#------------------------------------------------------------------------------ #$Date: 2015-01-27 19:58:39 +0000 (Tue, 27 Jan 2015) $ #$Revision: 130149 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/10/1101017.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1101017 loop_ _publ_author_name 'Raj Pal Sharma' 'Rajni Sharma' 'Ritu Bala' 'Miguel Quir\'os' 'Juan M. Salas' _journal_name_full 'Journal of Coordination Chemistry' _journal_page_first 1099 _journal_page_last 1104 _journal_paper_doi 10.1080/00958970500138355 _journal_volume 58 _journal_year 2005 _chemical_formula_sum 'C8 H32 Cl2 Co2 N8 O6 S4' _chemical_formula_weight 653.42 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _cell_angle_alpha 100.043(1) _cell_angle_beta 91.562(1) _cell_angle_gamma 107.339(1) _cell_formula_units_Z 1 _cell_length_a 6.3067(4) _cell_length_b 7.7820(5) _cell_length_c 12.7658(8) _cell_measurement_reflns_used 3923 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 23.27 _cell_measurement_theta_min 2.80 _cell_volume 586.80(6) _diffrn_ambient_temperature 298(2) _diffrn_detector_area_resol_mean 66.06 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4977 _diffrn_reflns_theta_max 23.27 _diffrn_reflns_theta_min 1.63 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 149 _exptl_absorpt_coefficient_mu 2.040 _exptl_absorpt_correction_T_max 0.7919 _exptl_absorpt_correction_T_min 0.6052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 336 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 139 _refine_ls_number_reflns 1687 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0199 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.0539 _reflns_number_gt 1647 _reflns_number_total 1687 _reflns_threshold_expression >2sigma(I) _cod_database_code 1101017 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Co1 Co 0.5000 0.0000 0.5000 0.02289(12) Uani 1 2 d S . . Cl Cl 0.19410(9) -0.07579(8) 0.38744(4) 0.03779(16) Uani 1 1 d . . . N1 N 0.4209(3) -0.2540(2) 0.52240(14) 0.0326(4) Uani 1 1 d . . . H11 H 0.3833 -0.3321 0.4592 0.039 Uiso 1 1 d R . . H12 H 0.5384 -0.2728 0.5548 0.039 Uiso 1 1 d R . . C1 C 0.2308(4) -0.2873(3) 0.5897(2) 0.0430(6) Uani 1 1 d . . . H13 H 0.2208 -0.3931 0.6220 0.052 Uiso 1 1 d R . . H14 H 0.0922 -0.3097 0.5471 0.052 Uiso 1 1 d R . . C2 C 0.2738(4) -0.1176(3) 0.67438(19) 0.0414(6) Uani 1 1 d . . . H23 H 0.1432 -0.1233 0.7138 0.050 Uiso 1 1 d R . . H24 H 0.3981 -0.1070 0.7241 0.050 Uiso 1 1 d R . . N2 N 0.3257(3) 0.0420(2) 0.62038(13) 0.0291(4) Uani 1 1 d . . . H21 H 0.4034 0.1441 0.6668 0.035 Uiso 1 1 d R . . H22 H 0.1983 0.0581 0.5970 0.035 Uiso 1 1 d R . . Co2 Co 0.0000 0.5000 0.0000 0.02163(12) Uani 1 2 d S . . S1 S 0.02512(8) 0.44871(7) 0.17265(4) 0.02864(15) Uani 1 1 d . . . S2 S 0.34270(8) 0.45443(7) 0.21612(4) 0.02587(14) Uani 1 1 d . . . O1T O 0.3416(3) 0.4327(2) 0.32654(11) 0.0377(4) Uani 1 1 d . . . O2T O 0.4971(2) 0.6323(2) 0.20384(12) 0.0354(4) Uani 1 1 d . . . O3T O 0.3922(3) 0.3060(2) 0.14413(12) 0.0385(4) Uani 1 1 d . . . N3 N 0.2841(3) 0.6983(2) 0.02043(14) 0.0291(4) Uani 1 1 d . . . H31 H 0.3695 0.6876 0.0751 0.035 Uiso 1 1 d R . . H32 H 0.3574 0.6900 -0.0388 0.035 Uiso 1 1 d R . . C3 C 0.2433(4) 0.8784(3) 0.04335(19) 0.0378(5) Uani 1 1 d . . . H33 H 0.2104 0.9145 -0.0227 0.045 Uiso 1 1 d R . . H34 H 0.3739 0.9714 0.0816 0.045 Uiso 1 1 d R . . C4 C 0.0480(4) 0.8577(3) 0.11021(18) 0.0376(5) Uani 1 1 d . . . H43 H 0.0902 0.8442 0.1813 0.045 Uiso 1 1 d R . . H44 H -0.0022 0.9651 0.1165 0.045 Uiso 1 1 d R . . N4 N -0.1324(3) 0.6923(2) 0.05686(13) 0.0291(4) Uani 1 1 d . . . H41 H -0.2051 0.7192 0.0034 0.035 Uiso 1 1 d R . . H42 H -0.2307 0.6529 0.1039 0.035 Uiso 1 1 d 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 Co1 0.0228(2) 0.0284(2) 0.0185(2) 0.00134(16) -0.00044(15) 0.01136(16) Cl 0.0298(3) 0.0564(4) 0.0268(3) -0.0003(2) -0.0058(2) 0.0181(3) N1 0.0396(11) 0.0326(10) 0.0274(10) 0.0033(8) 0.0008(8) 0.0152(8) C1 0.0484(15) 0.0375(13) 0.0423(14) 0.0134(11) 0.0107(11) 0.0081(11) C2 0.0486(15) 0.0483(15) 0.0299(12) 0.0104(11) 0.0120(11) 0.0162(12) N2 0.0250(9) 0.0359(10) 0.0253(9) -0.0008(8) 0.0004(7) 0.0116(8) Co2 0.0204(2) 0.0264(2) 0.0192(2) 0.00479(16) 0.00247(15) 0.00866(16) S1 0.0251(3) 0.0410(3) 0.0227(3) 0.0103(2) 0.0038(2) 0.0118(2) S2 0.0279(3) 0.0297(3) 0.0213(3) 0.0033(2) 0.0002(2) 0.0119(2) O1T 0.0450(9) 0.0491(10) 0.0249(8) 0.0095(7) 0.0001(7) 0.0225(8) O2T 0.0293(8) 0.0376(9) 0.0350(9) 0.0060(7) -0.0026(6) 0.0048(7) O3T 0.0427(9) 0.0408(9) 0.0353(9) -0.0020(7) 0.0020(7) 0.0231(7) N3 0.0266(9) 0.0336(10) 0.0278(9) 0.0095(8) 0.0019(7) 0.0085(7) C3 0.0409(13) 0.0288(12) 0.0405(13) 0.0071(10) -0.0033(11) 0.0061(10) C4 0.0494(14) 0.0337(12) 0.0310(12) -0.0021(10) -0.0040(11) 0.0201(11) N4 0.0317(10) 0.0379(10) 0.0224(9) 0.0068(8) 0.0038(7) 0.0168(8)