#------------------------------------------------------------------------------ #$Date: 2014-07-11 17:35:18 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100143.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_1100143 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 2(1)/c' loop_ _publ_author_name 'Raj Pal Sharma' 'Rajni Sharma' 'Ritu Bala' 'Miguel Quiros' 'Juan M. Salas' _journal_name_full 'Journal of Coordination Chemistry' _journal_volume 56 _journal_page_first 1581 _journal_page_last 1586 _journal_year 2003 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H16 Co N11 S' _chemical_formula_weight 321.28 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1950(6) _cell_length_b 9.0317(5) _cell_length_c 12.6017(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.4190(10) _cell_angle_gamma 90.00 _cell_volume 1273.63(12) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4678 _cell_measurement_theta_min 2.861 _cell_measurement_theta_max 25.019 _exptl_crystal_description 'irregular block' _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7605 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.22. ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 12953 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.92 _reflns_number_total 2253 _reflns_number_gt 2047 _reflns_threshold_expression >2sigma(I) _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^)+(0.0400P)^2^+0.5000P] 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 2253 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.17300(2) 0.46590(3) 0.31515(2) 0.02106(11) Uani 1 1 d . . . N1A N 0.02113(15) 0.56148(19) 0.24018(15) 0.0286(4) Uani 1 1 d . . . N2A N -0.03974(15) 0.53110(19) 0.13850(16) 0.0275(4) Uani 1 1 d . . . N3A N -0.10125(18) 0.5073(2) 0.04063(18) 0.0425(5) Uani 1 1 d . . . N4A N 0.12370(15) 0.3545(2) 0.42313(15) 0.0312(4) Uani 1 1 d . . . N5A N 0.02892(16) 0.35343(19) 0.42268(14) 0.0278(4) Uani 1 1 d . . . N6A N -0.06020(17) 0.3438(2) 0.42829(18) 0.0428(5) Uani 1 1 d . . . N1E N 0.23250(15) 0.5878(2) 0.21923(15) 0.0278(4) Uani 1 1 d . . . H11E H 0.2778 0.5327 0.1927 0.033 Uiso 1 1 d R . . H12E H 0.1710 0.6254 0.1583 0.033 Uiso 1 1 d R . . C1E C 0.3046(2) 0.7088(3) 0.2943(2) 0.0395(5) Uani 1 1 d . . . H13E H 0.3111 0.7901 0.2469 0.047 Uiso 1 1 d R . . H14E H 0.3844 0.6731 0.3406 0.047 Uiso 1 1 d R . . C2E C 0.2457(2) 0.7618(3) 0.3724(2) 0.0401(5) Uani 1 1 d . . . H23E H 0.2981 0.8293 0.4301 0.048 Uiso 1 1 d R . . H24E H 0.1718 0.8132 0.3277 0.048 Uiso 1 1 d R . . N2E N 0.22099(15) 0.6288(2) 0.42939(14) 0.0295(4) Uani 1 1 d . . . H21E H 0.1620 0.6483 0.4532 0.035 Uiso 1 1 d R . . H22E H 0.2868 0.6031 0.4914 0.035 Uiso 1 1 d R . . N3E N 0.13067(14) 0.30238(19) 0.19910(14) 0.0269(4) Uani 1 1 d . . . H31E H 0.0707 0.2484 0.2038 0.032 Uiso 1 1 d R . . H32E H 0.1051 0.3411 0.1275 0.032 Uiso 1 1 d R . . C3E C 0.2326(2) 0.2074(3) 0.21870(19) 0.0361(5) Uani 1 1 d . . . H33E H 0.2811 0.2467 0.1801 0.043 Uiso 1 1 d R . . H34E H 0.2066 0.1085 0.1896 0.043 Uiso 1 1 d R . . C4E C 0.3043(2) 0.2046(2) 0.35062(19) 0.0363(5) Uani 1 1 d . . . H43E H 0.2614 0.1485 0.3876 0.044 Uiso 1 1 d R . . H44E H 0.3815 0.1582 0.3690 0.044 Uiso 1 1 d R . . N4E N 0.32039(14) 0.3604(2) 0.39237(14) 0.0291(4) Uani 1 1 d . . . H41E H 0.3791 0.4036 0.3772 0.035 Uiso 1 1 d R . . H42E H 0.3410 0.3624 0.4693 0.035 Uiso 1 1 d R . . S S 0.43865(6) 0.45395(8) 0.12585(5) 0.04896(19) Uani 1 1 d . . . C1T C 0.5128(2) 0.4608(3) 0.2697(2) 0.0380(6) Uani 1 1 d . . . N1T N 0.5622(2) 0.4653(3) 0.3719(2) 0.0616(7) Uani 1 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 Co 0.01696(15) 0.02456(17) 0.02102(17) -0.00081(10) 0.00686(11) 0.00012(10) N1A 0.0214(8) 0.0335(10) 0.0289(10) 0.0008(8) 0.0077(8) 0.0039(7) N2A 0.0210(8) 0.0279(9) 0.0350(11) 0.0028(8) 0.0126(8) 0.0026(7) N3A 0.0324(11) 0.0520(13) 0.0350(12) -0.0058(9) 0.0047(9) 0.0022(9) N4A 0.0249(9) 0.0392(11) 0.0319(9) 0.0067(8) 0.0138(8) 0.0022(8) N5A 0.0322(10) 0.0256(9) 0.0272(9) -0.0021(7) 0.0134(8) -0.0021(7) N6A 0.0336(11) 0.0473(12) 0.0577(13) -0.0089(10) 0.0290(10) -0.0071(9) N1E 0.0239(8) 0.0292(9) 0.0319(9) -0.0001(8) 0.0129(7) -0.0003(7) C1E 0.0352(12) 0.0344(12) 0.0508(14) -0.0038(11) 0.0190(11) -0.0107(10) C2E 0.0412(13) 0.0308(12) 0.0466(13) -0.0109(10) 0.0156(11) -0.0065(10) N2E 0.0226(8) 0.0347(10) 0.0307(9) -0.0061(8) 0.0100(7) 0.0005(7) N3E 0.0256(9) 0.0272(9) 0.0245(8) 0.0001(7) 0.0065(7) 0.0000(7) C3E 0.0352(12) 0.0316(12) 0.0417(12) -0.0072(10) 0.0155(10) 0.0045(9) C4E 0.0315(12) 0.0349(12) 0.0408(13) 0.0021(10) 0.0127(10) 0.0090(10) N4E 0.0197(8) 0.0374(10) 0.0282(9) -0.0001(8) 0.0074(7) 0.0026(7) S 0.0374(3) 0.0716(5) 0.0344(3) -0.0008(3) 0.0106(3) 0.0032(3) C1T 0.0238(11) 0.0477(14) 0.0445(15) -0.0024(11) 0.0157(11) 0.0043(10) N1T 0.0471(14) 0.085(2) 0.0396(14) -0.0082(12) 0.0036(11) 0.0164(12) _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 N1A 1.9175(17) . ? Co N4E 1.9223(16) . ? Co N4A 1.9686(17) . ? Co N1E 1.9739(17) . ? Co N2E 1.9773(17) . ? Co N3E 1.9966(17) . ? N1A N2A 1.230(2) . ? N2A N3A 1.181(3) . ? N4A N5A 1.154(2) . ? N5A N6A 1.120(2) . ? N1E C1E 1.484(3) . ? C1E C2E 1.508(3) . ? C2E N2E 1.490(3) . ? N3E C3E 1.449(3) . ? C3E C4E 1.541(3) . ? C4E N4E 1.488(3) . ? S C1T 1.675(3) . ? C1T N1T 1.185(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Co N4E 176.60(7) . . ? N1A Co N4A 94.02(7) . . ? N4E Co N4A 82.98(7) . . ? N1A Co N1E 88.02(7) . . ? N4E Co N1E 95.11(7) . . ? N4A Co N1E 174.76(7) . . ? N1A Co N2E 88.41(7) . . ? N4E Co N2E 93.08(7) . . ? N4A Co N2E 87.73(7) . . ? N1E Co N2E 87.51(7) . . ? N1A Co N3E 93.11(7) . . ? N4E Co N3E 85.51(7) . . ? N4A Co N3E 93.85(7) . . ? N1E Co N3E 90.85(7) . . ? N2E Co N3E 177.73(7) . . ? N2A N1A Co 118.54(14) . . ? N3A N2A N1A 177.1(2) . . ? N5A N4A Co 125.56(15) . . ? N6A N5A N4A 174.7(2) . . ? C1E N1E Co 106.80(13) . . ? N1E C1E C2E 109.55(18) . . ? N2E C2E C1E 107.37(18) . . ? C2E N2E Co 107.86(13) . . ? C3E N3E Co 111.01(13) . . ? N3E C3E C4E 105.92(16) . . ? N4E C4E C3E 107.71(17) . . ? C4E N4E Co 108.94(12) . . ? N1T C1T S 178.1(2) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.422 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.056 _cod_database_code 1100143 _journal_paper_doi 10.1080/00958970310001641673