# Copyright The Royal Society of Chemistry, 1998 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Franc Meyer Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 6221 54-8315' _publ_contact_author_fax '049 6221 54-5707' _publ_contact_author_email Franc@sun0.urz.UNI-HEIDELBERG.DE _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; 'A novel one-dimensional nickel(II) alternating chain from discrete pyrazolate-based dinuclear complexes' ; loop_ _publ_author_name _publ_author_address 'Franc Meyer' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Uwe Ruschewitz' ; Institut fuer Anorganische Chemie der RWTH Aachen Prof.-Pirlet-Str. 1 56064 Aachen Bundesrepublik Deutschland ; 'Peter Schober' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Bjoern Antelmann' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Laszlo Zsolnai' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #============================================================================= data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17H35Cl3N6Ni2*2CHCl3' _chemical_formula_weight 786.0 _chemical_melting_point ? _chemical_compound_source ? 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' '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.308(2) _cell_length_b 13.031(2) _cell_length_c 25.771(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6484.0(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method ? _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 1.925 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5634 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5634 _reflns_number_observed 3535 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+60.3418P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5634 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_obs 0.0592 _refine_ls_wR_factor_all 0.1398 _refine_ls_wR_factor_obs 0.1062 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.000 _refine_ls_restrained_S_all 1.027 _refine_ls_restrained_S_obs 1.000 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.66067(5) 0.14267(7) 0.37771(3) 0.0175(2) Uani 1 d . . Ni2 Ni 0.50756(4) 0.02779(7) 0.29657(4) 0.0184(2) Uani 1 d . . Cl1 Cl 0.65746(10) 0.30619(14) 0.41034(8) 0.0277(4) Uani 1 d . . Cl2 Cl 0.53441(9) 0.13322(15) 0.37213(7) 0.0244(4) Uani 1 d . . Cl3 Cl 0.40780(10) 0.1172(2) 0.27943(8) 0.0305(5) Uani 1 d . . N1 N 0.6603(3) 0.0422(5) 0.3212(2) 0.0177(13) Uani 1 d . . N2 N 0.6075(3) 0.0025(5) 0.2922(2) 0.0196(14) Uani 1 d . . N3 N 0.7679(3) 0.1469(5) 0.3535(2) 0.0208(14) Uani 1 d . . N5 N 0.5164(3) -0.0400(5) 0.2195(2) 0.0231(14) Uani 1 d . . N6 N 0.4647(3) -0.1014(5) 0.3304(2) 0.0241(15) Uani 1 d . . N4 N 0.6808(3) 0.0644(5) 0.4461(2) 0.0224(15) Uani 1 d . . C1 C 0.7200(3) 0.0153(6) 0.2974(3) 0.020(2) Uani 1 d . . C2 C 0.7060(4) -0.0430(6) 0.2538(3) 0.024(2) Uani 1 d . . H2 H 0.7363(38) -0.0662(62) 0.2293(28) 0.030 Uiso 1 d . . C3 C 0.6344(4) -0.0486(6) 0.2518(3) 0.022(2) Uani 1 d . . C4 C 0.7843(4) 0.0514(6) 0.3241(3) 0.021(2) Uani 1 d . . H4A H 0.8009(4) -0.0012(6) 0.3476(3) 0.025(15) Uiso 1 calc R . H4B H 0.8202(4) 0.0651(6) 0.2987(3) 0.025(15) Uiso 1 calc R . C5 C 0.7728(4) 0.2338(6) 0.3163(3) 0.028(2) Uani 1 d . . H5A H 0.7604(25) 0.2965(8) 0.3335(6) 0.042(15) Uiso 1 calc R . H5B H 0.7419(20) 0.2221(19) 0.2878(10) 0.042(15) Uiso 1 calc R . H5C H 0.8194(7) 0.2390(25) 0.3036(15) 0.042(15) Uiso 1 calc R . C6 C 0.8190(4) 0.1645(6) 0.3958(3) 0.024(2) Uani 1 d . . H6A H 0.8132(4) 0.2337(6) 0.4090(3) 0.026(9) Uiso 1 calc R . H6B H 0.8653(4) 0.1592(6) 0.3816(3) 0.026(9) Uiso 1 calc R . C7 C 0.8119(4) 0.0896(6) 0.4403(3) 0.027(2) Uani 1 d . . H7A H 0.8510(4) 0.0988(6) 0.4635(3) 0.026(9) Uiso 1 calc R . H7B H 0.8145(4) 0.0204(6) 0.4266(3) 0.026(9) Uiso 1 calc R . C8 C 0.7456(4) 0.0996(7) 0.4717(3) 0.032(2) Uani 1 d . . H8A H 0.7513(4) 0.0611(7) 0.5036(3) 0.026(9) Uiso 1 calc R . H8B H 0.7399(4) 0.1712(7) 0.4811(3) 0.026(9) Uiso 1 calc R . C9 C 0.6836(4) -0.0463(6) 0.4350(3) 0.031(2) Uani 1 d . . H9A H 0.7170(21) -0.0587(9) 0.4104(16) 0.026(13) Uiso 1 calc R . H9B H 0.6414(19) -0.0679(13) 0.4228(17) 0.026(13) Uiso 1 calc R . H9C H 0.6943(23) -0.0814(16) 0.4649(13) 0.026(13) Uiso 1 calc R . C10 C 0.6237(4) 0.0812(7) 0.4834(3) 0.031(2) Uani 1 d . . H10A H 0.6199(16) 0.1531(8) 0.4909(14) 0.031(13) Uiso 1 calc R . H10B H 0.6330(12) 0.0442(29) 0.5148(7) 0.031(13) Uiso 1 calc R . H10C H 0.5810(6) 0.0573(32) 0.4686(8) 0.031(13) Uiso 1 calc R . C11 C 0.5835(4) -0.0965(6) 0.2160(3) 0.022(2) Uani 1 d . . H11A H 0.5766(4) -0.1679(6) 0.2253(3) 0.010(12) Uiso 1 calc R . H11B H 0.6009(4) -0.0938(6) 0.1807(3) 0.010(12) Uiso 1 calc R . C12 C 0.5206(5) 0.0487(6) 0.1834(3) 0.034(2) Uani 1 d . . H12A H 0.5607(14) 0.0891(20) 0.1915(11) 0.030(13) Uiso 1 calc R . H12B H 0.4798(12) 0.0902(20) 0.1870(13) 0.030(13) Uiso 1 calc R . H12C H 0.5239(23) 0.0242(6) 0.1483(3) 0.030(13) Uiso 1 calc R . C13 C 0.4573(4) -0.1067(6) 0.2044(3) 0.028(2) Uani 1 d . . H13A H 0.4682(4) -0.1398(6) 0.1717(3) 0.029(9) Uiso 1 calc R . H13B H 0.4169(4) -0.0639(6) 0.1988(3) 0.029(9) Uiso 1 calc R . C14 C 0.4396(4) -0.1879(6) 0.2435(3) 0.027(2) Uani 1 d . . H14A H 0.4808(4) -0.2286(6) 0.2498(3) 0.029(9) Uiso 1 calc R . H14B H 0.4053(4) -0.2331(6) 0.2282(3) 0.029(9) Uiso 1 calc R . C15 C 0.4122(4) -0.1517(6) 0.2953(3) 0.029(2) Uiso 1 d . . H15A H 0.3750(4) -0.1034(6) 0.2890(3) 0.029(9) Uiso 1 calc R . H15B H 0.3926(4) -0.2102(6) 0.3134(3) 0.029(9) Uiso 1 calc R . C16 C 0.5190(4) -0.1749(6) 0.3458(3) 0.028(2) Uani 1 d . . H16A H 0.5479(14) -0.1443(13) 0.3718(12) 0.026(9) Uiso 1 calc R . H16B H 0.5465(14) -0.1924(26) 0.3161(5) 0.026(9) Uiso 1 calc R . H16C H 0.4978(4) -0.2358(15) 0.3595(16) 0.026(9) Uiso 1 calc R . C17 C 0.4266(4) -0.0709(7) 0.3781(3) 0.033(2) Uani 1 d . . H17A H 0.3910(15) -0.0225(26) 0.3692(4) 0.026(9) Uiso 1 calc R . H17B H 0.4582(6) -0.0401(31) 0.4022(8) 0.026(9) Uiso 1 calc R . H17C H 0.4060(19) -0.1305(8) 0.3936(10) 0.026(9) Uiso 1 calc R . C20 C 0.4932(5) 0.2926(7) 0.4745(3) 0.037(2) Uani 1 d . . H20 H 0.5273(32) 0.2686(52) 0.4496(26) 0.012(18) Uiso 1 d . . Cl20 Cl 0.5301(2) 0.3676(3) 0.52365(11) 0.0695(8) Uani 1 d . . Cl21 Cl 0.45124(13) 0.1873(2) 0.50279(10) 0.0527(7) Uani 1 d . . Cl22 Cl 0.43388(14) 0.3651(2) 0.43808(9) 0.0561(7) Uani 1 d . . C30 C 0.2821(5) 0.2025(8) 0.3742(4) 0.051(3) Uani 1 d . . H30 H 0.3305(5) 0.1939(8) 0.3637(4) 0.035(24) Uiso 1 calc R . Cl30 Cl 0.26292(13) 0.3358(2) 0.37611(10) 0.0522(7) Uani 1 d . . Cl31 Cl 0.2719(3) 0.1512(3) 0.43417(13) 0.151(2) Uani 1 d . . Cl32 Cl 0.22971(14) 0.1416(3) 0.32907(11) 0.0680(9) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0186(5) 0.0176(4) 0.0162(4) -0.0004(4) 0.0001(4) -0.0009(4) Ni2 0.0166(5) 0.0200(5) 0.0187(5) -0.0029(4) -0.0012(4) 0.0019(4) Cl1 0.0269(10) 0.0182(9) 0.0380(11) -0.0046(9) 0.0024(9) -0.0014(8) Cl2 0.0197(9) 0.0309(10) 0.0226(9) -0.0098(9) 0.0009(8) 0.0017(8) Cl3 0.0228(10) 0.0310(11) 0.0376(11) -0.0085(9) -0.0105(9) 0.0093(8) N1 0.015(3) 0.022(3) 0.016(3) 0.000(3) -0.001(3) 0.003(3) N2 0.017(3) 0.028(4) 0.014(3) -0.003(3) 0.001(3) 0.001(3) N3 0.018(3) 0.016(3) 0.028(3) 0.002(3) 0.002(3) 0.000(3) N5 0.030(4) 0.018(3) 0.021(3) -0.006(3) -0.002(3) -0.003(3) N6 0.024(3) 0.027(4) 0.021(3) 0.000(3) 0.003(3) -0.001(3) N4 0.022(3) 0.025(4) 0.020(3) -0.007(3) 0.002(3) 0.006(3) C1 0.018(4) 0.021(4) 0.021(4) 0.011(4) 0.002(3) 0.001(3) C2 0.031(4) 0.032(5) 0.010(4) -0.002(4) 0.005(3) 0.009(4) C3 0.027(4) 0.025(4) 0.014(4) 0.002(3) 0.001(3) 0.003(3) C4 0.021(4) 0.018(4) 0.023(4) 0.004(3) 0.002(3) -0.001(3) C5 0.026(4) 0.023(4) 0.033(5) 0.006(4) 0.002(4) -0.010(4) C6 0.016(4) 0.022(4) 0.034(4) -0.004(4) -0.002(3) -0.003(3) C7 0.024(4) 0.029(5) 0.029(5) -0.003(4) -0.011(4) 0.001(4) C8 0.039(5) 0.034(5) 0.021(4) -0.001(4) -0.012(4) -0.007(4) C9 0.038(5) 0.027(5) 0.027(5) 0.004(4) -0.004(4) -0.004(4) C10 0.039(5) 0.033(5) 0.021(4) 0.000(4) 0.004(4) 0.009(4) C11 0.025(4) 0.022(4) 0.019(4) -0.007(3) 0.000(3) 0.003(3) C12 0.049(6) 0.033(5) 0.019(4) 0.000(4) -0.005(4) 0.005(4) C13 0.021(4) 0.037(5) 0.026(4) -0.010(4) -0.006(4) 0.003(4) C14 0.023(4) 0.025(4) 0.033(5) -0.013(4) -0.003(4) 0.001(3) C16 0.036(5) 0.025(4) 0.023(4) 0.002(4) -0.003(4) -0.006(4) C17 0.035(5) 0.035(5) 0.030(5) -0.006(4) 0.009(4) -0.009(4) C20 0.046(5) 0.034(5) 0.030(5) -0.008(4) 0.016(4) 0.009(4) Cl20 0.086(2) 0.071(2) 0.051(2) -0.021(2) -0.006(2) -0.006(2) Cl21 0.055(2) 0.0497(15) 0.054(2) 0.0151(13) 0.0193(13) 0.0022(13) Cl22 0.064(2) 0.063(2) 0.0410(14) 0.0113(14) 0.0070(12) 0.0211(15) C30 0.055(7) 0.053(6) 0.044(6) -0.002(5) -0.016(5) 0.012(5) Cl30 0.0506(15) 0.055(2) 0.0508(14) 0.0087(14) 0.0002(13) 0.0072(12) Cl31 0.326(7) 0.074(3) 0.054(2) 0.030(2) -0.064(3) -0.038(4) Cl32 0.056(2) 0.088(2) 0.060(2) -0.026(2) -0.0140(13) 0.004(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 N1 1.959(6) . ? Ni1 N4 2.074(6) . ? Ni1 N3 2.163(6) . ? Ni1 Cl1 2.292(2) . ? Ni1 Cl2 2.445(2) . ? Ni2 N2 1.961(6) . ? Ni2 N6 2.068(6) . ? Ni2 N5 2.182(6) . ? Ni2 Cl3 2.294(2) . ? Ni2 Cl2 2.439(2) . ? N1 C1 1.351(9) . ? N1 N2 1.365(8) . ? N2 C3 1.340(9) . ? N3 C5 1.486(9) . ? N3 C6 1.488(9) . ? N3 C4 1.491(9) . ? N5 C13 1.486(9) . ? N5 C12 1.486(10) . ? N5 C11 1.492(9) . ? N6 C16 1.474(10) . ? N6 C17 1.486(9) . ? N6 C15 1.508(9) . ? N4 C10 1.478(9) . ? N4 C9 1.472(10) . ? N4 C8 1.488(9) . ? C1 C2 1.383(11) . ? C1 C4 1.495(10) . ? C2 C3 1.385(10) . ? C3 C11 1.486(10) . ? C6 C7 1.514(10) . ? C7 C8 1.520(11) . ? C13 C14 1.502(11) . ? C14 C15 1.510(10) . ? C20 Cl20 1.751(9) . ? C20 Cl21 1.752(9) . ? C20 Cl22 1.757(9) . ? C30 Cl31 1.696(10) . ? C30 Cl32 1.734(10) . ? C30 Cl30 1.777(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 107.7(2) . . ? N1 Ni1 N3 78.8(2) . . ? N4 Ni1 N3 94.5(2) . . ? N1 Ni1 Cl1 153.4(2) . . ? N4 Ni1 Cl1 98.7(2) . . ? N3 Ni1 Cl1 96.2(2) . . ? N1 Ni1 Cl2 85.4(2) . . ? N4 Ni1 Cl2 102.2(2) . . ? N3 Ni1 Cl2 159.8(2) . . ? Cl1 Ni1 Cl2 92.38(7) . . ? N2 Ni2 N6 106.3(2) . . ? N2 Ni2 N5 78.6(2) . . ? N6 Ni2 N5 94.9(2) . . ? N2 Ni2 Cl3 154.2(2) . . ? N6 Ni2 Cl3 99.1(2) . . ? N5 Ni2 Cl3 95.5(2) . . ? N2 Ni2 Cl2 86.1(2) . . ? N6 Ni2 Cl2 102.0(2) . . ? N5 Ni2 Cl2 159.9(2) . . ? Cl3 Ni2 Cl2 92.64(7) . . ? Ni2 Cl2 Ni1 106.69(7) . . ? C1 N1 N2 106.9(5) . . ? C1 N1 Ni1 120.5(5) . . ? N2 N1 Ni1 131.5(4) . . ? C3 N2 N1 108.9(6) . . ? C3 N2 Ni2 120.6(5) . . ? N1 N2 Ni2 129.8(4) . . ? C5 N3 C6 108.2(6) . . ? C5 N3 C4 107.1(5) . . ? C6 N3 C4 111.1(6) . . ? C5 N3 Ni1 105.5(4) . . ? C6 N3 Ni1 115.3(4) . . ? C4 N3 Ni1 109.2(4) . . ? C13 N5 C12 109.4(6) . . ? C13 N5 C11 111.2(6) . . ? C12 N5 C11 107.4(6) . . ? C13 N5 Ni2 114.5(5) . . ? C12 N5 Ni2 105.0(4) . . ? C11 N5 Ni2 108.8(4) . . ? C16 N6 C17 107.6(6) . . ? C16 N6 C15 110.9(6) . . ? C17 N6 C15 106.2(6) . . ? C16 N6 Ni2 111.0(5) . . ? C17 N6 Ni2 109.2(5) . . ? C15 N6 Ni2 111.7(5) . . ? C10 N4 C9 107.5(6) . . ? C10 N4 C8 107.1(6) . . ? C9 N4 C8 110.9(6) . . ? C10 N4 Ni1 109.9(4) . . ? C9 N4 Ni1 108.9(5) . . ? C8 N4 Ni1 112.5(5) . . ? N1 C1 C2 110.2(6) . . ? N1 C1 C4 114.7(7) . . ? C2 C1 C4 135.1(7) . . ? C3 C2 C1 104.7(7) . . ? N2 C3 C2 109.4(7) . . ? N2 C3 C11 115.8(6) . . ? C2 C3 C11 134.8(7) . . ? N3 C4 C1 108.7(6) . . ? N3 C6 C7 113.4(6) . . ? C6 C7 C8 115.1(7) . . ? N4 C8 C7 116.5(6) . . ? C3 C11 N5 109.2(6) . . ? N5 C13 C14 114.3(6) . . ? C13 C14 C15 116.9(7) . . ? N6 C15 C14 115.5(6) . . ? Cl20 C20 Cl21 109.0(5) . . ? Cl20 C20 Cl22 110.6(5) . . ? Cl21 C20 Cl22 110.0(5) . . ? Cl31 C30 Cl32 111.3(6) . . ? Cl31 C30 Cl30 109.6(6) . . ? Cl32 C30 Cl30 110.1(5) . . ? _refine_diff_density_max 0.732 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.139 #=END data_2a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15H31Cl3N6Ni2*2CHCl3' _chemical_formula_weight 757.9 _chemical_melting_point ? _chemical_compound_source ? 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' '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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.038(4) _cell_length_b 11.857(3) _cell_length_c 12.847(3) _cell_angle_alpha 70.300(10) _cell_angle_beta 77.64(2) _cell_angle_gamma 86.96(3) _cell_volume 1545.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method ? _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 2.015 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5606 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5302 _reflns_number_observed 4429 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+2.4644P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5300 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_obs 0.0370 _refine_ls_wR_factor_all 0.0944 _refine_ls_wR_factor_obs 0.0869 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.059 _refine_ls_shift/esd_max 0.173 _refine_ls_shift/esd_mean 0.010 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.06874(4) 0.34706(4) 0.05133(3) 0.01954(12) Uani 1 d . . Ni2 Ni -0.37730(4) 0.74626(4) 0.11347(3) 0.02121(12) Uani 1 d . . Cl1 Cl 0.12208(7) 0.57081(7) -0.00582(7) 0.0233(2) Uani 1 d . . Cl2 Cl 0.16514(7) 0.30886(8) -0.13121(7) 0.0243(2) Uani 1 d . . Cl3 Cl -0.39729(8) 0.86916(8) 0.21890(8) 0.0315(2) Uani 1 d . . N1 N 0.2351(3) 0.3095(2) 0.0888(2) 0.0218(6) Uani 1 d . . N2 N -0.3379(3) 0.7328(3) -0.0372(2) 0.0235(6) Uani 1 d . . N3 N 0.0295(3) 0.3289(3) 0.2319(2) 0.0247(6) Uani 1 d . . N4 N -0.0040(3) 0.1633(3) 0.1164(2) 0.0263(6) Uani 1 d . . N5 N -0.5615(3) 0.7768(3) 0.0616(3) 0.0285(7) Uani 1 d . . N6 N -0.4539(3) 0.5817(3) 0.2196(2) 0.0276(7) Uani 1 d . . C1 C 0.2529(3) 0.3090(3) 0.1891(3) 0.0243(7) Uani 1 d . . C2 C 0.3696(3) 0.2643(3) 0.2039(3) 0.0272(8) Uani 1 d . . H2 H 0.4055(3) 0.2535(3) 0.2658(3) 0.038(11) Uiso 1 calc R . C3 C -0.4203(3) 0.7604(3) -0.1054(3) 0.0246(7) Uani 1 d . . C4 C 0.1485(3) 0.3572(3) 0.2561(3) 0.0275(8) Uani 1 d . . H4A H 0.1476(3) 0.3211(3) 0.3361(3) 0.031(7) Uiso 1 calc R . H4B H 0.1589(3) 0.4432(3) 0.2354(3) 0.031(7) Uiso 1 calc R . C5 C -0.0673(4) 0.4059(3) 0.2676(3) 0.0331(9) Uani 1 d . . H5A H -0.0483(12) 0.4879(4) 0.2213(14) 0.040(6) Uiso 1 calc R . H5B H -0.0710(15) 0.3973(16) 0.3453(7) 0.040(6) Uiso 1 calc R . H5C H -0.1460(5) 0.3829(14) 0.2596(19) 0.040(6) Uiso 1 calc R . C6 C -0.0051(4) 0.2002(3) 0.2940(3) 0.0309(8) Uani 1 d . . H6A H -0.0546(4) 0.1915(3) 0.3686(3) 0.035(5) Uiso 1 calc R . H6B H 0.0693(4) 0.1539(3) 0.3033(3) 0.035(5) Uiso 1 calc R . C7 C -0.0785(3) 0.1529(3) 0.2297(3) 0.0324(8) Uani 1 d . . H7A H -0.1018(3) 0.0695(3) 0.2716(3) 0.035(5) Uiso 1 calc R . H7B H -0.1539(3) 0.1980(3) 0.2219(3) 0.035(5) Uiso 1 calc R . C8 C -0.0867(4) 0.1375(3) 0.0497(3) 0.0340(9) Uani 1 d . . H8A H -0.0402(6) 0.1453(19) -0.0248(7) 0.031(4) Uiso 1 calc R . H8B H -0.1534(12) 0.1931(13) 0.0443(16) 0.031(4) Uiso 1 calc R . H8C H -0.1200(16) 0.0573(8) 0.0864(10) 0.031(4) Uiso 1 calc R . C9 C 0.0953(3) 0.0732(3) 0.1245(3) 0.0304(8) Uani 1 d . . H9A H 0.1420(13) 0.0812(13) 0.0501(3) 0.031(4) Uiso 1 calc R . H9B H 0.0586(4) -0.0058(3) 0.1596(17) 0.031(4) Uiso 1 calc R . H9C H 0.1494(12) 0.0858(13) 0.1691(16) 0.031(4) Uiso 1 calc R . C10 C -0.5392(3) 0.8143(4) -0.0636(3) 0.0328(9) Uani 1 d . . H10A H -0.5332(3) 0.9010(4) -0.0960(3) 0.043(8) Uiso 1 calc R . H10B H -0.6076(3) 0.7870(4) -0.0862(3) 0.043(8) Uiso 1 calc R . C11 C -0.6445(3) 0.8634(4) 0.1021(4) 0.0372(9) Uani 1 d . . H11A H -0.6557(20) 0.8407(14) 0.1827(4) 0.050(7) Uiso 1 calc R . H11B H -0.7234(9) 0.8629(18) 0.0822(20) 0.050(7) Uiso 1 calc R . H11C H -0.6077(12) 0.9424(5) 0.0673(17) 0.050(7) Uiso 1 calc R . C12 C -0.6191(3) 0.6534(3) 0.1111(3) 0.0325(8) Uani 1 d . . C13 C -0.5900(3) 0.5916(3) 0.2275(3) 0.0325(9) Uani 1 d . . H13A H -0.6242(3) 0.6370(3) 0.2768(3) 0.031(7) Uiso 1 calc R . H13B H -0.6284(3) 0.5122(3) 0.2600(3) 0.031(7) Uiso 1 calc R . C15 C -0.4037(4) 0.4862(3) 0.1737(4) 0.0366(9) Uani 1 d . . H15A H -0.4283(18) 0.4989(12) 0.1034(10) 0.038(5) Uiso 1 calc R . H15B H -0.4353(17) 0.4097(4) 0.2266(9) 0.038(5) Uiso 1 calc R . H15C H -0.3148(4) 0.4877(14) 0.1614(19) 0.038(5) Uiso 1 calc R . C14 C -0.4278(4) 0.5506(4) 0.3340(3) 0.0356(9) Uani 1 d . . H14A H -0.4560(20) 0.6134(10) 0.3644(9) 0.038(5) Uiso 1 calc R . H14B H -0.3401(4) 0.5414(21) 0.3298(4) 0.038(5) Uiso 1 calc R . H14C H -0.4702(18) 0.4769(12) 0.3822(6) 0.038(5) Uiso 1 calc R . C20 C -0.6224(4) 0.8604(4) 0.4542(4) 0.0487(11) Uani 1 d . . H20 H -0.5389(4) 0.8629(4) 0.4079(4) 0.052(13) Uiso 1 calc R . Cl20 Cl -0.69552(14) 0.72550(11) 0.47191(12) 0.0718(4) Uani 1 d . . Cl21 Cl -0.60787(13) 0.86657(15) 0.58613(11) 0.0723(4) Uani 1 d . . Cl22 Cl -0.7009(2) 0.98200(13) 0.38561(15) 0.1015(7) Uani 1 d . . C50 C 0.1615(5) 0.2794(4) -0.3954(4) 0.0595(14) Uani 1 d . . H50 H 0.1906(5) 0.2679(4) -0.3256(4) 0.048(12) Uiso 1 calc R 1 Cl50 Cl 0.2275(4) 0.1737(2) -0.4528(2) 0.0863(9) Uani 0.70 d P 1 Cl51 Cl 0.1902(10) 0.4274(7) -0.4822(6) 0.066(2) Uani 0.70 d P 1 Cl52 Cl -0.0045(4) 0.2556(4) -0.3606(4) 0.113(2) Uani 0.70 d P 1 Cl53 Cl 0.3051(6) 0.2389(7) -0.4914(4) 0.086(2) Uani 0.30 d P 2 Cl54 Cl 0.1573(22) 0.4290(15) -0.4749(16) 0.068(5) Uani 0.30 d P 2 Cl55 Cl 0.0495(12) 0.1978(8) -0.3885(9) 0.145(6) Uani 0.30 d P 2 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 0.0180(2) 0.0236(2) 0.0181(2) -0.0072(2) -0.0058(2) 0.0017(2) Ni2 0.0177(2) 0.0243(2) 0.0220(2) -0.0075(2) -0.0054(2) 0.0008(2) Cl1 0.0199(4) 0.0253(4) 0.0257(4) -0.0087(3) -0.0073(3) 0.0023(3) Cl2 0.0195(4) 0.0343(5) 0.0221(4) -0.0119(3) -0.0078(3) 0.0043(3) Cl3 0.0337(5) 0.0334(5) 0.0325(5) -0.0164(4) -0.0097(4) 0.0058(4) N1 0.0211(14) 0.0245(15) 0.0201(14) -0.0068(12) -0.0070(11) 0.0033(12) N2 0.0198(14) 0.028(2) 0.0230(14) -0.0075(12) -0.0078(12) 0.0011(12) N3 0.026(2) 0.028(2) 0.0186(14) -0.0070(12) -0.0044(12) 0.0032(12) N4 0.0222(15) 0.027(2) 0.030(2) -0.0098(13) -0.0070(12) 0.0018(12) N5 0.0207(15) 0.032(2) 0.035(2) -0.0127(13) -0.0077(13) 0.0039(13) N6 0.0221(15) 0.029(2) 0.029(2) -0.0072(13) -0.0039(12) -0.0014(12) C1 0.029(2) 0.025(2) 0.020(2) -0.0056(14) -0.0093(14) -0.0031(15) C2 0.028(2) 0.031(2) 0.024(2) -0.0054(15) -0.0150(15) -0.002(2) C3 0.023(2) 0.024(2) 0.027(2) -0.0037(14) -0.0126(14) 0.0003(14) C4 0.032(2) 0.032(2) 0.021(2) -0.0101(15) -0.0094(15) 0.001(2) C5 0.036(2) 0.038(2) 0.023(2) -0.011(2) -0.002(2) 0.008(2) C6 0.034(2) 0.029(2) 0.023(2) -0.0023(15) -0.002(2) 0.004(2) C7 0.028(2) 0.030(2) 0.032(2) -0.005(2) 0.001(2) -0.004(2) C8 0.030(2) 0.031(2) 0.046(2) -0.016(2) -0.011(2) -0.003(2) C9 0.031(2) 0.023(2) 0.036(2) -0.008(2) -0.007(2) 0.003(2) C10 0.025(2) 0.037(2) 0.037(2) -0.008(2) -0.015(2) 0.005(2) C11 0.023(2) 0.046(2) 0.048(2) -0.022(2) -0.012(2) 0.011(2) C12 0.024(2) 0.036(2) 0.038(2) -0.009(2) -0.009(2) -0.007(2) C13 0.022(2) 0.036(2) 0.038(2) -0.012(2) -0.002(2) -0.004(2) C15 0.034(2) 0.027(2) 0.047(2) -0.012(2) -0.006(2) -0.002(2) C14 0.035(2) 0.036(2) 0.028(2) 0.000(2) -0.007(2) -0.002(2) C20 0.047(3) 0.041(2) 0.040(2) 0.000(2) 0.003(2) 0.003(2) Cl20 0.0808(10) 0.0469(7) 0.0682(9) -0.0161(6) 0.0233(7) -0.0120(7) Cl21 0.0618(8) 0.1021(11) 0.0433(7) -0.0128(7) -0.0084(6) -0.0003(8) Cl22 0.176(2) 0.0548(8) 0.0923(11) -0.0244(8) -0.0793(13) 0.0524(11) C50 0.094(4) 0.050(3) 0.043(3) -0.013(2) -0.035(3) -0.002(3) Cl50 0.161(3) 0.0567(13) 0.0552(14) -0.0227(11) -0.053(2) 0.0314(15) Cl51 0.106(5) 0.056(3) 0.038(2) -0.007(2) -0.020(2) -0.033(3) Cl52 0.087(2) 0.113(3) 0.111(3) 0.014(2) -0.033(2) -0.042(2) Cl53 0.111(5) 0.120(5) 0.049(3) -0.049(3) -0.047(3) 0.082(4) Cl54 0.114(13) 0.040(5) 0.068(6) -0.034(5) -0.032(6) 0.013(6) Cl55 0.212(14) 0.099(7) 0.101(7) 0.051(5) -0.095(9) -0.105(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.987(3) . ? Ni1 N4 2.182(3) . ? Ni1 N3 2.205(3) . ? Ni1 Cl1 2.3775(12) 2_565 ? Ni1 Cl2 2.5364(11) . ? Ni1 Cl1 2.5674(12) . ? Ni2 N2 1.950(3) . ? Ni2 N6 2.066(3) . ? Ni2 N5 2.246(3) . ? Ni2 Cl3 2.2749(11) . ? Ni2 Cl2 2.4349(12) 2_565 ? Cl1 Ni1 2.3775(12) 2_565 ? Cl2 Ni2 2.4350(12) 2_565 ? N1 C1 1.342(4) . ? N1 N2 1.349(4) 2_565 ? N2 N1 1.349(4) 2_565 ? N2 C3 1.349(4) . ? N3 C5 1.468(4) . ? N3 C4 1.491(4) . ? N3 C6 1.491(4) . ? N4 C7 1.478(5) . ? N4 C9 1.484(4) . ? N4 C8 1.485(5) . ? N5 C10 1.486(5) . ? N5 C11 1.490(5) . ? N5 C12 1.500(5) . ? N6 C15 1.477(5) . ? N6 C14 1.478(5) . ? N6 C13 1.485(4) . ? C1 C2 1.394(5) . ? C1 C4 1.494(5) . ? C2 C3 1.389(5) 2_565 ? C3 C2 1.389(5) 2_565 ? C3 C10 1.503(5) . ? C6 C7 1.518(5) . ? C12 C13 1.523(5) . ? C20 Cl22 1.716(4) . ? C20 Cl20 1.753(5) . ? C20 Cl21 1.762(5) . ? C50 Cl55 1.580(10) . ? C50 Cl50 1.715(6) . ? C50 Cl54 1.73(2) . ? C50 Cl51 1.735(9) . ? C50 Cl52 1.805(7) . ? C50 Cl53 1.935(8) . ? 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 N1 Ni1 N4 96.98(11) . . ? N1 Ni1 N3 78.25(11) . . ? N4 Ni1 N3 83.13(11) . . ? N1 Ni1 Cl1 169.09(8) . 2_565 ? N4 Ni1 Cl1 93.22(8) . 2_565 ? N3 Ni1 Cl1 99.22(8) . 2_565 ? N1 Ni1 Cl2 85.20(8) . . ? N4 Ni1 Cl2 87.35(8) . . ? N3 Ni1 Cl2 159.70(8) . . ? Cl1 Ni1 Cl2 99.18(4) 2_565 . ? N1 Ni1 Cl1 88.84(9) . . ? N4 Ni1 Cl1 170.77(8) . . ? N3 Ni1 Cl1 91.10(8) . . ? Cl1 Ni1 Cl1 80.57(4) 2_565 . ? Cl2 Ni1 Cl1 100.31(4) . . ? N2 Ni2 N6 105.21(12) . . ? N2 Ni2 N5 77.45(11) . . ? N6 Ni2 N5 84.68(12) . . ? N2 Ni2 Cl3 147.02(9) . . ? N6 Ni2 Cl3 107.11(9) . . ? N5 Ni2 Cl3 99.08(8) . . ? N2 Ni2 Cl2 88.64(9) . 2_565 ? N6 Ni2 Cl2 94.74(9) . 2_565 ? N5 Ni2 Cl2 165.36(8) . 2_565 ? Cl3 Ni2 Cl2 95.07(4) . 2_565 ? Ni1 Cl1 Ni1 99.43(4) 2_565 . ? Ni2 Cl2 Ni1 104.23(4) 2_565 . ? C1 N1 N2 108.2(3) . 2_565 ? C1 N1 Ni1 119.5(2) . . ? N2 N1 Ni1 131.8(2) 2_565 . ? N1 N2 C3 108.6(3) 2_565 . ? N1 N2 Ni2 129.3(2) 2_565 . ? C3 N2 Ni2 122.0(2) . . ? C5 N3 C4 108.8(3) . . ? C5 N3 C6 110.4(3) . . ? C4 N3 C6 109.7(3) . . ? C5 N3 Ni1 116.2(2) . . ? C4 N3 Ni1 106.2(2) . . ? C6 N3 Ni1 105.3(2) . . ? C7 N4 C9 110.9(3) . . ? C7 N4 C8 108.2(3) . . ? C9 N4 C8 107.2(3) . . ? C7 N4 Ni1 103.4(2) . . ? C9 N4 Ni1 112.8(2) . . ? C8 N4 Ni1 114.2(2) . . ? C10 N5 C11 109.8(3) . . ? C10 N5 C12 108.9(3) . . ? C11 N5 C12 110.6(3) . . ? C10 N5 Ni2 108.5(2) . . ? C11 N5 Ni2 116.6(2) . . ? C12 N5 Ni2 102.1(2) . . ? C15 N6 C14 107.8(3) . . ? C15 N6 C13 111.2(3) . . ? C14 N6 C13 109.1(3) . . ? C15 N6 Ni2 110.5(2) . . ? C14 N6 Ni2 112.1(2) . . ? C13 N6 Ni2 106.3(2) . . ? N1 C1 C2 109.6(3) . . ? N1 C1 C4 115.0(3) . . ? C2 C1 C4 135.3(3) . . ? C3 C2 C1 104.4(3) 2_565 . ? N2 C3 C2 109.2(3) . 2_565 ? N2 C3 C10 116.0(3) . . ? C2 C3 C10 134.7(3) 2_565 . ? N3 C4 C1 108.7(3) . . ? N3 C6 C7 110.4(3) . . ? N4 C7 C6 110.5(3) . . ? N5 C10 C3 108.6(3) . . ? N5 C12 C13 109.5(3) . . ? N6 C13 C12 110.6(3) . . ? Cl22 C20 Cl20 111.5(3) . . ? Cl22 C20 Cl21 110.5(3) . . ? Cl20 C20 Cl21 110.3(2) . . ? Cl55 C50 Cl54 116.3(9) . . ? Cl50 C50 Cl51 115.6(4) . . ? Cl50 C50 Cl52 108.1(3) . . ? Cl51 C50 Cl52 106.9(5) . . ? Cl55 C50 Cl53 107.3(6) . . ? Cl54 C50 Cl53 97.3(8) . . ? _refine_diff_density_max 0.715 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.078 #=END data_2b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15H31Cl3N6Ni2*CH2Cl2' _chemical_formula_weight 604.1 _chemical_melting_point ? _chemical_compound_source ? 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' '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 'C2/c 1 CH' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.950(3) _cell_length_b 13.374(2) _cell_length_c 13.277(2) _cell_angle_alpha 90.00 _cell_angle_beta 130.700(10) _cell_angle_gamma 90.00 _cell_volume 2416.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method ? _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.127 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2262 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.25 _reflns_number_total 2191 _reflns_number_observed 1966 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0370P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2188 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_obs 0.0440 _refine_ls_wR_factor_all 0.1395 _refine_ls_wR_factor_obs 0.1314 _refine_ls_goodness_of_fit_all 2.455 _refine_ls_goodness_of_fit_obs 2.451 _refine_ls_restrained_S_all 2.455 _refine_ls_restrained_S_obs 2.451 _refine_ls_shift/esd_max -0.016 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.35951(4) 0.80032(4) 0.17364(6) 0.0152(2) Uani 1 d . . Cl1 Cl 0.5000 0.68632(11) 0.2500 0.0171(4) Uani 1 d S . Cl2 Cl 0.23238(8) 0.67781(8) 0.07699(11) 0.0193(3) Uani 1 d . . Cl3 Cl 0.40002(14) 0.3533(2) 0.2009(2) 0.0645(6) Uani 1 d . . N1 N 0.4503(3) 0.9102(3) 0.2175(4) 0.0156(8) Uani 1 d . . N2 N 0.2812(3) 0.9323(3) 0.1617(4) 0.0173(8) Uani 1 d . . N3 N 0.4024(3) 0.7852(3) 0.3673(4) 0.0200(9) Uani 1 d . . C1 C 0.4226(3) 1.0052(3) 0.2016(4) 0.0169(10) Uani 1 d . . C2 C 0.3138(3) 1.0185(3) 0.1283(5) 0.0214(10) Uani 1 d . . H2A H 0.3031(3) 1.0806(3) 0.1550(5) 0.042(12) Uiso 1 calc R . H2B H 0.2766(3) 1.0209(3) 0.0332(5) 0.042(12) Uiso 1 calc R . C3 C 0.3141(4) 0.9446(4) 0.2964(5) 0.0247(11) Uani 1 d . . H3A H 0.2655(4) 0.9825(4) 0.2910(5) 0.022(7) Uiso 1 calc R . H3B H 0.3755(4) 0.9813(4) 0.3521(5) 0.022(7) Uiso 1 calc R . C4 C 0.3281(3) 0.8441(4) 0.3570(5) 0.0224(11) Uani 1 d . . H4A H 0.3490(3) 0.8528(4) 0.4447(5) 0.022(7) Uiso 1 calc R . H4B H 0.2661(3) 0.8082(4) 0.3027(5) 0.022(7) Uiso 1 calc R . C5 C 0.5000 1.0684(5) 0.2500 0.0172(14) Uani 1 d S . C6 C 0.1723(3) 0.9258(4) 0.0624(5) 0.0221(11) Uani 1 d . . H6A H 0.1505(3) 0.8738(16) 0.0876(17) 0.028(5) Uiso 1 calc R . H6B H 0.1516(3) 0.9109(23) -0.0234(7) 0.028(5) Uiso 1 calc R . H6C H 0.1445(3) 0.9884(8) 0.0586(22) 0.028(5) Uiso 1 calc R . C7 C 0.5012(3) 0.8246(4) 0.4733(5) 0.0230(11) Uani 1 d . . H7A H 0.5486(4) 0.7848(14) 0.4798(21) 0.028(5) Uiso 1 calc R . H7B H 0.5147(9) 0.8224(22) 0.5562(7) 0.028(5) Uiso 1 calc R . H7C H 0.5048(7) 0.8925(8) 0.4534(16) 0.028(5) Uiso 1 calc R . C8 C 0.3992(4) 0.6810(4) 0.4008(5) 0.0265(12) Uani 1 d . . H8A H 0.3348(8) 0.6539(8) 0.3328(16) 0.028(5) Uiso 1 calc R . H8B H 0.4138(23) 0.6795(4) 0.4844(16) 0.028(5) Uiso 1 calc R . H8C H 0.4469(16) 0.6419(6) 0.4070(31) 0.028(5) Uiso 1 calc R . C9 C 0.5000 0.4268(6) 0.2500 0.101(6) Uani 1 d S . H5 H 0.5000 1.1445(70) 0.2500 0.050 Uiso 1 d S . H9 H 0.5333 0.4698 0.3325 0.070 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0181(4) 0.0124(4) 0.0178(4) -0.0010(2) 0.0130(3) -0.0006(2) Cl1 0.0153(7) 0.0131(8) 0.0205(8) 0.000 0.0106(7) 0.000 Cl2 0.0200(6) 0.0186(6) 0.0199(6) -0.0024(4) 0.0134(5) -0.0038(4) Cl3 0.0519(11) 0.096(2) 0.0570(11) 0.0276(11) 0.0404(10) 0.0297(11) N1 0.016(2) 0.013(2) 0.018(2) 0.001(2) 0.011(2) 0.003(2) N2 0.012(2) 0.020(2) 0.015(2) 0.000(2) 0.006(2) 0.002(2) N3 0.023(2) 0.022(2) 0.021(2) 0.000(2) 0.017(2) -0.001(2) C1 0.019(2) 0.014(2) 0.018(2) 0.003(2) 0.012(2) 0.004(2) C2 0.023(3) 0.013(2) 0.027(3) -0.001(2) 0.016(2) 0.001(2) C3 0.028(3) 0.026(3) 0.026(3) -0.007(2) 0.020(2) 0.000(2) C4 0.021(2) 0.029(3) 0.022(2) -0.008(2) 0.015(2) -0.007(2) C5 0.014(3) 0.014(3) 0.013(3) 0.000 0.004(3) 0.000 C6 0.005(2) 0.025(3) 0.021(2) -0.002(2) 0.002(2) 0.004(2) C7 0.015(2) 0.036(3) 0.015(2) 0.000(2) 0.009(2) 0.000(2) C8 0.034(3) 0.026(3) 0.024(3) 0.004(2) 0.020(2) -0.002(2) C9 0.151(12) 0.009(4) 0.024(5) 0.000 0.005(6) 0.000 _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 N1 1.979(4) . ? Ni1 N3 2.160(4) . ? Ni1 N2 2.197(4) . ? Ni1 Cl2 2.3916(12) . ? Ni1 Cl1 2.5254(11) . ? Ni1 Cl2 2.5924(14) 7_565 ? Cl1 Ni1 2.5254(11) 2_655 ? Cl2 Ni1 2.5924(14) 7_565 ? Cl3 C9 1.757(5) . ? N1 C1 1.330(6) . ? N1 N1 1.385(7) 2_655 ? N2 C3 1.482(6) . ? N2 C6 1.485(5) . ? N2 C2 1.486(6) . ? N3 C7 1.466(6) . ? N3 C8 1.475(6) . ? N3 C4 1.477(6) . ? C1 C5 1.377(6) . ? C1 C2 1.521(6) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.501(7) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C1 1.377(6) 2_655 ? C5 H5 1.02(9) . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 Cl3 1.757(5) 2_655 ? C9 H9 1.017(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 N1 Ni1 N3 97.7(2) . . ? N1 Ni1 N2 77.87(14) . . ? N3 Ni1 N2 82.87(14) . . ? N1 Ni1 Cl2 168.85(11) . . ? N3 Ni1 Cl2 92.82(11) . . ? N2 Ni1 Cl2 99.79(10) . . ? N1 Ni1 Cl1 85.13(11) . . ? N3 Ni1 Cl1 88.75(11) . . ? N2 Ni1 Cl1 159.80(10) . . ? Cl2 Ni1 Cl1 98.94(5) . . ? N1 Ni1 Cl2 90.37(11) . 7_565 ? N3 Ni1 Cl2 166.74(11) . 7_565 ? N2 Ni1 Cl2 88.57(10) . 7_565 ? Cl2 Ni1 Cl2 78.63(4) . 7_565 ? Cl1 Ni1 Cl2 102.49(3) . 7_565 ? Ni1 Cl1 Ni1 105.73(6) 2_655 . ? Ni1 Cl2 Ni1 101.37(4) . 7_565 ? C1 N1 N1 107.2(3) . 2_655 ? C1 N1 Ni1 120.7(3) . . ? N1 N1 Ni1 131.46(11) 2_655 . ? C3 N2 C6 109.7(4) . . ? C3 N2 C2 110.5(4) . . ? C6 N2 C2 109.1(4) . . ? C3 N2 Ni1 105.6(3) . . ? C6 N2 Ni1 115.2(3) . . ? C2 N2 Ni1 106.7(3) . . ? C7 N3 C8 108.1(4) . . ? C7 N3 C4 110.6(4) . . ? C8 N3 C4 108.7(4) . . ? C7 N3 Ni1 112.2(3) . . ? C8 N3 Ni1 113.2(3) . . ? C4 N3 Ni1 103.9(3) . . ? N1 C1 C5 110.7(4) . . ? N1 C1 C2 113.9(4) . . ? C5 C1 C2 135.3(4) . . ? N2 C2 C1 108.0(4) . . ? N2 C2 H2A 110.1(2) . . ? C1 C2 H2A 110.1(2) . . ? N2 C2 H2B 110.1(2) . . ? C1 C2 H2B 110.1(3) . . ? H2A C2 H2B 108.4 . . ? N2 C3 C4 110.1(4) . . ? N2 C3 H3A 109.6(2) . . ? C4 C3 H3A 109.6(3) . . ? N2 C3 H3B 109.6(2) . . ? C4 C3 H3B 109.6(3) . . ? H3A C3 H3B 108.2 . . ? N3 C4 C3 110.6(4) . . ? N3 C4 H4A 109.5(2) . . ? C3 C4 H4A 109.5(2) . . ? N3 C4 H4B 109.5(2) . . ? C3 C4 H4B 109.5(3) . . ? H4A C4 H4B 108.1 . . ? C1 C5 C1 104.2(6) . 2_655 ? C1 C5 H5 127.9(3) . . ? C1 C5 H5 127.9(3) 2_655 . ? N2 C6 H6A 109.5(3) . . ? N2 C6 H6B 109.5(2) . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5(2) . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 H7A 109.5(2) . . ? N3 C7 H7B 109.5(2) . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5(3) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5(3) . . ? N3 C8 H8B 109.5(2) . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5(3) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Cl3 C9 Cl3 112.0(5) . 2_655 ? Cl3 C9 H9 117.18(9) . . ? Cl3 C9 H9 100.14(11) 2_655 . ? 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 N1 Ni1 Cl1 Ni1 2.01(11) . . . 2_655 ? N3 Ni1 Cl1 Ni1 -95.80(10) . . . 2_655 ? N2 Ni1 Cl1 Ni1 -30.6(3) . . . 2_655 ? Cl2 Ni1 Cl1 Ni1 171.54(4) . . . 2_655 ? Cl2 Ni1 Cl1 Ni1 91.31(3) 7_565 . . 2_655 ? N1 Ni1 Cl2 Ni1 9.7(6) . . . 7_565 ? N3 Ni1 Cl2 Ni1 169.77(11) . . . 7_565 ? N2 Ni1 Cl2 Ni1 86.53(11) . . . 7_565 ? Cl1 Ni1 Cl2 Ni1 -101.05(4) . . . 7_565 ? Cl2 Ni1 Cl2 Ni1 0.0 7_565 . . 7_565 ? N3 Ni1 N1 C1 -91.1(4) . . . . ? N2 Ni1 N1 C1 -10.1(4) . . . . ? Cl2 Ni1 N1 C1 68.9(7) . . . . ? Cl1 Ni1 N1 C1 -179.2(4) . . . . ? Cl2 Ni1 N1 C1 78.3(4) 7_565 . . . ? N3 Ni1 N1 N1 78.8(5) . . . 2_655 ? N2 Ni1 N1 N1 159.8(5) . . . 2_655 ? Cl2 Ni1 N1 N1 -121.2(6) . . . 2_655 ? Cl1 Ni1 N1 N1 -9.3(5) . . . 2_655 ? Cl2 Ni1 N1 N1 -111.8(5) 7_565 . . 2_655 ? N1 Ni1 N2 C3 -91.0(3) . . . . ? N3 Ni1 N2 C3 8.5(3) . . . . ? Cl2 Ni1 N2 C3 100.2(3) . . . . ? Cl1 Ni1 N2 C3 -57.7(5) . . . . ? Cl2 Ni1 N2 C3 178.4(3) 7_565 . . . ? N1 Ni1 N2 C6 147.9(3) . . . . ? N3 Ni1 N2 C6 -112.7(3) . . . . ? Cl2 Ni1 N2 C6 -21.0(3) . . . . ? Cl1 Ni1 N2 C6 -178.8(2) . . . . ? Cl2 Ni1 N2 C6 57.2(3) 7_565 . . . ? N1 Ni1 N2 C2 26.6(3) . . . . ? N3 Ni1 N2 C2 126.1(3) . . . . ? Cl2 Ni1 N2 C2 -142.3(3) . . . . ? Cl1 Ni1 N2 C2 59.9(4) . . . . ? Cl2 Ni1 N2 C2 -64.0(3) 7_565 . . . ? N1 Ni1 N3 C7 -22.3(3) . . . . ? N2 Ni1 N3 C7 -99.0(3) . . . . ? Cl2 Ni1 N3 C7 161.5(3) . . . . ? Cl1 Ni1 N3 C7 62.6(3) . . . . ? Cl2 Ni1 N3 C7 -149.2(4) 7_565 . . . ? N1 Ni1 N3 C8 -145.0(3) . . . . ? N2 Ni1 N3 C8 138.3(3) . . . . ? Cl2 Ni1 N3 C8 38.8(3) . . . . ? Cl1 Ni1 N3 C8 -60.1(3) . . . . ? Cl2 Ni1 N3 C8 88.1(6) 7_565 . . . ? N1 Ni1 N3 C4 97.2(3) . . . . ? N2 Ni1 N3 C4 20.5(3) . . . . ? Cl2 Ni1 N3 C4 -79.0(3) . . . . ? Cl1 Ni1 N3 C4 -177.9(3) . . . . ? Cl2 Ni1 N3 C4 -29.7(6) 7_565 . . . ? N1 N1 C1 C5 2.2(6) 2_655 . . . ? Ni1 N1 C1 C5 174.2(2) . . . . ? N1 N1 C1 C2 178.6(4) 2_655 . . . ? Ni1 N1 C1 C2 -9.3(6) . . . . ? C3 N2 C2 C1 76.8(4) . . . . ? C6 N2 C2 C1 -162.5(4) . . . . ? Ni1 N2 C2 C1 -37.5(4) . . . . ? N1 C1 C2 N2 32.4(6) . . . . ? C5 C1 C2 N2 -152.3(4) . . . . ? C6 N2 C3 C4 88.1(5) . . . . ? C2 N2 C3 C4 -151.6(4) . . . . ? Ni1 N2 C3 C4 -36.6(4) . . . . ? C7 N3 C4 C3 73.0(5) . . . . ? C8 N3 C4 C3 -168.5(4) . . . . ? Ni1 N3 C4 C3 -47.6(4) . . . . ? N2 C3 C4 N3 59.8(5) . . . . ? N1 C1 C5 C1 -0.9(2) . . . 2_655 ? C2 C1 C5 C1 -176.3(6) . . . 2_655 ? _refine_diff_density_max 1.361 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.118