Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Youhei Yamamoto' 'Takayoshi Suzuki' 'Sumio Kaizaki' _publ_contact_author_name 'Prof Sumio Kaizaki' _publ_contact_author_address ; Prof Sumio Kaizaki Department of Chemistry, Graduate School of Science Osaka University Toyonaka 560-0043 JAPAN ; _publ_contact_author_email 'KAIZAKI@CHEM.SCI.OSAKA-U.AC.JP' data_mnim2py _database_code_CSD 161343 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(2-(2-pyridyl)-4,4,5,5-tetramethylimidazpline-1-oxy)manganese(II) ; _chemical_name_common '[MnCl~2~(IM2py)~2~]' _chemical_melting_point '>300' _chemical_formula_moiety '(Mn Cl2 (C12 H16 N3 O)2)' _chemical_formula_sum 'C24 H32 Cl2 Mn N6 O2' _chemical_formula_weight 562.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' 0.3368 0.7283 '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 18.454(2) _cell_length_b 9.156(2) _cell_length_c 15.8346(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.856(8) _cell_angle_gamma 90.00 _cell_volume 2627.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.4 _cell_measurement_theta_max 14.9 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dak red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.49 _diffrn_reflns_number 3953 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.01 _reflns_number_total 3846 _reflns_number_gt 2240 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0435P)^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 3846 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Mn Mn 0.5000 0.16778(5) 0.7500 0.03314(13) Uani 1 2 d S . . Cl Cl 0.60393(4) -0.00244(7) 0.78378(4) 0.05599(19) Uani 1 1 d . . . O O 0.65592(12) 0.4806(3) 1.01829(11) 0.0796(7) Uani 1 1 d . . . N1 N 0.58241(10) 0.34848(19) 0.81681(11) 0.0339(4) Uani 1 1 d . . . N2 N 0.64205(11) 0.4446(2) 0.93978(12) 0.0466(5) Uani 1 1 d . . . N3 N 0.48249(9) 0.2009(2) 0.88900(11) 0.0344(4) Uani 1 1 d . . . C1 C 0.58500(12) 0.3581(2) 0.89866(13) 0.0346(5) Uani 1 1 d . . . C2 C 0.64093(12) 0.4445(3) 0.79269(14) 0.0391(5) Uani 1 1 d . . . C3 C 0.69355(13) 0.4759(3) 0.87975(15) 0.0424(5) Uani 1 1 d . . . C4 C 0.67806(16) 0.3691(3) 0.72714(18) 0.0635(8) Uani 1 1 d . . . H4A H 0.6898 0.2704 0.7450 0.077 Uiso 1 1 calc R . . H4B H 0.7225 0.4203 0.7225 0.077 Uiso 1 1 calc R . . H4C H 0.6454 0.3688 0.6723 0.077 Uiso 1 1 calc R . . C5 C 0.60145(16) 0.5812(3) 0.75239(18) 0.0611(8) Uani 1 1 d . . . H5A H 0.6367 0.6461 0.7348 0.071 Uiso 1 1 calc R . . H5B H 0.5778 0.6293 0.7938 0.071 Uiso 1 1 calc R . . H5C H 0.5650 0.5541 0.7032 0.071 Uiso 1 1 calc R . . C6 C 0.75648(16) 0.3659(4) 0.9010(2) 0.0686(8) Uani 1 1 d . . . H6A H 0.7371 0.2687 0.8921 0.080 Uiso 1 1 calc R . . H6B H 0.7803 0.3774 0.9600 0.080 Uiso 1 1 calc R . . H6C H 0.7915 0.3826 0.8643 0.080 Uiso 1 1 calc R . . C7 C 0.72242(17) 0.6305(3) 0.89357(19) 0.0660(8) Uani 1 1 d . . . H7A H 0.7489 0.6410 0.9515 0.079 Uiso 1 1 calc R . . H7B H 0.6818 0.6978 0.8836 0.079 Uiso 1 1 calc R . . H7C H 0.7549 0.6509 0.8543 0.079 Uiso 1 1 calc R . . C8 C 0.53260(12) 0.2804(2) 0.94253(13) 0.0351(5) Uani 1 1 d . . . C9 C 0.53605(14) 0.2834(3) 1.03068(15) 0.0486(6) Uani 1 1 d . . . H9 H 0.5720 0.3376 1.0663 0.058 Uiso 1 1 calc R . . C10 C 0.48410(15) 0.2029(3) 1.06452(15) 0.0511(6) Uani 1 1 d . . . H10 H 0.4852 0.2019 1.1235 0.061 Uiso 1 1 calc R . . C11 C 0.43187(13) 0.1260(3) 1.01055(15) 0.0449(6) Uani 1 1 d . . . H11 H 0.3959 0.0739 1.0318 0.053 Uiso 1 1 calc R . . C12 C 0.43304(13) 0.1262(3) 0.92360(15) 0.0421(5) Uani 1 1 d . . . H12 H 0.3976 0.0717 0.8873 0.050 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 Mn 0.0379(3) 0.0357(3) 0.0265(2) 0.000 0.00792(17) 0.000 Cl 0.0607(4) 0.0556(4) 0.0554(4) 0.0169(3) 0.0203(3) 0.0206(3) O 0.0854(15) 0.1171(18) 0.0365(10) -0.0241(11) 0.0117(10) -0.0494(14) N1 0.0352(9) 0.0367(10) 0.0313(8) 0.0008(7) 0.0102(7) -0.0046(8) N2 0.0478(11) 0.0564(13) 0.0354(10) -0.0069(9) 0.0070(8) -0.0155(10) N3 0.0346(9) 0.0406(10) 0.0291(8) 0.0020(7) 0.0088(7) -0.0014(8) C1 0.0350(11) 0.0384(12) 0.0301(9) -0.0027(8) 0.0057(8) -0.0050(9) C2 0.0430(12) 0.0404(12) 0.0366(11) 0.0012(9) 0.0142(9) -0.0106(10) C3 0.0378(12) 0.0468(13) 0.0423(12) 0.0017(10) 0.0071(10) -0.0103(10) C4 0.0646(18) 0.077(2) 0.0575(16) -0.0177(15) 0.0340(14) -0.0216(15) C5 0.0632(18) 0.0598(18) 0.0573(16) 0.0217(14) 0.0041(13) -0.0070(14) C6 0.0472(16) 0.079(2) 0.077(2) 0.0215(17) 0.0057(14) 0.0037(15) C7 0.0663(19) 0.0631(18) 0.0678(18) -0.0082(15) 0.0105(15) -0.0289(15) C8 0.0386(11) 0.0411(11) 0.0272(9) -0.0010(9) 0.0100(8) -0.0007(10) C9 0.0560(15) 0.0609(15) 0.0295(11) -0.0068(10) 0.0098(10) -0.0090(13) C10 0.0622(16) 0.0628(17) 0.0332(11) -0.0010(11) 0.0220(11) -0.0015(13) C11 0.0438(13) 0.0542(14) 0.0424(12) 0.0076(11) 0.0227(10) 0.0002(11) C12 0.0362(11) 0.0513(14) 0.0402(12) 0.0051(10) 0.0111(9) -0.0052(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn N3 2.3040(16) . ? Mn N3 2.3040(16) 2_656 ? Mn N1 2.3586(18) 2_656 ? Mn N1 2.3586(18) . ? Mn Cl 2.4509(8) . ? Mn Cl 2.4509(8) 2_656 ? O N2 1.265(2) . ? N1 C1 1.291(2) . ? N1 C2 1.497(3) . ? N2 C1 1.379(3) . ? N2 C3 1.493(3) . ? N3 C12 1.337(3) . ? N3 C8 1.345(3) . ? C1 C8 1.475(3) . ? C2 C4 1.514(3) . ? C2 C5 1.526(3) . ? C2 C3 1.556(3) . ? C3 C7 1.514(3) . ? C3 C6 1.526(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.385(3) . ? C9 C10 1.394(3) . ? C9 H9 0.9300 . ? C10 C11 1.358(4) . ? C10 H10 0.9300 . ? C11 C12 1.381(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 N3 Mn N3 164.89(9) . 2_656 ? N3 Mn N1 98.15(6) . 2_656 ? N3 Mn N1 70.97(6) 2_656 2_656 ? N3 Mn N1 70.97(6) . . ? N3 Mn N1 98.15(6) 2_656 . ? N1 Mn N1 90.91(9) 2_656 . ? N3 Mn Cl 96.88(5) . . ? N3 Mn Cl 92.71(5) 2_656 . ? N1 Mn Cl 162.92(4) 2_656 . ? N1 Mn Cl 86.34(5) . . ? N3 Mn Cl 92.71(5) . 2_656 ? N3 Mn Cl 96.88(5) 2_656 2_656 ? N1 Mn Cl 86.34(5) 2_656 2_656 ? N1 Mn Cl 162.92(4) . 2_656 ? Cl Mn Cl 101.03(4) . 2_656 ? C1 N1 C2 108.90(17) . . ? C1 N1 Mn 113.39(13) . . ? C2 N1 Mn 137.12(13) . . ? O N2 C1 127.5(2) . . ? O N2 C3 122.7(2) . . ? C1 N2 C3 109.29(17) . . ? C12 N3 C8 117.37(18) . . ? C12 N3 Mn 123.61(15) . . ? C8 N3 Mn 118.02(13) . . ? N1 C1 N2 113.20(18) . . ? N1 C1 C8 122.42(19) . . ? N2 C1 C8 124.36(18) . . ? N1 C2 C4 110.39(19) . . ? N1 C2 C5 106.13(19) . . ? C4 C2 C5 109.2(2) . . ? N1 C2 C3 104.02(17) . . ? C4 C2 C3 113.8(2) . . ? C5 C2 C3 112.8(2) . . ? N2 C3 C7 109.6(2) . . ? N2 C3 C6 106.4(2) . . ? C7 C3 C6 110.7(2) . . ? N2 C3 C2 99.37(17) . . ? C7 C3 C2 116.4(2) . . ? C6 C3 C2 113.3(2) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 122.8(2) . . ? N3 C8 C1 113.46(17) . . ? C9 C8 C1 123.7(2) . . ? C8 C9 C10 118.2(2) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 119.4(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? N3 C12 C11 123.3(2) . . ? N3 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? 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 N3 Mn N1 C1 10.45(15) . . . . ? N3 Mn N1 C1 179.65(15) 2_656 . . . ? N1 Mn N1 C1 108.75(16) 2_656 . . . ? Cl Mn N1 C1 -88.13(15) . . . . ? Cl Mn N1 C1 28.3(3) 2_656 . . . ? N3 Mn N1 C2 -179.6(2) . . . . ? N3 Mn N1 C2 -10.4(2) 2_656 . . . ? N1 Mn N1 C2 -81.3(2) 2_656 . . . ? Cl Mn N1 C2 81.8(2) . . . . ? Cl Mn N1 C2 -161.77(16) 2_656 . . . ? N3 Mn N3 C12 134.99(18) 2_656 . . . ? N1 Mn N3 C12 92.20(18) 2_656 . . . ? N1 Mn N3 C12 -179.65(19) . . . . ? Cl Mn N3 C12 -95.95(17) . . . . ? Cl Mn N3 C12 5.51(18) 2_656 . . . ? N3 Mn N3 C8 -56.76(15) 2_656 . . . ? N1 Mn N3 C8 -99.55(16) 2_656 . . . ? N1 Mn N3 C8 -11.40(15) . . . . ? Cl Mn N3 C8 72.31(16) . . . . ? Cl Mn N3 C8 173.76(15) 2_656 . . . ? C2 N1 C1 N2 -3.6(3) . . . . ? Mn N1 C1 N2 169.24(15) . . . . ? C2 N1 C1 C8 177.8(2) . . . . ? Mn N1 C1 C8 -9.4(3) . . . . ? O N2 C1 N1 175.8(3) . . . . ? C3 N2 C1 N1 -12.0(3) . . . . ? O N2 C1 C8 -5.6(4) . . . . ? C3 N2 C1 C8 166.6(2) . . . . ? C1 N1 C2 C4 139.1(2) . . . . ? Mn N1 C2 C4 -31.1(3) . . . . ? C1 N1 C2 C5 -102.6(2) . . . . ? Mn N1 C2 C5 87.1(2) . . . . ? C1 N1 C2 C3 16.7(2) . . . . ? Mn N1 C2 C3 -153.61(16) . . . . ? O N2 C3 C7 -44.2(3) . . . . ? C1 N2 C3 C7 143.1(2) . . . . ? O N2 C3 C6 75.5(3) . . . . ? C1 N2 C3 C6 -97.2(2) . . . . ? O N2 C3 C2 -166.7(2) . . . . ? C1 N2 C3 C2 20.6(2) . . . . ? N1 C2 C3 N2 -21.5(2) . . . . ? C4 C2 C3 N2 -141.7(2) . . . . ? C5 C2 C3 N2 93.1(2) . . . . ? N1 C2 C3 C7 -139.0(2) . . . . ? C4 C2 C3 C7 100.8(3) . . . . ? C5 C2 C3 C7 -24.4(3) . . . . ? N1 C2 C3 C6 91.0(2) . . . . ? C4 C2 C3 C6 -29.2(3) . . . . ? C5 C2 C3 C6 -154.4(2) . . . . ? C12 N3 C8 C9 2.2(3) . . . . ? Mn N3 C8 C9 -166.78(19) . . . . ? C12 N3 C8 C1 179.7(2) . . . . ? Mn N3 C8 C1 10.7(2) . . . . ? N1 C1 C8 N3 -0.4(3) . . . . ? N2 C1 C8 N3 -178.9(2) . . . . ? N1 C1 C8 C9 177.0(2) . . . . ? N2 C1 C8 C9 -1.5(4) . . . . ? N3 C8 C9 C10 -1.5(4) . . . . ? C1 C8 C9 C10 -178.7(2) . . . . ? C8 C9 C10 C11 -0.6(4) . . . . ? C9 C10 C11 C12 1.9(4) . . . . ? C8 N3 C12 C11 -0.8(3) . . . . ? Mn N3 C12 C11 167.49(18) . . . . ? C10 C11 C12 N3 -1.2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.289 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.058 #===END data_coim2py _database_code_CSD 161344 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(2-(2-pyridyl)-4,4,5,5-tetramethylimidazpline-1-oxy)cobalt(II) ; _chemical_name_common '[CoCl~2~(IM2py)~2~]' _chemical_melting_point 220 _chemical_formula_moiety '(Co Cl2 (C12 H16 N3 O)2)' _chemical_formula_sum 'C24 H32 Cl2 Co N6 O2' _chemical_formula_weight 566.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 18.5308(8) _cell_length_b 8.9969(5) _cell_length_c 15.9308(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.837(4) _cell_angle_gamma 90.00 _cell_volume 2599.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2807 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean '100 x 100 pixel' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2807 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2807 _reflns_number_gt 2028 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0529P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2807 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.0000 0.18060(4) 0.7500 0.03708(13) Uani 1 2 d S . . Cl Cl -0.10015(4) 0.00838(7) 0.70611(4) 0.0622(2) Uani 1 1 d . . . O O -0.15403(11) 0.4815(3) 0.48539(11) 0.0814(6) Uani 1 1 d . . . N1 N -0.07883(9) 0.35237(19) 0.68844(10) 0.0388(4) Uani 1 1 d . . . N2 N -0.13940(10) 0.4482(2) 0.56451(12) 0.0504(5) Uani 1 1 d . . . N3 N 0.01788(9) 0.19659(19) 0.61979(10) 0.0393(4) Uani 1 1 d . . . C1 C -0.08161(11) 0.3618(2) 0.60720(13) 0.0396(5) Uani 1 1 d . . . C2 C -0.13718(12) 0.4506(3) 0.71140(14) 0.0452(5) Uani 1 1 d . . . C3 C -0.19076(12) 0.4798(3) 0.62328(15) 0.0484(5) Uani 1 1 d . . . C4 C -0.17442(16) 0.3735(3) 0.77607(18) 0.0704(8) Uani 1 1 d . . . H4A H -0.1412 0.3707 0.8309 0.078 Uiso 1 1 calc R . . H4B H -0.1874 0.2739 0.7572 0.078 Uiso 1 1 calc R . . H4C H -0.2181 0.4272 0.7809 0.078 Uiso 1 1 calc R . . C5 C -0.09884(15) 0.5895(3) 0.75105(18) 0.0665(7) Uani 1 1 d . . . H5A H -0.0764 0.6394 0.7097 0.078 Uiso 1 1 calc R . . H5B H -0.0616 0.5631 0.8001 0.078 Uiso 1 1 calc R . . H5C H -0.1342 0.6543 0.7686 0.078 Uiso 1 1 calc R . . C6 C -0.25260(15) 0.3652(3) 0.6015(2) 0.0749(8) Uani 1 1 d . . . H6A H -0.2778 0.3778 0.5430 0.078 Uiso 1 1 calc R . . H6B H -0.2868 0.3787 0.6387 0.078 Uiso 1 1 calc R . . H6C H -0.2321 0.2669 0.6092 0.078 Uiso 1 1 calc R . . C7 C -0.22076(15) 0.6351(3) 0.6086(2) 0.0711(8) Uani 1 1 d . . . H7A H -0.2497 0.6431 0.5515 0.078 Uiso 1 1 calc R . . H7B H -0.1806 0.7045 0.6158 0.078 Uiso 1 1 calc R . . H7C H -0.2511 0.6569 0.6492 0.078 Uiso 1 1 calc R . . C8 C -0.02955(11) 0.2821(2) 0.56455(13) 0.0403(5) Uani 1 1 d . . . C9 C -0.02957(14) 0.2888(3) 0.47804(15) 0.0552(6) Uani 1 1 d . . . H9 H -0.0632 0.3484 0.4416 0.078 Uiso 1 1 calc R . . C10 C 0.02162(14) 0.2047(3) 0.44657(15) 0.0589(7) Uani 1 1 d . . . H10 H 0.0223 0.2060 0.3884 0.078 Uiso 1 1 calc R . . C11 C 0.07073(13) 0.1205(3) 0.50137(15) 0.0528(6) Uani 1 1 d . . . H11 H 0.1061 0.0652 0.4813 0.078 Uiso 1 1 calc R . . C12 C 0.06767(12) 0.1176(3) 0.58785(15) 0.0477(5) Uani 1 1 d . . . H12 H 0.1013 0.0590 0.6249 0.078 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 Co 0.0445(2) 0.0357(2) 0.0323(2) 0.000 0.01077(15) 0.000 Cl 0.0716(4) 0.0572(4) 0.0622(4) -0.0181(3) 0.0243(3) -0.0225(3) O 0.0932(14) 0.1094(17) 0.0402(10) 0.0204(10) 0.0104(9) 0.0373(12) N1 0.0461(9) 0.0388(10) 0.0334(9) -0.0004(7) 0.0128(7) 0.0044(7) N2 0.0561(11) 0.0576(12) 0.0376(10) 0.0081(9) 0.0100(8) 0.0138(9) N3 0.0413(9) 0.0433(10) 0.0346(9) -0.0061(8) 0.0105(7) -0.0005(7) C1 0.0452(11) 0.0394(12) 0.0348(11) 0.0043(9) 0.0092(8) 0.0025(8) C2 0.0502(12) 0.0471(13) 0.0421(12) 0.0009(10) 0.0184(9) 0.0110(10) C3 0.0488(12) 0.0509(14) 0.0469(13) -0.0007(11) 0.0130(10) 0.0083(10) C4 0.0767(18) 0.083(2) 0.0633(17) 0.0190(15) 0.0429(14) 0.0269(14) C5 0.0770(18) 0.0621(18) 0.0588(16) -0.0215(14) 0.0106(13) 0.0117(13) C6 0.0576(16) 0.082(2) 0.085(2) -0.0140(17) 0.0128(14) -0.0020(14) C7 0.0706(18) 0.0669(18) 0.0759(19) 0.0102(15) 0.0153(14) 0.0262(13) C8 0.0466(11) 0.0415(12) 0.0347(10) -0.0016(9) 0.0131(8) -0.0004(9) C9 0.0717(15) 0.0602(16) 0.0366(11) 0.0062(11) 0.0179(10) 0.0066(12) C10 0.0756(16) 0.0688(18) 0.0402(12) -0.0009(12) 0.0304(12) -0.0001(13) C11 0.0515(13) 0.0601(15) 0.0536(14) -0.0136(12) 0.0268(11) -0.0035(11) C12 0.0439(12) 0.0537(14) 0.0479(13) -0.0104(11) 0.0145(9) 0.0008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N3 2.1715(16) 2_556 ? Co N3 2.1716(16) . ? Co N1 2.2128(17) . ? Co N1 2.2128(17) 2_556 ? Co Cl 2.4087(6) . ? Co Cl 2.4087(6) 2_556 ? O N2 1.269(2) . ? N1 C1 1.287(3) . ? N1 C2 1.498(2) . ? N2 C1 1.384(3) . ? N2 C3 1.493(3) . ? N3 C12 1.344(3) . ? N3 C8 1.350(3) . ? C1 C8 1.475(3) . ? C2 C5 1.511(3) . ? C2 C4 1.520(3) . ? C2 C3 1.567(3) . ? C3 C7 1.504(3) . ? C3 C6 1.528(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.379(3) . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.356(4) . ? C10 H10 0.9300 . ? C11 C12 1.391(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 N3 Co N3 172.40(9) 2_556 . ? N3 Co N1 99.26(6) 2_556 . ? N3 Co N1 75.32(6) . . ? N3 Co N1 75.32(6) 2_556 2_556 ? N3 Co N1 99.26(6) . 2_556 ? N1 Co N1 91.40(9) . 2_556 ? N3 Co Cl 93.47(5) 2_556 . ? N3 Co Cl 91.42(5) . . ? N1 Co Cl 85.49(5) . . ? N1 Co Cl 167.76(4) 2_556 . ? N3 Co Cl 91.42(5) 2_556 2_556 ? N3 Co Cl 93.47(5) . 2_556 ? N1 Co Cl 167.75(4) . 2_556 ? N1 Co Cl 85.48(5) 2_556 2_556 ? Cl Co Cl 99.92(4) . 2_556 ? C1 N1 C2 108.93(17) . . ? C1 N1 Co 112.22(13) . . ? C2 N1 Co 138.36(13) . . ? O N2 C1 127.35(19) . . ? O N2 C3 122.95(19) . . ? C1 N2 C3 109.11(18) . . ? C12 N3 C8 117.40(18) . . ? C12 N3 Co 125.28(15) . . ? C8 N3 Co 117.00(13) . . ? N1 C1 N2 113.48(18) . . ? N1 C1 C8 122.42(19) . . ? N2 C1 C8 124.05(19) . . ? N1 C2 C5 106.80(18) . . ? N1 C2 C4 110.32(19) . . ? C5 C2 C4 109.5(2) . . ? N1 C2 C3 103.69(16) . . ? C5 C2 C3 113.1(2) . . ? C4 C2 C3 113.0(2) . . ? N2 C3 C7 110.0(2) . . ? N2 C3 C6 105.9(2) . . ? C7 C3 C6 110.8(2) . . ? N2 C3 C2 99.30(16) . . ? C7 C3 C2 116.2(2) . . ? C6 C3 C2 113.5(2) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 122.88(19) . . ? N3 C8 C1 112.13(17) . . ? C9 C8 C1 125.0(2) . . ? C8 C9 C10 118.6(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.4(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.3(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N3 C12 C11 122.4(2) . . ? N3 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? 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 N3 Co N1 C1 -177.24(15) 2_556 . . . ? N3 Co N1 C1 8.21(14) . . . . ? N1 Co N1 C1 107.41(16) 2_556 . . . ? Cl Co N1 C1 -84.45(14) . . . . ? Cl Co N1 C1 32.4(3) 2_556 . . . ? N3 Co N1 C2 -6.5(2) 2_556 . . . ? N3 Co N1 C2 179.0(2) . . . . ? N1 Co N1 C2 -81.8(2) 2_556 . . . ? Cl Co N1 C2 86.3(2) . . . . ? Cl Co N1 C2 -156.86(19) 2_556 . . . ? N3 Co N3 C12 134.07(17) 2_556 . . . ? N1 Co N3 C12 179.16(18) . . . . ? N1 Co N3 C12 90.14(18) 2_556 . . . ? Cl Co N3 C12 -95.88(17) . . . . ? Cl Co N3 C12 4.15(17) 2_556 . . . ? N3 Co N3 C8 -52.62(15) 2_556 . . . ? N1 Co N3 C8 -7.53(15) . . . . ? N1 Co N3 C8 -96.55(15) 2_556 . . . ? Cl Co N3 C8 77.43(15) . . . . ? Cl Co N3 C8 177.46(15) 2_556 . . . ? C2 N1 C1 N2 -4.5(3) . . . . ? Co N1 C1 N2 169.00(15) . . . . ? C2 N1 C1 C8 177.91(19) . . . . ? Co N1 C1 C8 -8.6(3) . . . . ? O N2 C1 N1 177.2(2) . . . . ? C3 N2 C1 N1 -11.5(3) . . . . ? O N2 C1 C8 -5.3(4) . . . . ? C3 N2 C1 C8 166.0(2) . . . . ? C1 N1 C2 C5 -102.1(2) . . . . ? Co N1 C2 C5 86.9(2) . . . . ? C1 N1 C2 C4 138.9(2) . . . . ? Co N1 C2 C4 -32.0(3) . . . . ? C1 N1 C2 C3 17.6(2) . . . . ? Co N1 C2 C3 -153.36(16) . . . . ? O N2 C3 C7 -45.1(3) . . . . ? C1 N2 C3 C7 143.1(2) . . . . ? O N2 C3 C6 74.7(3) . . . . ? C1 N2 C3 C6 -97.0(2) . . . . ? O N2 C3 C2 -167.5(2) . . . . ? C1 N2 C3 C2 20.7(2) . . . . ? N1 C2 C3 N2 -22.1(2) . . . . ? C5 C2 C3 N2 93.2(2) . . . . ? C4 C2 C3 N2 -141.6(2) . . . . ? N1 C2 C3 C7 -139.9(2) . . . . ? C5 C2 C3 C7 -24.6(3) . . . . ? C4 C2 C3 C7 100.6(3) . . . . ? N1 C2 C3 C6 89.8(2) . . . . ? C5 C2 C3 C6 -154.8(2) . . . . ? C4 C2 C3 C6 -29.6(3) . . . . ? C12 N3 C8 C9 1.3(3) . . . . ? Co N3 C8 C9 -172.58(18) . . . . ? C12 N3 C8 C1 179.50(18) . . . . ? Co N3 C8 C1 5.6(2) . . . . ? N1 C1 C8 N3 2.3(3) . . . . ? N2 C1 C8 N3 -175.0(2) . . . . ? N1 C1 C8 C9 -179.5(2) . . . . ? N2 C1 C8 C9 3.2(4) . . . . ? N3 C8 C9 C10 -0.4(4) . . . . ? C1 C8 C9 C10 -178.4(2) . . . . ? C8 C9 C10 C11 -1.0(4) . . . . ? C9 C10 C11 C12 1.4(4) . . . . ? C8 N3 C12 C11 -0.8(3) . . . . ? Co N3 C12 C11 172.46(16) . . . . ? C10 C11 C12 N3 -0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.423 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.072 #===END data_niim2py _database_code_CSD 161345 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(2-(2-pyridyl)-4,4,5,5-tetramethylimidazpline-1-oxy)nickel(II) ; _chemical_name_common '[NiCl~2~(IM2py)~2~]' _chemical_melting_point '>280' _chemical_formula_moiety '(Ni Cl2 (C12 H16 N3 O)2)' _chemical_formula_sum 'C24 H32 Cl2 N6 Ni O2' _chemical_formula_weight 566.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 18.6043(12) _cell_length_b 8.9489(6) _cell_length_c 15.9286(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.633(3) _cell_angle_gamma 90.00 _cell_volume 2587.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2815 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean '100 x 100 pixel' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2815 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2815 _reflns_number_gt 2377 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0545P)^2^+0.0784P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2815 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.18458(3) 0.7500 0.03085(11) Uani 1 2 d S . . Cl Cl 0.40221(3) 0.00633(6) 0.70259(4) 0.05487(16) Uani 1 1 d . . . O O 0.34685(9) 0.4835(2) 0.48617(10) 0.0709(5) Uani 1 1 d . . . N1 N 0.42084(8) 0.35013(16) 0.69045(9) 0.0332(3) Uani 1 1 d . . . N2 N 0.36107(8) 0.44891(19) 0.56550(10) 0.0431(4) Uani 1 1 d . . . N3 N 0.51823(7) 0.19602(15) 0.62391(9) 0.0331(3) Uani 1 1 d . . . C1 C 0.41862(9) 0.36142(19) 0.60900(11) 0.0337(3) Uani 1 1 d . . . C2 C 0.36277(10) 0.4488(2) 0.71277(11) 0.0392(4) Uani 1 1 d . . . C3 C 0.30974(10) 0.4801(2) 0.62339(12) 0.0420(4) Uani 1 1 d . . . C4 C 0.32521(13) 0.3725(3) 0.77681(15) 0.0595(6) Uani 1 1 d . . . H4A H 0.2823 0.4284 0.7817 0.073 Uiso 1 1 calc R . . H4B H 0.3587 0.3677 0.8320 0.073 Uiso 1 1 calc R . . H4C H 0.3110 0.2731 0.7573 0.073 Uiso 1 1 calc R . . C5 C 0.40208(13) 0.5886(3) 0.75364(15) 0.0562(5) Uani 1 1 d . . . H5A H 0.4401 0.5610 0.8023 0.067 Uiso 1 1 calc R . . H5B H 0.3673 0.6532 0.7722 0.067 Uiso 1 1 calc R . . H5C H 0.4236 0.6400 0.7122 0.067 Uiso 1 1 calc R . . C6 C 0.24779(13) 0.3650(3) 0.59974(19) 0.0655(6) Uani 1 1 d . . . H6A H 0.2118 0.3823 0.6337 0.082 Uiso 1 1 calc R . . H6B H 0.2678 0.2663 0.6109 0.082 Uiso 1 1 calc R . . H6C H 0.2249 0.3743 0.5398 0.082 Uiso 1 1 calc R . . C7 C 0.27969(13) 0.6368(3) 0.60868(17) 0.0624(6) Uani 1 1 d . . . H7A H 0.3198 0.7063 0.6143 0.075 Uiso 1 1 calc R . . H7B H 0.2512 0.6597 0.6505 0.075 Uiso 1 1 calc R . . H7C H 0.2490 0.6441 0.5519 0.075 Uiso 1 1 calc R . . C8 C 0.47076(9) 0.28257(19) 0.56758(11) 0.0343(3) Uani 1 1 d . . . C9 C 0.47088(11) 0.2900(2) 0.48075(12) 0.0470(4) Uani 1 1 d . . . H9 H 0.4372 0.3500 0.4438 0.058 Uiso 1 1 calc R . . C10 C 0.52253(12) 0.2056(2) 0.44996(13) 0.0504(5) Uani 1 1 d . . . H10 H 0.5238 0.2075 0.3919 0.061 Uiso 1 1 calc R . . C11 C 0.57131(10) 0.1201(2) 0.50655(13) 0.0455(5) Uani 1 1 d . . . H11 H 0.6068 0.0643 0.4876 0.054 Uiso 1 1 calc R . . C12 C 0.56755(10) 0.1170(2) 0.59287(12) 0.0409(4) Uani 1 1 d . . . H12 H 0.6008 0.0573 0.6305 0.050 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 Ni 0.03727(17) 0.03074(17) 0.02591(16) 0.000 0.00991(11) 0.000 Cl 0.0654(3) 0.0499(3) 0.0544(3) -0.0172(2) 0.0241(2) -0.0207(2) O 0.0790(11) 0.0994(14) 0.0338(8) 0.0188(8) 0.0114(7) 0.0365(10) N1 0.0397(7) 0.0344(7) 0.0281(7) -0.0011(5) 0.0128(6) 0.0030(6) N2 0.0480(8) 0.0499(9) 0.0312(8) 0.0070(7) 0.0082(6) 0.0130(7) N3 0.0362(6) 0.0362(8) 0.0279(7) -0.0034(6) 0.0096(5) 0.0001(6) C1 0.0381(8) 0.0348(8) 0.0290(8) 0.0013(7) 0.0090(6) 0.0028(7) C2 0.0445(9) 0.0411(9) 0.0354(9) 0.0001(7) 0.0158(7) 0.0117(8) C3 0.0416(9) 0.0447(10) 0.0401(10) 0.0004(8) 0.0100(8) 0.0092(8) C4 0.0630(12) 0.0695(14) 0.0566(13) 0.0157(11) 0.0365(11) 0.0206(11) C5 0.0634(12) 0.0525(12) 0.0510(12) -0.0174(10) 0.0089(10) 0.0099(10) C6 0.0491(11) 0.0723(16) 0.0740(17) -0.0136(13) 0.0112(11) -0.0012(11) C7 0.0639(13) 0.0579(14) 0.0650(15) 0.0102(11) 0.0129(11) 0.0268(11) C8 0.0390(8) 0.0365(9) 0.0297(8) -0.0014(7) 0.0123(7) -0.0003(7) C9 0.0581(11) 0.0540(12) 0.0321(9) 0.0052(8) 0.0166(8) 0.0068(9) C10 0.0653(12) 0.0590(13) 0.0336(9) -0.0021(9) 0.0256(9) -0.0002(10) C11 0.0451(9) 0.0531(11) 0.0447(11) -0.0114(9) 0.0232(8) -0.0028(9) C12 0.0380(8) 0.0472(10) 0.0392(10) -0.0089(8) 0.0119(7) 0.0018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N3 2.1112(14) . ? Ni N3 2.1112(14) 2_656 ? Ni N1 2.1568(14) 2_656 ? Ni N1 2.1569(14) . ? Ni Cl 2.4132(5) 2_656 ? Ni Cl 2.4132(5) . ? O N2 1.271(2) . ? N1 C1 1.293(2) . ? N1 C2 1.497(2) . ? N2 C1 1.384(2) . ? N2 C3 1.492(2) . ? N3 C12 1.336(2) . ? N3 C8 1.356(2) . ? C1 C8 1.468(2) . ? C2 C4 1.519(3) . ? C2 C5 1.522(3) . ? C2 C3 1.570(2) . ? C3 C7 1.509(3) . ? C3 C6 1.530(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.385(2) . ? C9 C10 1.393(3) . ? C9 H9 0.9300 . ? C10 C11 1.365(3) . ? C10 H10 0.9300 . ? C11 C12 1.392(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 N3 Ni N3 174.44(8) . 2_656 ? N3 Ni N1 98.56(5) . 2_656 ? N3 Ni N1 77.56(5) 2_656 2_656 ? N3 Ni N1 77.56(5) . . ? N3 Ni N1 98.56(5) 2_656 . ? N1 Ni N1 93.24(8) 2_656 . ? N3 Ni Cl 93.60(4) . 2_656 ? N3 Ni Cl 90.07(4) 2_656 2_656 ? N1 Ni Cl 85.46(4) 2_656 2_656 ? N1 Ni Cl 170.80(4) . 2_656 ? N3 Ni Cl 90.07(4) . . ? N3 Ni Cl 93.60(4) 2_656 . ? N1 Ni Cl 170.80(4) 2_656 . ? N1 Ni Cl 85.46(4) . . ? Cl Ni Cl 97.24(3) 2_656 . ? C1 N1 C2 109.02(14) . . ? C1 N1 Ni 111.34(11) . . ? C2 N1 Ni 139.41(11) . . ? O N2 C1 127.27(16) . . ? O N2 C3 123.12(15) . . ? C1 N2 C3 109.04(14) . . ? C12 N3 C8 117.27(15) . . ? C12 N3 Ni 126.34(13) . . ? C8 N3 Ni 116.13(10) . . ? N1 C1 N2 113.46(15) . . ? N1 C1 C8 122.29(15) . . ? N2 C1 C8 124.19(15) . . ? N1 C2 C4 110.88(16) . . ? N1 C2 C5 106.39(15) . . ? C4 C2 C5 109.33(18) . . ? N1 C2 C3 103.48(13) . . ? C4 C2 C3 113.53(16) . . ? C5 C2 C3 112.87(16) . . ? N2 C3 C7 110.10(18) . . ? N2 C3 C6 105.73(17) . . ? C7 C3 C6 110.72(18) . . ? N2 C3 C2 99.60(13) . . ? C7 C3 C2 116.43(17) . . ? C6 C3 C2 113.14(18) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 123.05(16) . . ? N3 C8 C1 112.09(14) . . ? C9 C8 C1 124.83(16) . . ? C8 C9 C10 118.50(18) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 118.79(18) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 119.58(18) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N3 C12 C11 122.80(18) . . ? N3 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? 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 N3 Ni N1 C1 6.65(12) . . . . ? N3 Ni N1 C1 -177.40(12) 2_656 . . . ? N1 Ni N1 C1 104.70(13) 2_656 . . . ? Cl Ni N1 C1 23.1(3) 2_656 . . . ? Cl Ni N1 C1 -84.43(12) . . . . ? N3 Ni N1 C2 -179.78(18) . . . . ? N3 Ni N1 C2 -3.82(18) 2_656 . . . ? N1 Ni N1 C2 -81.72(18) 2_656 . . . ? Cl Ni N1 C2 -163.32(19) 2_656 . . . ? Cl Ni N1 C2 89.14(18) . . . . ? N3 Ni N3 C12 133.93(15) 2_656 . . . ? N1 Ni N3 C12 88.56(15) 2_656 . . . ? N1 Ni N3 C12 -179.99(15) . . . . ? Cl Ni N3 C12 2.62(15) 2_656 . . . ? Cl Ni N3 C12 -94.65(15) . . . . ? N3 Ni N3 C8 -52.17(12) 2_656 . . . ? N1 Ni N3 C8 -97.53(12) 2_656 . . . ? N1 Ni N3 C8 -6.08(12) . . . . ? Cl Ni N3 C8 176.52(12) 2_656 . . . ? Cl Ni N3 C8 79.26(12) . . . . ? C2 N1 C1 N2 -5.0(2) . . . . ? Ni N1 C1 N2 170.62(12) . . . . ? C2 N1 C1 C8 177.58(16) . . . . ? Ni N1 C1 C8 -6.8(2) . . . . ? O N2 C1 N1 177.45(19) . . . . ? C3 N2 C1 N1 -11.0(2) . . . . ? O N2 C1 C8 -5.1(3) . . . . ? C3 N2 C1 C8 166.39(16) . . . . ? C1 N1 C2 C4 139.78(18) . . . . ? Ni N1 C2 C4 -33.9(3) . . . . ? C1 N1 C2 C5 -101.44(18) . . . . ? Ni N1 C2 C5 84.9(2) . . . . ? C1 N1 C2 C3 17.72(19) . . . . ? Ni N1 C2 C3 -155.95(14) . . . . ? O N2 C3 C7 -44.8(3) . . . . ? C1 N2 C3 C7 143.26(18) . . . . ? O N2 C3 C6 74.9(2) . . . . ? C1 N2 C3 C6 -97.1(2) . . . . ? O N2 C3 C2 -167.64(19) . . . . ? C1 N2 C3 C2 20.40(19) . . . . ? N1 C2 C3 N2 -22.01(18) . . . . ? C4 C2 C3 N2 -142.29(17) . . . . ? C5 C2 C3 N2 92.58(18) . . . . ? N1 C2 C3 C7 -140.25(18) . . . . ? C4 C2 C3 C7 99.5(2) . . . . ? C5 C2 C3 C7 -25.7(2) . . . . ? N1 C2 C3 C6 89.79(19) . . . . ? C4 C2 C3 C6 -30.5(2) . . . . ? C5 C2 C3 C6 -155.62(18) . . . . ? C12 N3 C8 C9 1.0(3) . . . . ? Ni N3 C8 C9 -173.50(15) . . . . ? C12 N3 C8 C1 178.95(15) . . . . ? Ni N3 C8 C1 4.47(18) . . . . ? N1 C1 C8 N3 1.9(2) . . . . ? N2 C1 C8 N3 -175.33(16) . . . . ? N1 C1 C8 C9 179.78(18) . . . . ? N2 C1 C8 C9 2.6(3) . . . . ? N3 C8 C9 C10 -0.5(3) . . . . ? C1 C8 C9 C10 -178.23(18) . . . . ? C8 C9 C10 C11 -0.6(3) . . . . ? C9 C10 C11 C12 1.2(3) . . . . ? C8 N3 C12 C11 -0.3(3) . . . . ? Ni N3 C12 C11 173.49(13) . . . . ? C10 C11 C12 N3 -0.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.463 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.074 #===END data_znim2py _database_code_CSD 161346 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(2-(2-pyridyl)-4,4,5,5-tetramethylimidazpline-1-oxy)zink(II) ; _chemical_name_common '[ZnCl~2~(IM2py)~2~]' _chemical_melting_point 155 _chemical_formula_moiety '(Zn Cl2 (C12 H16 N3 O)2)' _chemical_formula_sum 'C24 H32 Cl2 N6 O2 Zn' _chemical_formula_weight 572.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 18.550(3) _cell_length_b 9.1216(16) _cell_length_c 15.8060(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.460(10) _cell_angle_gamma 90.00 _cell_volume 2611.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details Coppens_numerical _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.11 _diffrn_reflns_number 3923 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.02 _reflns_number_total 3817 _reflns_number_gt 2632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0401P)^2^+1.5022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3817 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Zn Zn 0.5000 0.15857(4) 0.2500 0.03261(10) Uani 1 2 d S . . Cl Cl 0.39888(4) -0.00329(7) 0.20781(4) 0.05520(18) Uani 1 1 d . . . O O 0.34506(12) 0.4788(3) -0.01602(11) 0.0716(6) Uani 1 1 d . . . N1 N 0.41800(9) 0.34565(18) 0.18853(10) 0.0321(3) Uani 1 1 d . . . N2 N 0.35881(10) 0.4441(2) 0.06342(11) 0.0405(4) Uani 1 1 d . . . N3 N 0.51642(9) 0.19386(18) 0.11925(10) 0.0304(3) Uani 1 1 d . . . C1 C 0.41601(11) 0.3566(2) 0.10710(12) 0.0313(4) Uani 1 1 d . . . C2 C 0.35985(12) 0.4436(2) 0.21089(13) 0.0364(4) Uani 1 1 d . . . C3 C 0.30732(12) 0.4761(2) 0.12165(14) 0.0392(5) Uani 1 1 d . . . C4 C 0.32213(16) 0.3678(3) 0.27474(18) 0.0604(7) Uani 1 1 d . . . H4A H 0.2785 0.4214 0.2791 0.073 Uiso 1 1 calc R . . H4B H 0.3552 0.3640 0.3305 0.073 Uiso 1 1 calc R . . H4C H 0.3087 0.2700 0.2551 0.073 Uiso 1 1 calc R . . C5 C 0.40009(15) 0.5797(3) 0.25278(17) 0.0572(7) Uani 1 1 d . . . H5A H 0.4379 0.5512 0.3016 0.070 Uiso 1 1 calc R . . H5B H 0.3656 0.6435 0.2718 0.070 Uiso 1 1 calc R . . H5C H 0.4221 0.6300 0.2113 0.070 Uiso 1 1 calc R . . C6 C 0.24416(14) 0.3666(3) 0.0972(2) 0.0629(7) Uani 1 1 d . . . H6A H 0.2095 0.3813 0.1336 0.076 Uiso 1 1 calc R . . H6B H 0.2634 0.2686 0.1048 0.076 Uiso 1 1 calc R . . H6C H 0.2198 0.3809 0.0377 0.076 Uiso 1 1 calc R . . C7 C 0.27857(16) 0.6317(3) 0.10673(19) 0.0597(7) Uani 1 1 d . . . H7A H 0.3194 0.6988 0.1162 0.072 Uiso 1 1 calc R . . H7B H 0.2474 0.6535 0.1463 0.072 Uiso 1 1 calc R . . H7C H 0.2508 0.6414 0.0483 0.072 Uiso 1 1 calc R . . C8 C 0.46876(11) 0.2792(2) 0.06492(12) 0.0311(4) Uani 1 1 d . . . C9 C 0.46833(14) 0.2892(3) -0.02267(14) 0.0457(5) Uani 1 1 d . . . H9 H 0.4343 0.3485 -0.0590 0.055 Uiso 1 1 calc R . . C10 C 0.51994(14) 0.2085(3) -0.05487(15) 0.0479(6) Uani 1 1 d . . . H10 H 0.5203 0.2118 -0.1136 0.057 Uiso 1 1 calc R . . C11 C 0.57001(12) 0.1245(3) 0.00014(14) 0.0425(5) Uani 1 1 d . . . H11 H 0.6061 0.0725 -0.0200 0.051 Uiso 1 1 calc R . . C12 C 0.56612(11) 0.1182(2) 0.08676(13) 0.0366(4) Uani 1 1 d . . . H12 H 0.5995 0.0588 0.1239 0.045 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 Zn 0.04022(18) 0.03464(18) 0.02482(14) 0.000 0.01109(12) 0.000 Cl 0.0645(4) 0.0543(4) 0.0520(3) -0.0192(3) 0.0242(3) -0.0236(3) O 0.0824(14) 0.0996(16) 0.0332(8) 0.0216(9) 0.0132(9) 0.0457(12) N1 0.0365(8) 0.0352(8) 0.0266(7) 0.0015(7) 0.0113(6) 0.0070(7) N2 0.0433(10) 0.0486(11) 0.0298(8) 0.0057(8) 0.0084(7) 0.0142(8) N3 0.0305(8) 0.0354(8) 0.0262(7) -0.0031(6) 0.0083(6) -0.0001(6) C1 0.0344(9) 0.0332(10) 0.0269(8) 0.0015(7) 0.0080(7) 0.0046(8) C2 0.0393(11) 0.0386(11) 0.0336(10) 0.0001(8) 0.0126(8) 0.0105(9) C3 0.0354(11) 0.0420(12) 0.0407(11) 0.0001(9) 0.0089(9) 0.0102(9) C4 0.0620(16) 0.0741(19) 0.0561(14) 0.0188(13) 0.0369(13) 0.0252(14) C5 0.0633(16) 0.0542(15) 0.0514(14) -0.0202(12) 0.0061(12) 0.0094(13) C6 0.0438(14) 0.0718(19) 0.0723(18) -0.0170(15) 0.0107(13) -0.0037(13) C7 0.0629(17) 0.0542(16) 0.0619(16) 0.0062(12) 0.0134(13) 0.0263(13) C8 0.0348(10) 0.0348(10) 0.0252(8) 0.0004(7) 0.0101(7) 0.0013(8) C9 0.0551(13) 0.0556(14) 0.0295(10) 0.0081(9) 0.0163(9) 0.0110(11) C10 0.0602(14) 0.0571(14) 0.0327(10) 0.0013(10) 0.0240(10) 0.0024(12) C11 0.0414(12) 0.0518(13) 0.0398(11) -0.0095(9) 0.0207(9) 0.0010(10) C12 0.0341(10) 0.0438(11) 0.0331(9) -0.0057(8) 0.0102(8) 0.0048(8) _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 Zn N3 2.1769(15) . ? Zn N3 2.1769(15) 2_655 ? Zn N1 2.3520(16) . ? Zn N1 2.3521(16) 2_655 ? Zn Cl 2.3671(7) 2_655 ? Zn Cl 2.3671(7) . ? O N2 1.266(2) . ? N1 C1 1.283(2) . ? N1 C2 1.501(2) . ? N2 C1 1.387(2) . ? N2 C3 1.491(3) . ? N3 C12 1.339(2) . ? N3 C8 1.340(2) . ? C1 C8 1.477(3) . ? C2 C4 1.514(3) . ? C2 C5 1.524(3) . ? C2 C3 1.560(3) . ? C3 C7 1.517(3) . ? C3 C6 1.524(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.386(3) . ? C9 C10 1.388(3) . ? C9 H9 0.9300 . ? C10 C11 1.363(3) . ? C10 H10 0.9300 . ? C11 C12 1.388(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? 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 N3 Zn N3 162.99(9) . 2_655 ? N3 Zn N1 73.20(6) . . ? N3 Zn N1 94.27(6) 2_655 . ? N3 Zn N1 94.27(6) . 2_655 ? N3 Zn N1 73.20(6) 2_655 2_655 ? N1 Zn N1 86.98(8) . 2_655 ? N3 Zn Cl 95.45(5) . 2_655 ? N3 Zn Cl 95.13(5) 2_655 2_655 ? N1 Zn Cl 166.27(4) . 2_655 ? N1 Zn Cl 86.19(5) 2_655 2_655 ? N3 Zn Cl 95.13(5) . . ? N3 Zn Cl 95.45(5) 2_655 . ? N1 Zn Cl 86.19(5) . . ? N1 Zn Cl 166.27(4) 2_655 . ? Cl Zn Cl 102.82(4) 2_655 . ? C1 N1 C2 108.86(16) . . ? C1 N1 Zn 110.30(12) . . ? C2 N1 Zn 140.22(12) . . ? O N2 C1 127.32(18) . . ? O N2 C3 122.98(18) . . ? C1 N2 C3 109.16(16) . . ? C12 N3 C8 117.82(16) . . ? C12 N3 Zn 122.46(13) . . ? C8 N3 Zn 119.08(12) . . ? N1 C1 N2 113.41(17) . . ? N1 C1 C8 122.46(17) . . ? N2 C1 C8 124.10(16) . . ? N1 C2 C4 110.12(18) . . ? N1 C2 C5 106.12(18) . . ? C4 C2 C5 109.6(2) . . ? N1 C2 C3 103.91(15) . . ? C4 C2 C3 113.6(2) . . ? C5 C2 C3 112.98(19) . . ? N2 C3 C7 109.7(2) . . ? N2 C3 C6 105.97(19) . . ? C7 C3 C6 110.4(2) . . ? N2 C3 C2 99.37(15) . . ? C7 C3 C2 116.6(2) . . ? C6 C3 C2 113.6(2) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 122.63(18) . . ? N3 C8 C1 113.45(15) . . ? C9 C8 C1 123.89(19) . . ? C8 C9 C10 118.4(2) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 119.5(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 118.6(2) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N3 C12 C11 122.9(2) . . ? N3 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zn N1 C1 10.25(13) . . . . ? N3 Zn N1 C1 178.52(14) 2_655 . . . ? N1 Zn N1 C1 105.63(15) 2_655 . . . ? Cl Zn N1 C1 45.4(3) 2_655 . . . ? Cl Zn N1 C1 -86.29(14) . . . . ? N3 Zn N1 C2 179.6(2) . . . . ? N3 Zn N1 C2 -12.1(2) 2_655 . . . ? N1 Zn N1 C2 -85.0(2) 2_655 . . . ? Cl Zn N1 C2 -145.27(18) 2_655 . . . ? Cl Zn N1 C2 83.0(2) . . . . ? N3 Zn N3 C12 135.42(16) 2_655 . . . ? N1 Zn N3 C12 179.28(17) . . . . ? N1 Zn N3 C12 93.74(16) 2_655 . . . ? Cl Zn N3 C12 7.16(16) 2_655 . . . ? Cl Zn N3 C12 -96.27(16) . . . . ? N3 Zn N3 C8 -53.96(14) 2_655 . . . ? N1 Zn N3 C8 -10.11(14) . . . . ? N1 Zn N3 C8 -95.65(15) 2_655 . . . ? Cl Zn N3 C8 177.78(14) 2_655 . . . ? Cl Zn N3 C8 74.34(15) . . . . ? C2 N1 C1 N2 -4.6(2) . . . . ? Zn N1 C1 N2 168.21(14) . . . . ? C2 N1 C1 C8 177.02(18) . . . . ? Zn N1 C1 C8 -10.2(2) . . . . ? O N2 C1 N1 177.2(2) . . . . ? C3 N2 C1 N1 -11.1(3) . . . . ? O N2 C1 C8 -4.5(4) . . . . ? C3 N2 C1 C8 167.21(19) . . . . ? C1 N1 C2 C4 139.5(2) . . . . ? Zn N1 C2 C4 -29.9(3) . . . . ? C1 N1 C2 C5 -101.9(2) . . . . ? Zn N1 C2 C5 88.6(2) . . . . ? C1 N1 C2 C3 17.4(2) . . . . ? Zn N1 C2 C3 -152.01(16) . . . . ? O N2 C3 C7 -44.8(3) . . . . ? C1 N2 C3 C7 143.1(2) . . . . ? O N2 C3 C6 74.4(3) . . . . ? C1 N2 C3 C6 -97.7(2) . . . . ? O N2 C3 C2 -167.6(2) . . . . ? C1 N2 C3 C2 20.3(2) . . . . ? N1 C2 C3 N2 -21.7(2) . . . . ? C4 C2 C3 N2 -141.44(19) . . . . ? C5 C2 C3 N2 92.8(2) . . . . ? N1 C2 C3 C7 -139.5(2) . . . . ? C4 C2 C3 C7 100.8(3) . . . . ? C5 C2 C3 C7 -24.9(3) . . . . ? N1 C2 C3 C6 90.4(2) . . . . ? C4 C2 C3 C6 -29.3(3) . . . . ? C5 C2 C3 C6 -155.1(2) . . . . ? C12 N3 C8 C9 1.3(3) . . . . ? Zn N3 C8 C9 -169.76(17) . . . . ? C12 N3 C8 C1 179.50(18) . . . . ? Zn N3 C8 C1 8.4(2) . . . . ? N1 C1 C8 N3 2.1(3) . . . . ? N2 C1 C8 N3 -176.06(19) . . . . ? N1 C1 C8 C9 -179.7(2) . . . . ? N2 C1 C8 C9 2.1(3) . . . . ? N3 C8 C9 C10 -0.7(4) . . . . ? C1 C8 C9 C10 -178.7(2) . . . . ? C8 C9 C10 C11 -1.1(4) . . . . ? C9 C10 C11 C12 2.2(4) . . . . ? C8 N3 C12 C11 -0.1(3) . . . . ? Zn N3 C12 C11 170.61(16) . . . . ? C10 C11 C12 N3 -1.7(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.241 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.065