1 1 d . . . H2*4 H 0.8033 0.2657 0.6475 0.072 Uiso 1 1 calc R . . C3*4 C 0.8881(5) 0.1836(3) 0.71224(19) 0.0782(12) Uani 1 1 d . . . H3*4 H 0.837 0.2029 0.7474 0.094 Uiso 1 1 calc R . . C4*4 C 0.9819(6) 0.1186(3) 0.7197(2) 0.0920(15) Uani 1 1 d . . . H4*4 H 0.9931 0.0927 0.7597 0.11 Uiso 1 1 calc R . . C5*4 C 1.0600(6) 0.0911(3) 0.6684(3) 0.0941(15) Uani 1 1 d . . . H5*4 H 1.1256 0.0471 0.6741 0.113 Uiso 1 1 calc R . . C6*4 C 1.0429(5) 0.1277(2) 0.60804(19) 0.0678(10) Uani 1 1 d . . . H6*4 H 1.0962 0.1086 0.5734 0.081 Uiso 1 1 calc R . . C1*4 C 0.9440(3) 0.19410(19) 0.59994(14) 0.0453(7) Uani 1 1 d . . . C1S C 0.4167(6) 0.0716(4) 0.4945(4) 0.1066(19) Uani 1 1 d . . . C2S C 0.5033(7) 0.0517(5) 0.5531(3) 0.117(2) Uani 1 1 d . . . C3S C 0.5862(7) -0.0209(5) 0.5578(4) 0.129(3) Uani 1 1 d . . . C4S C 0.5142(14) 0.0964(8) 0.6035(5) 0.110(4) Uani 0.5 1 d P . . 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 0.02490(19) 0.0450(2) 0.0366(2) -0.00520(15) 0.00225(14) -0.00316(14) P2 0.0294(4) 0.0423(4) 0.0344(4) -0.0014(3) 0.0028(3) -0.0036(3) P1 0.0301(4) 0.0418(4) 0.0330(4) -0.0042(3) 0.0025(3) -0.0006(3) Cl1 0.0379(4) 0.0821(6) 0.0585(5) -0.0095(4) 0.0165(3) -0.0132(4) Cl2 0.0409(4) 0.1122(8) 0.0519(5) 0.0020(5) -0.0121(4) -0.0213(5) C1 0.0295(14) 0.0484(17) 0.0413(16) -0.0084(13) 0.0004(11) -0.0040(12) C2 0.0324(14) 0.0461(17) 0.0435(16) -0.0068(13) 0.0042(12) -0.0104(12) C3 0.0417(17) 0.086(3) 0.0503(19) -0.0159(18) -0.0062(14) -0.0177(18) C4 0.062(2) 0.0443(18) 0.066(2) -0.0059(16) 0.0067(17) -0.0095(16) C2*1 0.060(2) 0.058(2) 0.069(2) 0.0035(18) 0.0190(18) -0.0036(17) C3*1 0.087(3) 0.069(3) 0.073(3) 0.018(2) 0.022(2) -0.014(2) C4*1 0.092(3) 0.052(2) 0.074(3) 0.016(2) -0.004(2) 0.004(2) C5*1 0.071(2) 0.057(2) 0.068(2) 0.0087(19) -0.0007(19) 0.0175(19) C6*1 0.0549(19) 0.055(2) 0.0493(19) 0.0035(15) 0.0024(15) 0.0119(16) C1*1 0.0392(15) 0.0433(16) 0.0393(16) -0.0020(13) -0.0005(12) -0.0033(13) C2*2 0.062(2) 0.068(2) 0.0398(17) -0.0085(16) -0.0009(15) 0.0212(17) C3*2 0.089(3) 0.088(3) 0.055(2) -0.016(2) 0.002(2) 0.045(2) C4*2 0.085(3) 0.083(3) 0.046(2) -0.0265(19) 0.0080(19) 0.018(2) C5*2 0.067(2) 0.077(2) 0.0334(16) -0.0105(16) -0.0007(15) -0.0040(19) C6*2 0.0448(17) 0.059(2) 0.0394(16) -0.0024(14) -0.0001(13) 0.0019(15) C1*2 0.0390(15) 0.0456(16) 0.0346(15) -0.0049(12) 0.0062(12) -0.0002(13) C2*3 0.0390(16) 0.0505(18) 0.0510(18) -0.0056(14) 0.0001(13) -0.0086(14) C3*3 0.063(2) 0.0431(18) 0.055(2) -0.0078(15) -0.0009(16) -0.0068(16) C4*3 0.063(2) 0.0495(19) 0.0420(17) 0.0008(14) 0.0048(15) 0.0129(16) C5*3 0.0413(16) 0.0556(19) 0.0429(17) 0.0028(14) 0.0074(13) 0.0063(14) C6*3 0.0356(15) 0.0481(17) 0.0391(15) -0.0008(13) 0.0044(12) -0.0031(13) C1*3 0.0346(14) 0.0438(16) 0.0288(13) 0.0009(12) 0.0028(11) -0.0024(12) C2*4 0.055(2) 0.078(3) 0.0461(19) 0.0079(17) 0.0059(15) 0.0024(18) C3*4 0.084(3) 0.105(3) 0.046(2) 0.018(2) 0.0068(19) -0.010(3) C4*4 0.105(4) 0.109(4) 0.059(3) 0.041(3) -0.012(2) -0.011(3) C5*4 0.095(3) 0.093(3) 0.093(3) 0.038(3) -0.009(3) 0.016(3) C6*4 0.068(2) 0.069(2) 0.066(2) 0.015(2) 0.0039(19) 0.011(2) C1*4 0.0386(16) 0.0566(19) 0.0402(16) 0.0077(14) -0.0009(12) -0.0042(14) C1S 0.068(3) 0.128(5) 0.124(5) 0.056(4) 0.009(3) -0.012(3) C2S 0.074(3) 0.149(6) 0.129(5) 0.050(5) 0.023(3) -0.030(4) C3S 0.081(4) 0.137(6) 0.170(7) 0.076(5) 0.010(4) 0.004(4) C4S 0.112(9) 0.150(11) 0.066(6) -0.002(7) 0.001(6) -0.029(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.1451(13) . ? Ni1 P1 2.1656(12) . ? Ni1 Cl2 2.1826(13) . ? Ni1 Cl1 2.2061(13) . ? P2 C1*3 1.810(3) . ? P2 C1*4 1.820(3) . ? P2 C2 1.844(3) . ? P1 C1*2 1.818(3) . ? P1 C1*1 1.820(3) . ? P1 C1 1.867(3) . ? C1 C3 1.534(4) . ? C1 C2 1.535(4) . ? C2 C4 1.522(4) . ? C2*1 C3*1 1.394(5) . ? C2*1 C1*1 1.389(4) . ? C3*1 C4*1 1.363(6) . ? C4*1 C5*1 1.366(5) . ? C5*1 C6*1 1.374(5) . ? C6*1 C1*1 1.388(4) . ? C2*2 C3*2 1.370(5) . ? C2*2 C1*2 1.381(4) . ? C3*2 C4*2 1.369(5) . ? C4*2 C5*2 1.361(5) . ? C5*2 C6*2 1.381(4) . ? C6*2 C1*2 1.384(4) . ? C2*3 C3*3 1.371(5) . ? C2*3 C1*3 1.389(4) . ? C3*3 C4*3 1.385(5) . ? C4*3 C5*3 1.370(5) . ? C5*3 C6*3 1.375(4) . ? C6*3 C1*3 1.401(4) . ? C2*4 C3*4 1.385(5) . ? C2*4 C1*4 1.374(5) . ? C3*4 C4*4 1.357(7) . ? C4*4 C5*4 1.370(7) . ? C5*4 C6*4 1.383(6) . ? C6*4 C1*4 1.402(5) . ? C1S C3S 1.374(9) 3_656 ? C1S C2S 1.404(8) . ? C2S C4S 1.279(12) . ? C2S C3S 1.411(9) . ? C3S C1S 1.374(9) 3_656 ? 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 P1 85.52(5) . . ? P2 Ni1 Cl2 89.71(5) . . ? P1 Ni1 Cl2 174.36(3) . . ? P2 Ni1 Cl1 175.06(4) . . ? P1 Ni1 Cl1 90.01(5) . . ? Cl2 Ni1 Cl1 94.64(5) . . ? C1*3 P2 C1*4 105.34(14) . . ? C1*3 P2 C2 106.51(13) . . ? C1*4 P2 C2 107.91(14) . . ? C1*3 P2 Ni1 106.68(9) . . ? C1*4 P2 Ni1 121.77(10) . . ? C2 P2 Ni1 107.73(10) . . ? C1*2 P1 C1*1 106.48(13) . . ? C1*2 P1 C1 107.37(14) . . ? C1*1 P1 C1 105.25(14) . . ? C1*2 P1 Ni1 113.63(10) . . ? C1*1 P1 Ni1 112.91(10) . . ? C1 P1 Ni1 110.68(10) . . ? C3 C1 C2 114.7(3) . . ? C3 C1 P1 114.8(2) . . ? C2 C1 P1 108.30(19) . . ? C4 C2 C1 115.0(2) . . ? C4 C2 P2 110.5(2) . . ? C1 C2 P2 105.64(19) . . ? C3*1 C2*1 C1*1 119.4(3) . . ? C2*1 C3*1 C4*1 121.1(3) . . ? C5*1 C4*1 C3*1 119.8(4) . . ? C6*1 C5*1 C4*1 120.1(4) . . ? C5*1 C6*1 C1*1 121.2(3) . . ? C6*1 C1*1 C2*1 118.4(3) . . ? C6*1 C1*1 P1 121.3(2) . . ? C2*1 C1*1 P1 120.0(2) . . ? C3*2 C2*2 C1*2 120.6(3) . . ? C4*2 C3*2 C2*2 120.3(3) . . ? C3*2 C4*2 C5*2 120.0(3) . . ? C6*2 C5*2 C4*2 120.3(3) . . ? C5*2 C6*2 C1*2 120.2(3) . . ? C6*2 C1*2 C2*2 118.6(3) . . ? C6*2 C1*2 P1 122.9(2) . . ? C2*2 C1*2 P1 118.4(2) . . ? C3*3 C2*3 C1*3 120.6(3) . . ? C4*3 C3*3 C2*3 120.4(3) . . ? C3*3 C4*3 C5*3 119.4(3) . . ? C6*3 C5*3 C4*3 121.2(3) . . ? C5*3 C6*3 C1*3 119.7(3) . . ? C6*3 C1*3 C2*3 118.7(3) . . ? C6*3 C1*3 P2 122.4(2) . . ? C2*3 C1*3 P2 118.9(2) . . ? C3*4 C2*4 C1*4 120.8(4) . . ? C4*4 C3*4 C2*4 120.1(4) . . ? C5*4 C4*4 C3*4 120.1(4) . . ? C4*4 C5*4 C6*4 121.0(4) . . ? C1*4 C6*4 C5*4 119.0(4) . . ? C6*4 C1*4 C2*4 119.0(3) . . ? C6*4 C1*4 P2 120.1(3) . . ? C2*4 C1*4 P2 120.9(3) . . ? C3S C1S C2S 120.0(6) 3_656 . ? C4S C2S C1S 123.8(9) . . ? C4S C2S C3S 116.7(9) . . ? C1S C2S C3S 119.5(7) . . ? C1S C3S C2S 120.5(7) 3_656 . ? data_[Ni2Cl4(cyclo-tetraphos)] _database_code_CSD 218038 _chemical_name_common (Ni2Cl4(cyclo-tetraphos)) _audit_creation_method SHELXL-97 _chemical_name_systematic [Ni2Cl4(cyclo-tetraphos)] _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cl4 P4 Ni2 x 2 C3 H7 N O' _chemical_formula_sum 'C58 H58 Cl4 N2 Ni2 O2 P4' _chemical_formula_weight 1198.20 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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' _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 12.018(2) _cell_length_b 18.891(4) _cell_length_c 13.241(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.53(3) _cell_angle_gamma 90.00 _cell_volume 2850.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6861 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.4668 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5713 _reflns_number_gt 1112 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5713 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max -0.022 _refine_ls_shift/su_mean 0.004 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 0.02301(14) 0.08723(7) 0.23717(9) 0.0484(5) Uani 1 1 d . . . P1 P -0.1234(3) 0.03257(13) 0.12620(19) 0.0449(9) Uani 1 1 d . . . P2 P 0.1328(3) 0.00786(13) 0.20053(19) 0.0448(9) Uani 1 1 d . . . Cl1 Cl -0.1001(3) 0.15788(15) 0.2821(2) 0.0829(12) Uani 1 1 d . . . Cl2 Cl 0.1777(3) 0.12997(16) 0.3573(2) 0.0881(12) Uani 1 1 d . . . C1 C -0.0743(10) -0.0171(4) 0.0276(6) 0.039(3) Uani 1 1 d . . . H1A H -0.1191 -0.0607 0.0035 0.059 Uiso 1 1 calc R . . C2 C 0.0616(9) -0.0293(5) 0.0670(6) 0.042(3) Uani 1 1 d . . . H2A H 0.0826 -0.0790 0.0617 0.064 Uiso 1 1 calc R . . C11 C -0.2464(11) 0.0855(7) 0.0488(8) 0.048(3) Uani 1 1 d . . . C12 C -0.2224(12) 0.1521(6) 0.0210(9) 0.069(4) Uani 1 1 d . . . H12A H -0.1460 0.1694 0.0423 0.104 Uiso 1 1 calc R . . C13 C -0.3151(15) 0.1933(7) -0.0398(10) 0.080(5) Uani 1 1 d . . . H13A H -0.2990 0.2384 -0.0598 0.120 Uiso 1 1 calc R . . C14 C -0.4274(14) 0.1711(8) -0.0713(10) 0.078(5) Uani 1 1 d . . . H14A H -0.4883 0.2005 -0.1093 0.116 Uiso 1 1 calc R . . C15 C -0.4486(13) 0.1020(8) -0.0446(11) 0.099(5) Uani 1 1 d . . . H15A H -0.5247 0.0841 -0.0670 0.149 Uiso 1 1 calc R . . C16 C -0.3582(14) 0.0606(6) 0.0143(10) 0.070(4) Uani 1 1 d . . . H16A H -0.3733 0.0146 0.0312 0.105 Uiso 1 1 calc R . . C21 C -0.1769(7) -0.0370(4) 0.1964(6) 0.053(3) Uani 1 1 d G . . C22 C -0.2110(8) -0.1037(4) 0.1533(5) 0.083(4) Uani 1 1 d G . . C23 C -0.2371(8) -0.1565(3) 0.2153(8) 0.100(5) Uani 1 1 d G . . C24 C -0.2291(8) -0.1426(5) 0.3205(7) 0.085(5) Uani 1 1 d G . . C25 C -0.1950(9) -0.0759(6) 0.3636(5) 0.139(7) Uani 1 1 d G . . C26 C -0.1688(8) -0.0231(4) 0.3016(6) 0.103(5) Uani 1 1 d G . . H22A H -0.2179 -0.1121 0.0861 0.154 Uiso 1 1 calc G . . H23A H -0.2584 -0.2002 0.1887 0.154 Uiso 1 1 d G . . H24A H -0.2453 -0.1783 0.3616 0.154 Uiso 1 1 d G . . H25A H -0.1932 -0.0668 0.4287 0.154 Uiso 1 1 d G . . H26A H -0.1442 0.0201 0.3314 0.154 Uiso 1 1 d G . . C31 C 0.1435(8) -0.0666(4) 0.2901(6) 0.052(3) Uani 1 1 d G . . C32 C 0.1581(11) -0.0514(4) 0.3963(7) 0.184(10) Uani 1 1 d G . . C33 C 0.1608(11) -0.1060(6) 0.4674(5) 0.190(11) Uani 1 1 d G . . C34 C 0.1488(9) -0.1758(5) 0.4323(8) 0.111(5) Uani 1 1 d G . . C35 C 0.1341(11) -0.1910(3) 0.3262(8) 0.257(15) Uani 1 1 d G . . C36 C 0.1315(11) -0.1364(4) 0.2551(5) 0.190(11) Uani 1 1 d G . . H32A H 0.1608 -0.0102 0.4125 0.285 Uiso 1 1 calc G . . H33A H 0.1778 -0.0988 0.5353 0.285 Uiso 1 1 d G . . H34A H 0.1455 -0.2091 0.4768 0.285 Uiso 1 1 d G . . H35A H 0.1243 -0.2349 0.3083 0.285 Uiso 1 1 d G . . H36A H 0.1302 -0.1431 0.1913 0.285 Uiso 1 1 d G . . C41 C 0.2815(11) 0.0308(6) 0.2089(8) 0.052(3) Uani 1 1 d . . . C42 C 0.3060(13) 0.0939(7) 0.1666(8) 0.064(4) Uani 1 1 d . . . H42A H 0.2448 0.1245 0.1332 0.096 Uiso 1 1 calc R . . C43 C 0.4204(15) 0.1123(7) 0.1729(9) 0.074(4) Uani 1 1 d . . . H43A H 0.4354 0.1553 0.1455 0.111 Uiso 1 1 calc R . . C44 C 0.5091(15) 0.0671(8) 0.2194(11) 0.096(5) Uani 1 1 d . . . H44A H 0.5860 0.0792 0.2253 0.144 Uiso 1 1 calc R . . C45 C 0.4861(14) 0.0050(9) 0.2568(11) 0.099(5) Uani 1 1 d . . . H45A H 0.5478 -0.0261 0.2870 0.149 Uiso 1 1 calc R . . C46 C 0.3711(14) -0.0152(6) 0.2521(9) 0.074(4) Uani 1 1 d . . . H46A H 0.3572 -0.0590 0.2779 0.111 Uiso 1 1 calc R . . O1 O 0.4354(11) -0.3129(5) 0.5004(8) 0.129(4) Uani 1 1 d . . . N1 N 0.4746(10) -0.2033(6) 0.4735(10) 0.082(3) Uani 1 1 d . . . C3 C 0.465(2) -0.2487(13) 0.528(2) 0.29(2) Uani 1 1 d . . . H3A H 0.4797 -0.2377 0.5997 0.432 Uiso 1 1 calc R . . C4 C 0.459(2) -0.2128(11) 0.3641(15) 0.256(13) Uani 1 1 d . . . H4A H 0.4374 -0.2610 0.3446 0.384 Uiso 1 1 calc R . . H4B H 0.5308 -0.2020 0.3504 0.384 Uiso 1 1 calc R . . H4C H 0.3980 -0.1819 0.3230 0.384 Uiso 1 1 calc R . . C5 C 0.5079(16) -0.1320(8) 0.5034(14) 0.200(10) Uani 1 1 d . . . H5A H 0.5606 -0.1309 0.5751 0.300 Uiso 1 1 calc R . . H5B H 0.4392 -0.1046 0.4989 0.300 Uiso 1 1 calc R . . H5C H 0.5462 -0.1125 0.4562 0.300 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 0.0580(13) 0.0434(7) 0.0441(7) -0.0069(6) 0.0167(8) 0.0059(9) P1 0.051(3) 0.0436(15) 0.0441(14) -0.0013(13) 0.0215(17) -0.0031(18) P2 0.048(3) 0.0422(16) 0.0395(13) -0.0011(12) 0.0069(16) 0.0026(18) Cl1 0.104(3) 0.074(2) 0.0790(19) -0.0196(16) 0.041(2) 0.019(2) Cl2 0.095(3) 0.085(2) 0.0708(18) -0.0347(17) 0.007(2) -0.003(2) C1 0.061(9) 0.033(5) 0.029(4) 0.003(4) 0.022(6) -0.001(6) C2 0.030(8) 0.059(6) 0.031(5) -0.002(4) -0.001(5) 0.013(6) C11 0.031(9) 0.064(8) 0.057(6) -0.009(6) 0.026(7) 0.012(8) C12 0.064(12) 0.040(7) 0.110(10) 0.008(7) 0.036(9) 0.001(8) C13 0.097(15) 0.064(9) 0.097(10) 0.015(8) 0.055(11) 0.020(11) C14 0.055(13) 0.087(11) 0.096(10) 0.032(8) 0.031(10) 0.042(10) C15 0.071(14) 0.106(11) 0.141(12) 0.058(10) 0.061(11) 0.016(11) C16 0.067(13) 0.057(8) 0.096(9) 0.027(7) 0.040(10) 0.018(9) C21 0.046(9) 0.059(7) 0.067(7) 0.013(6) 0.039(7) 0.019(7) C22 0.103(13) 0.082(9) 0.087(8) 0.009(7) 0.061(9) -0.011(9) C23 0.120(15) 0.062(8) 0.144(12) 0.041(9) 0.080(12) 0.003(9) C24 0.058(12) 0.102(12) 0.107(10) 0.058(9) 0.041(10) 0.023(10) C25 0.22(2) 0.127(14) 0.091(10) 0.006(10) 0.077(13) -0.055(15) C26 0.147(16) 0.105(11) 0.084(8) -0.002(8) 0.076(10) -0.012(11) C31 0.048(9) 0.057(7) 0.048(6) 0.002(5) 0.012(6) 0.012(7) C32 0.38(3) 0.108(12) 0.103(11) 0.051(10) 0.122(17) 0.091(16) C33 0.36(3) 0.147(15) 0.097(11) 0.023(12) 0.126(17) 0.09(2) C34 0.095(14) 0.122(14) 0.118(12) 0.024(10) 0.035(11) -0.031(12) C35 0.51(4) 0.073(10) 0.085(10) 0.039(9) -0.047(18) -0.105(18) C36 0.35(3) 0.063(9) 0.076(9) 0.025(8) -0.040(14) -0.054(15) C41 0.041(10) 0.047(7) 0.063(6) -0.010(6) 0.007(7) -0.004(7) C42 0.063(12) 0.067(8) 0.058(7) 0.010(6) 0.014(8) 0.003(9) C43 0.066(13) 0.083(10) 0.078(9) 0.002(7) 0.030(9) -0.022(10) C44 0.094(15) 0.091(11) 0.111(11) 0.015(9) 0.044(11) 0.008(12) C45 0.065(14) 0.102(12) 0.144(13) 0.028(11) 0.053(11) 0.035(12) C46 0.065(12) 0.068(9) 0.099(9) 0.020(7) 0.039(10) 0.010(10) O1 0.139(11) 0.090(7) 0.162(9) 0.051(7) 0.052(8) -0.001(8) N1 0.069(10) 0.053(6) 0.112(8) -0.003(6) 0.013(8) 0.006(7) C3 0.22(3) 0.27(3) 0.43(4) 0.31(3) 0.18(3) 0.13(3) C4 0.35(4) 0.27(3) 0.17(2) 0.008(18) 0.13(2) 0.14(2) C5 0.135(19) 0.099(13) 0.26(2) 0.022(14) -0.079(16) -0.007(14) _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 2.152(3) . ? Ni1 P1 2.162(3) . ? Ni1 Cl2 2.182(4) . ? Ni1 Cl1 2.210(3) . ? P1 C11 1.809(11) . ? P1 C21 1.840(6) . ? P1 C1 1.849(8) . ? P2 C41 1.807(12) . ? P2 C31 1.818(6) . ? P2 C2 1.841(8) . ? C1 C2 1.566(12) . ? C1 C2 1.576(10) 3 ? C2 C1 1.576(10) 3 ? C11 C16 1.358(14) . ? C11 C12 1.368(14) . ? C12 C13 1.387(15) . ? C13 C14 1.347(16) . ? C14 C15 1.396(15) . ? C15 C16 1.364(15) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C46 1.361(14) . ? C41 C42 1.388(14) . ? C42 C43 1.394(15) . ? C43 C44 1.353(16) . ? C44 C45 1.337(16) . ? C45 C46 1.416(16) . ? O1 C3 1.28(3) . ? N1 C3 1.151(16) . ? N1 C4 1.412(17) . ? N1 C5 1.425(15) . ? 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 P1 86.49(12) . . ? P2 Ni1 Cl2 88.91(13) . . ? P1 Ni1 Cl2 173.15(13) . . ? P2 Ni1 Cl1 172.91(14) . . ? P1 Ni1 Cl1 90.10(13) . . ? Cl2 Ni1 Cl1 93.92(13) . . ? C11 P1 C21 109.1(5) . . ? C11 P1 C1 105.5(4) . . ? C21 P1 C1 103.6(4) . . ? C11 P1 Ni1 117.6(4) . . ? C21 P1 Ni1 109.7(3) . . ? C1 P1 Ni1 110.4(4) . . ? C41 P2 C31 106.4(5) . . ? C41 P2 C2 107.4(5) . . ? C31 P2 C2 104.2(4) . . ? C41 P2 Ni1 118.9(4) . . ? C31 P2 Ni1 108.3(3) . . ? C2 P2 Ni1 110.6(4) . . ? C2 C1 C2 89.6(8) . 3 ? C2 C1 P1 111.9(6) . . ? C2 C1 P1 114.3(6) 3 . ? C1 C2 C1 90.4(8) . 3 ? C1 C2 P2 112.4(6) . . ? C1 C2 P2 114.7(7) 3 . ? C16 C11 C12 119.9(12) . . ? C16 C11 P1 122.8(11) . . ? C12 C11 P1 117.2(11) . . ? C11 C12 C13 118.3(13) . . ? C14 C13 C12 123.0(14) . . ? C13 C14 C15 117.3(14) . . ? C16 C15 C14 120.2(14) . . ? C11 C16 C15 121.1(12) . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 123.0(5) . . ? C26 C21 P1 116.6(5) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 117.4(5) . . ? C36 C31 P2 122.5(5) . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C46 C41 C42 118.5(12) . . ? C46 C41 P2 120.5(11) . . ? C42 C41 P2 120.9(11) . . ? C41 C42 C43 121.4(12) . . ? C44 C43 C42 119.3(14) . . ? C45 C44 C43 119.8(16) . . ? C44 C45 C46 122.3(15) . . ? C41 C46 C45 118.6(12) . . ? C3 N1 C4 123(2) . . ? C3 N1 C5 127(2) . . ? C4 N1 C5 109.8(15) . . ? N1 C3 O1 127(3) . . ? 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 P2 Ni1 P1 C11 -146.2(4) . . . . ? Cl2 Ni1 P1 C11 166.0(12) . . . . ? Cl1 Ni1 P1 C11 40.1(4) . . . . ? P2 Ni1 P1 C21 88.5(3) . . . . ? Cl2 Ni1 P1 C21 40.6(13) . . . . ? Cl1 Ni1 P1 C21 -85.3(3) . . . . ? P2 Ni1 P1 C1 -25.1(3) . . . . ? Cl2 Ni1 P1 C1 -73.0(12) . . . . ? Cl1 Ni1 P1 C1 161.1(3) . . . . ? P1 Ni1 P2 C41 150.6(4) . . . . ? Cl2 Ni1 P2 C41 -34.5(4) . . . . ? Cl1 Ni1 P2 C41 -148.1(10) . . . . ? P1 Ni1 P2 C31 -88.0(3) . . . . ? Cl2 Ni1 P2 C31 86.9(3) . . . . ? Cl1 Ni1 P2 C31 -26.6(12) . . . . ? P1 Ni1 P2 C2 25.6(3) . . . . ? Cl2 Ni1 P2 C2 -159.4(4) . . . . ? Cl1 Ni1 P2 C2 87.0(11) . . . . ? C11 P1 C1 C2 146.9(7) . . . . ? C21 P1 C1 C2 -98.5(7) . . . . ? Ni1 P1 C1 C2 18.9(7) . . . . ? C11 P1 C1 C2 46.9(10) . . . 3 ? C21 P1 C1 C2 161.5(8) . . . 3 ? Ni1 P1 C1 C2 -81.1(8) . . . 3 ? C2 C1 C2 C1 0.0 3 . . 3 ? P1 C1 C2 C1 -116.2(6) . . . 3 ? C2 C1 C2 P2 117.1(7) 3 . . . ? P1 C1 C2 P2 0.9(9) . . . . ? C41 P2 C2 C1 -151.7(7) . . . . ? C31 P2 C2 C1 95.6(7) . . . . ? Ni1 P2 C2 C1 -20.5(7) . . . . ? C41 P2 C2 C1 -50.3(10) . . . 3 ? C31 P2 C2 C1 -162.9(8) . . . 3 ? Ni1 P2 C2 C1 80.9(8) . . . 3 ? C21 P1 C11 C16 -24.6(10) . . . . ? C1 P1 C11 C16 86.2(10) . . . . ? Ni1 P1 C11 C16 -150.3(8) . . . . ? C21 P1 C11 C12 158.4(8) . . . . ? C1 P1 C11 C12 -90.9(9) . . . . ? Ni1 P1 C11 C12 32.7(9) . . . . ? C16 C11 C12 C13 1.9(16) . . . . ? P1 C11 C12 C13 179.0(8) . . . . ? C11 C12 C13 C14 1.0(19) . . . . ? C12 C13 C14 C15 -3(2) . . . . ? C13 C14 C15 C16 2(2) . . . . ? C12 C11 C16 C15 -2.6(18) . . . . ? P1 C11 C16 C15 -179.5(9) . . . . ? C14 C15 C16 C11 0(2) . . . . ? C11 P1 C21 C22 90.6(6) . . . . ? C1 P1 C21 C22 -21.4(6) . . . . ? Ni1 P1 C21 C22 -139.3(4) . . . . ? C11 P1 C21 C26 -96.8(5) . . . . ? C1 P1 C21 C26 151.2(5) . . . . ? Ni1 P1 C21 C26 33.2(5) . . . . ? C26 C21 C22 C23 0.0 . . . . ? P1 C21 C22 C23 172.3(6) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? P1 C21 C26 C25 -172.8(5) . . . . ? C41 P2 C31 C32 86.9(7) . . . . ? C2 P2 C31 C32 -159.8(6) . . . . ? Ni1 P2 C31 C32 -42.0(6) . . . . ? C41 P2 C31 C36 -96.6(7) . . . . ? C2 P2 C31 C36 16.8(8) . . . . ? Ni1 P2 C31 C36 134.5(6) . . . . ? C36 C31 C32 C33 0.0 . . . . ? P2 C31 C32 C33 176.7(7) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? P2 C31 C36 C35 -176.5(7) . . . . ? C31 P2 C41 C46 16.2(10) . . . . ? C2 P2 C41 C46 -95.0(10) . . . . ? Ni1 P2 C41 C46 138.6(8) . . . . ? C31 P2 C41 C42 -167.3(8) . . . . ? C2 P2 C41 C42 81.5(9) . . . . ? Ni1 P2 C41 C42 -44.9(10) . . . . ? C46 C41 C42 C43 -3.7(16) . . . . ? P2 C41 C42 C43 179.7(9) . . . . ? C41 C42 C43 C44 1.4(18) . . . . ? C42 C43 C44 C45 1(2) . . . . ? C43 C44 C45 C46 -2(2) . . . . ? C42 C41 C46 C45 3.3(17) . . . . ? P2 C41 C46 C45 179.9(9) . . . . ? C44 C45 C46 C41 -1(2) . . . . ? C4 N1 C3 O1 -2(4) . . . . ? C5 N1 C3 O1 -180(2) . . . . ? _diffrn_measured_fraction 0.969 _diffrn_reflns_theta_full 26.50 _refine_diff_density_max 0.483 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.095 data_[NiCl2(R,R-chiraphos)] _database_code_CSD 218039 _chemical_name_common (NiCl2(R,R-chiraphos)) _audit_creation_method SHELXL-97 _chemical_name_systematic [NiCl2(R,R-chiraphos)] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Cl2 Ni P2' _chemical_formula_weight 556.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.7509(1) _cell_length_b 17.4206(2) _cell_length_c 9.7140(5) _cell_angle_alpha 90.000 _cell_angle_beta 102.218(1) _cell_angle_gamma 90.000 _cell_volume 1281.93(7) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 28362 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.105 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 243(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 'Kappa CCD' _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_% 0 _diffrn_reflns_number 11313 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4411 _reflns_number_gt 2756 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL PLUS' _computing_publication_material 'SHELXTL PLUS' _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^)+(0.0241P)^2^+0.1553P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(9) _refine_ls_number_reflns 4411 _refine_ls_number_parameters 300 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0165 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0434 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.29010(4) 0.335050(18) 0.75202(3) 0.02647(8) Uani 1 1 d . . . Cl1 Cl 0.11060(8) 0.27905(4) 0.87051(7) 0.03698(16) Uani 1 1 d . . . Cl2 Cl 0.16412(9) 0.44720(4) 0.74416(8) 0.04654(19) Uani 1 1 d . . . P1 P 0.42556(8) 0.22812(4) 0.75564(7) 0.02778(15) Uani 1 1 d . . . P2 P 0.48365(8) 0.38137(4) 0.64507(7) 0.02734(15) Uani 1 1 d . . . C1 C 0.5800(3) 0.23197(15) 0.6342(3) 0.0313(6) Uani 1 1 d . . . H1 H 0.5082 0.2295 0.5383 0.047 Uiso 1 1 calc R . . C1A C 0.7119(4) 0.16532(16) 0.6493(3) 0.0429(7) Uani 1 1 d . . . H1AA H 0.7707 0.1660 0.5717 0.064 Uiso 1 1 calc R . . H1AB H 0.6502 0.1176 0.6497 0.064 Uiso 1 1 calc R . . H1AC H 0.7976 0.1707 0.7360 0.064 Uiso 1 1 calc R . . C2 C 0.6653(3) 0.31172(14) 0.6518(3) 0.0305(6) Uani 1 1 d . . . H2 H 0.7392 0.3140 0.7469 0.046 Uiso 1 1 calc R . . C2A C 0.7855(3) 0.32743(19) 0.5488(3) 0.0405(6) Uani 1 1 d . . . H2AA H 0.8856 0.2937 0.5691 0.061 Uiso 1 1 calc R . . H2AB H 0.8252 0.3797 0.5584 0.061 Uiso 1 1 calc R . . H2AC H 0.7212 0.3187 0.4542 0.061 Uiso 1 1 calc R . . C11 C 0.5642(3) 0.21490(15) 0.9300(3) 0.0327(6) Uani 1 1 d . . . C12 C 0.5951(3) 0.27828(18) 1.0173(3) 0.0406(6) Uani 1 1 d . . . H12A H 0.5373 0.3242 0.9883 0.049 Uiso 1 1 calc R . . C13 C 0.7104(4) 0.2747(2) 1.1469(3) 0.0512(7) Uani 1 1 d . . . H13A H 0.7311 0.3181 1.2036 0.061 Uiso 1 1 calc R . . C14 C 0.7933(4) 0.2077(2) 1.1915(3) 0.0572(9) Uani 1 1 d . . . H14A H 0.8716 0.2055 1.2783 0.069 Uiso 1 1 calc R . . C15 C 0.7618(4) 0.1427(2) 1.1084(3) 0.0574(9) Uani 1 1 d . . . H15A H 0.8161 0.0965 1.1404 0.069 Uiso 1 1 calc R . . C16 C 0.6484(4) 0.14657(17) 0.9764(3) 0.0455(7) Uani 1 1 d . . . H16A H 0.6292 0.1032 0.9194 0.055 Uiso 1 1 calc R . . C21 C 0.2893(3) 0.14392(14) 0.7030(3) 0.0315(6) Uani 1 1 d . . . C22 C 0.2175(3) 0.13299(15) 0.5608(3) 0.0370(6) Uani 1 1 d . . . H22A H 0.2468 0.1665 0.4948 0.044 Uiso 1 1 calc R . . C23 C 0.1030(4) 0.07283(17) 0.5166(3) 0.0443(7) Uani 1 1 d . . . H23A H 0.0553 0.0661 0.4212 0.053 Uiso 1 1 calc R . . C24 C 0.0595(4) 0.02287(17) 0.6134(3) 0.0493(8) Uani 1 1 d . . . H24A H -0.0162 -0.0181 0.5837 0.059 Uiso 1 1 calc R . . C25 C 0.1283(4) 0.03379(18) 0.7540(3) 0.0515(8) Uani 1 1 d . . . H25A H 0.0972 0.0004 0.8195 0.062 Uiso 1 1 calc R . . C26 C 0.2432(4) 0.09364(16) 0.8000(3) 0.0454(7) Uani 1 1 d . . . H26A H 0.2895 0.1002 0.8957 0.054 Uiso 1 1 calc R . . C31 C 0.5865(3) 0.47129(15) 0.7105(3) 0.0311(6) Uani 1 1 d . . . C32 C 0.5034(4) 0.54096(16) 0.6701(3) 0.0402(7) Uani 1 1 d . . . H32A H 0.3967 0.5416 0.6048 0.048 Uiso 1 1 calc R . . C33 C 0.5783(4) 0.60953(17) 0.7266(3) 0.0493(8) Uani 1 1 d . . . H33A H 0.5214 0.6557 0.6987 0.059 Uiso 1 1 calc R . . C34 C 0.7353(4) 0.60953(19) 0.8229(3) 0.0519(8) Uani 1 1 d . . . H34A H 0.7850 0.6556 0.8605 0.062 Uiso 1 1 calc R . . C35 C 0.8196(4) 0.5408(2) 0.8640(3) 0.0510(8) Uani 1 1 d . . . H35A H 0.9263 0.5409 0.9293 0.061 Uiso 1 1 calc R . . C36 C 0.7473(3) 0.47201(17) 0.8092(3) 0.0386(6) Uani 1 1 d . . . H36A H 0.8052 0.4261 0.8378 0.046 Uiso 1 1 calc R . . C41 C 0.3929(3) 0.39449(14) 0.4576(3) 0.0300(6) Uani 1 1 d . . . C42 C 0.2466(3) 0.35154(16) 0.3928(3) 0.0390(7) Uani 1 1 d . . . H42A H 0.1885 0.3210 0.4472 0.047 Uiso 1 1 calc R . . C43 C 0.1872(4) 0.35385(18) 0.2490(3) 0.0497(9) Uani 1 1 d . . . H43A H 0.0919 0.3236 0.2064 0.060 Uiso 1 1 calc R . . C44 C 0.2687(4) 0.40088(18) 0.1681(3) 0.0495(8) Uani 1 1 d . . . H44A H 0.2267 0.4032 0.0711 0.059 Uiso 1 1 calc R . . C45 C 0.4111(4) 0.44419(16) 0.2300(3) 0.0454(7) Uani 1 1 d . . . H45A H 0.4663 0.4757 0.1750 0.054 Uiso 1 1 calc R . . C46 C 0.4731(4) 0.44125(16) 0.3739(3) 0.0403(7) Uani 1 1 d . . . H46A H 0.5698 0.4710 0.4154 0.048 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 0.02416(13) 0.02437(16) 0.03078(16) -0.00101(14) 0.00562(11) 0.00034(13) Cl1 0.0342(3) 0.0372(4) 0.0423(4) -0.0004(3) 0.0143(3) -0.0034(3) Cl2 0.0373(3) 0.0292(4) 0.0762(5) 0.0051(3) 0.0190(3) 0.0077(3) P1 0.0282(3) 0.0235(4) 0.0322(4) -0.0025(3) 0.0077(3) -0.0008(3) P2 0.0263(3) 0.0245(3) 0.0305(4) 0.0001(3) 0.0045(3) -0.0019(3) C1 0.0321(13) 0.0299(14) 0.0332(14) -0.0049(12) 0.0099(11) 0.0014(12) C1A 0.0422(15) 0.0329(17) 0.0581(18) -0.0070(14) 0.0208(13) 0.0028(13) C2 0.0296(13) 0.0305(15) 0.0310(13) 0.0012(10) 0.0058(10) 0.0010(10) C2A 0.0337(13) 0.0464(18) 0.0443(15) -0.0004(15) 0.0152(11) -0.0044(14) C11 0.0301(13) 0.0319(16) 0.0370(15) 0.0050(12) 0.0092(11) -0.0001(11) C12 0.0416(14) 0.0381(16) 0.0403(16) -0.0012(13) 0.0044(12) 0.0046(13) C13 0.0531(17) 0.058(2) 0.0375(16) -0.0029(15) -0.0015(14) -0.0044(17) C14 0.0467(18) 0.072(3) 0.0477(19) 0.0121(18) -0.0006(14) -0.0003(17) C15 0.0435(16) 0.063(2) 0.065(2) 0.0324(19) 0.0097(16) 0.0176(16) C16 0.0513(16) 0.0331(17) 0.0547(18) 0.0061(14) 0.0168(14) 0.0033(13) C21 0.0309(13) 0.0236(14) 0.0415(15) -0.0086(11) 0.0106(11) -0.0034(11) C22 0.0377(14) 0.0293(15) 0.0457(17) -0.0030(12) 0.0125(12) -0.0030(11) C23 0.0412(15) 0.0418(18) 0.0479(18) -0.0141(14) 0.0048(13) -0.0018(13) C24 0.0410(16) 0.0373(18) 0.071(2) -0.0163(15) 0.0153(15) -0.0151(14) C25 0.0574(19) 0.0382(18) 0.062(2) 0.0006(15) 0.0199(16) -0.0186(15) C26 0.0535(17) 0.0389(18) 0.0462(17) -0.0033(14) 0.0163(14) -0.0103(15) C31 0.0344(13) 0.0292(15) 0.0311(14) -0.0048(11) 0.0100(11) -0.0039(11) C32 0.0439(15) 0.0332(17) 0.0467(17) -0.0028(13) 0.0171(13) -0.0047(13) C33 0.066(2) 0.0278(16) 0.063(2) -0.0036(14) 0.0343(17) -0.0040(15) C34 0.064(2) 0.042(2) 0.060(2) -0.0248(16) 0.0349(17) -0.0287(17) C35 0.0514(18) 0.060(2) 0.0445(18) -0.0189(16) 0.0158(14) -0.0189(17) C36 0.0408(15) 0.0395(17) 0.0370(16) -0.0068(13) 0.0117(12) -0.0053(13) C41 0.0309(13) 0.0250(14) 0.0324(14) -0.0024(10) 0.0027(11) 0.0004(10) C42 0.0348(13) 0.0375(18) 0.0434(15) -0.0015(12) 0.0053(11) -0.0021(12) C43 0.0443(16) 0.051(2) 0.0466(17) -0.0145(14) -0.0057(13) -0.0020(14) C44 0.069(2) 0.0429(19) 0.0317(16) -0.0014(14) -0.0017(15) 0.0094(15) C45 0.0640(19) 0.0350(17) 0.0371(17) 0.0069(13) 0.0103(14) 0.0004(15) C46 0.0493(16) 0.0307(16) 0.0399(17) 0.0013(12) 0.0075(13) -0.0082(13) _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 P1 2.1350(8) . ? Ni1 P2 2.1542(8) . ? Ni1 Cl2 2.1783(8) . ? Ni1 Cl1 2.2115(8) . ? P1 C21 1.817(2) . ? P1 C11 1.818(3) . ? P1 C1 1.851(2) . ? P2 C31 1.811(3) . ? P2 C41 1.822(3) . ? P2 C2 1.849(2) . ? C1 C2 1.533(3) . ? C1 C1A 1.534(4) . ? C2 C2A 1.529(3) . ? C11 C12 1.382(4) . ? C11 C16 1.386(4) . ? C12 C13 1.383(4) . ? C13 C14 1.359(5) . ? C14 C15 1.382(5) . ? C15 C16 1.394(4) . ? C21 C26 1.388(4) . ? C21 C22 1.388(4) . ? C22 C23 1.382(4) . ? C23 C24 1.375(4) . ? C24 C25 1.370(4) . ? C25 C26 1.383(4) . ? C31 C32 1.391(4) . ? C31 C36 1.402(4) . ? C32 C33 1.389(4) . ? C33 C34 1.369(4) . ? C34 C35 1.382(5) . ? C35 C36 1.381(4) . ? C41 C46 1.388(4) . ? C41 C42 1.393(3) . ? C42 C43 1.376(4) . ? C43 C44 1.378(4) . ? C44 C45 1.367(4) . ? C45 C46 1.380(4) . ? 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 Ni1 P2 86.82(3) . . ? P1 Ni1 Cl2 176.77(3) . . ? P2 Ni1 Cl2 89.99(3) . . ? P1 Ni1 Cl1 88.16(3) . . ? P2 Ni1 Cl1 174.46(3) . . ? Cl2 Ni1 Cl1 95.00(3) . . ? C21 P1 C11 110.73(12) . . ? C21 P1 C1 105.41(11) . . ? C11 P1 C1 105.28(11) . . ? C21 P1 Ni1 116.44(8) . . ? C11 P1 Ni1 108.52(9) . . ? C1 P1 Ni1 109.88(9) . . ? C31 P2 C41 106.89(12) . . ? C31 P2 C2 106.26(12) . . ? C41 P2 C2 104.33(11) . . ? C31 P2 Ni1 117.03(8) . . ? C41 P2 Ni1 111.58(9) . . ? C2 P2 Ni1 109.88(8) . . ? C2 C1 C1A 114.35(19) . . ? C2 C1 P1 106.51(16) . . ? C1A C1 P1 114.83(19) . . ? C2A C2 C1 113.5(2) . . ? C2A C2 P2 115.11(18) . . ? C1 C2 P2 106.47(15) . . ? C12 C11 C16 118.5(2) . . ? C12 C11 P1 117.5(2) . . ? C16 C11 P1 123.8(2) . . ? C11 C12 C13 121.2(3) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C16 119.7(3) . . ? C11 C16 C15 120.2(3) . . ? C26 C21 C22 118.9(2) . . ? C26 C21 P1 122.4(2) . . ? C22 C21 P1 118.52(19) . . ? C23 C22 C21 120.6(3) . . ? C24 C23 C22 120.1(3) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 121.0(3) . . ? C25 C26 C21 119.8(3) . . ? C32 C31 C36 118.4(2) . . ? C32 C31 P2 120.8(2) . . ? C36 C31 P2 120.6(2) . . ? C33 C32 C31 120.6(3) . . ? C34 C33 C32 120.4(3) . . ? C33 C34 C35 119.7(3) . . ? C36 C35 C34 120.8(3) . . ? C35 C36 C31 120.0(3) . . ? C46 C41 C42 118.3(2) . . ? C46 C41 P2 122.21(19) . . ? C42 C41 P2 119.3(2) . . ? C43 C42 C41 120.6(3) . . ? C42 C43 C44 120.1(3) . . ? C45 C44 C43 120.2(3) . . ? C44 C45 C46 120.0(3) . . ? C45 C46 C41 120.8(3) . . ? 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 P2 Ni1 P1 C21 -133.38(10) . . . . ? Cl2 Ni1 P1 C21 -142.8(6) . . . . ? Cl1 Ni1 P1 C21 48.96(10) . . . . ? P2 Ni1 P1 C11 100.93(9) . . . . ? Cl2 Ni1 P1 C11 91.5(6) . . . . ? Cl1 Ni1 P1 C11 -76.74(9) . . . . ? P2 Ni1 P1 C1 -13.69(9) . . . . ? Cl2 Ni1 P1 C1 -23.1(6) . . . . ? Cl1 Ni1 P1 C1 168.65(9) . . . . ? P1 Ni1 P2 C31 -132.06(10) . . . . ? Cl2 Ni1 P2 C31 47.41(10) . . . . ? Cl1 Ni1 P2 C31 -107.1(3) . . . . ? P1 Ni1 P2 C41 104.40(9) . . . . ? Cl2 Ni1 P2 C41 -76.13(9) . . . . ? Cl1 Ni1 P2 C41 129.4(3) . . . . ? P1 Ni1 P2 C2 -10.82(9) . . . . ? Cl2 Ni1 P2 C2 168.65(9) . . . . ? Cl1 Ni1 P2 C2 14.2(3) . . . . ? C21 P1 C1 C2 166.61(16) . . . . ? C11 P1 C1 C2 -76.27(18) . . . . ? Ni1 P1 C1 C2 40.40(17) . . . . ? C21 P1 C1 C1A -65.7(2) . . . . ? C11 P1 C1 C1A 51.4(2) . . . . ? Ni1 P1 C1 C1A 168.07(16) . . . . ? C1A C1 C2 C2A 57.2(3) . . . . ? P1 C1 C2 C2A -174.83(17) . . . . ? C1A C1 C2 P2 -175.15(18) . . . . ? P1 C1 C2 P2 -47.20(18) . . . . ? C31 P2 C2 C2A -67.8(2) . . . . ? C41 P2 C2 C2A 44.9(2) . . . . ? Ni1 P2 C2 C2A 164.65(17) . . . . ? C31 P2 C2 C1 165.51(16) . . . . ? C41 P2 C2 C1 -81.73(18) . . . . ? Ni1 P2 C2 C1 38.01(17) . . . . ? C21 P1 C11 C12 -143.79(19) . . . . ? C1 P1 C11 C12 102.8(2) . . . . ? Ni1 P1 C11 C12 -14.8(2) . . . . ? C21 P1 C11 C16 40.2(2) . . . . ? C1 P1 C11 C16 -73.2(2) . . . . ? Ni1 P1 C11 C16 169.20(19) . . . . ? C16 C11 C12 C13 1.5(4) . . . . ? P1 C11 C12 C13 -174.7(2) . . . . ? C11 C12 C13 C14 -1.1(4) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 1.9(5) . . . . ? C12 C11 C16 C15 -0.2(4) . . . . ? P1 C11 C16 C15 175.8(2) . . . . ? C14 C15 C16 C11 -1.5(4) . . . . ? C11 P1 C21 C26 24.9(3) . . . . ? C1 P1 C21 C26 138.3(2) . . . . ? Ni1 P1 C21 C26 -99.7(2) . . . . ? C11 P1 C21 C22 -160.26(19) . . . . ? C1 P1 C21 C22 -46.9(2) . . . . ? Ni1 P1 C21 C22 75.2(2) . . . . ? C26 C21 C22 C23 -0.4(4) . . . . ? P1 C21 C22 C23 -175.4(2) . . . . ? C21 C22 C23 C24 -0.3(4) . . . . ? C22 C23 C24 C25 1.0(4) . . . . ? C23 C24 C25 C26 -1.0(5) . . . . ? C24 C25 C26 C21 0.4(5) . . . . ? C22 C21 C26 C25 0.3(4) . . . . ? P1 C21 C26 C25 175.1(2) . . . . ? C41 P2 C31 C32 43.3(2) . . . . ? C2 P2 C31 C32 154.3(2) . . . . ? Ni1 P2 C31 C32 -82.6(2) . . . . ? C41 P2 C31 C36 -140.3(2) . . . . ? C2 P2 C31 C36 -29.3(2) . . . . ? Ni1 P2 C31 C36 93.8(2) . . . . ? C36 C31 C32 C33 -0.1(4) . . . . ? P2 C31 C32 C33 176.5(2) . . . . ? C31 C32 C33 C34 0.0(4) . . . . ? C32 C33 C34 C35 0.0(4) . . . . ? C33 C34 C35 C36 -0.1(4) . . . . ? C34 C35 C36 C31 0.1(4) . . . . ? C32 C31 C36 C35 0.0(4) . . . . ? P2 C31 C36 C35 -176.5(2) . . . . ? C31 P2 C41 C46 33.5(3) . . . . ? C2 P2 C41 C46 -78.9(2) . . . . ? Ni1 P2 C41 C46 162.6(2) . . . . ? C31 P2 C41 C42 -152.0(2) . . . . ? C2 P2 C41 C42 95.6(2) . . . . ? Ni1 P2 C41 C42 -22.9(2) . . . . ? C46 C41 C42 C43 2.0(4) . . . . ? P2 C41 C42 C43 -172.7(2) . . . . ? C41 C42 C43 C44 -2.2(4) . . . . ? C42 C43 C44 C45 1.4(5) . . . . ? C43 C44 C45 C46 -0.4(5) . . . . ? C44 C45 C46 C41 0.2(4) . . . . ? C42 C41 C46 C45 -1.0(4) . . . . ? P2 C41 C46 C45 173.6(2) . . . . ? _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction 0.994 _refine_diff_density_max 0.110 _refine_diff_density_min -0.140 _refine_diff_density_rms 0.030