#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:44:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179153 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/14/4311442.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_4311442
loop_
_publ_author_name
'Christopher A. Dodds'
'Mario-Alexander Lehmann'
'Jonathan F. Ojo'
'John Reglinski'
'Mark D. Spicer'
_publ_section_title
;
 Cobalt Half-Sandwich, Sandwich, and Mixed Sandwich Complexes with Soft
 Tripodal Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4927
_journal_page_last               4934
_journal_paper_doi               10.1021/ic0496525
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H16 B1 Br1 Co1 N6 S3'
_chemical_formula_sum            'C12 H16 B Br Co N6 S3'
_chemical_formula_weight         490.14
_chemical_name_common
'bromo hydrotris(methimazolyl)borato cobalt(II)'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-04-12T14:02:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.714(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0655(6)
_cell_length_b                   12.4897(7)
_cell_length_c                   12.7057(7)
_cell_measurement_reflns_used    32592
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     1905.17(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.426014E-1
_diffrn_orient_matrix_UB_12      -0.713915E-1
_diffrn_orient_matrix_UB_13      -0.51387E-2
_diffrn_orient_matrix_UB_21      0.483542E-1
_diffrn_orient_matrix_UB_22      0.246165E-1
_diffrn_orient_matrix_UB_23      0.588766E-1
_diffrn_orient_matrix_UB_31      -0.440843E-1
_diffrn_orient_matrix_UB_32      -0.392829E-1
_diffrn_orient_matrix_UB_33      0.526298E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13621
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.334
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0488P)²+0.0244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2950
_reflns_number_total             4210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0496525si20040507_093809_1.cif
_cod_data_source_block           cotmbr
_cod_database_code               4311442
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Br1 Br 0.20978(3) 0.19136(4) 0.27591(3) 0.03201(14) Uani 1 1 d . . .
Co1 Co 0.24653(4) 0.22514(4) 0.46160(4) 0.02285(15) Uani 1 1 d . . .
S1 S 0.43773(8) 0.23181(8) 0.50496(8) 0.0252(2) Uani 1 1 d . . .
S2 S 0.16532(8) 0.38412(8) 0.51100(8) 0.0260(2) Uani 1 1 d . . .
S3 S 0.18352(8) 0.08774(8) 0.56419(8) 0.0287(3) Uani 1 1 d . . .
N3 N 0.3353(2) 0.3801(2) 0.6768(2) 0.0212(7) Uani 1 1 d . . .
N5 N 0.1896(3) 0.2426(3) 0.7222(2) 0.0230(7) Uani 1 1 d . . .
N6 N 0.0228(3) 0.1899(3) 0.6616(2) 0.0268(8) Uani 1 1 d . . .
N2 N 0.5317(3) 0.0954(3) 0.6534(3) 0.0290(8) Uani 1 1 d . . .
N4 N 0.3386(3) 0.5156(3) 0.5685(2) 0.0264(8) Uani 1 1 d . . .
N1 N 0.3979(2) 0.1877(3) 0.7134(2) 0.0226(7) Uani 1 1 d . . .
C5 C 0.2808(3) 0.4273(3) 0.5900(3) 0.0215(8) Uani 1 1 d . . .
C10 C 0.1135(3) 0.2993(3) 0.7746(3) 0.0276(9) Uani 1 1 d . . .
H10 H 0.1306 0.3515 0.8281 0.033 Uiso 1 1 calc R . .
C11 C 0.0109(4) 0.2674(3) 0.7364(3) 0.0315(10) Uani 1 1 d . . .
H11 H -0.0574 0.2936 0.7574 0.038 Uiso 1 1 calc R . .
C9 C 0.1330(3) 0.1751(3) 0.6534(3) 0.0222(9) Uani 1 1 d . . .
C1 C 0.4544(3) 0.1720(3) 0.6280(3) 0.0227(9) Uani 1 1 d . . .
C8 C 0.3087(4) 0.5899(4) 0.4807(3) 0.0381(11) Uani 1 1 d . . .
H8A H 0.3638 0.6476 0.4824 0.057 Uiso 1 1 calc R . .
H8B H 0.2349 0.6203 0.4877 0.057 Uiso 1 1 calc R . .
H8C H 0.3073 0.5513 0.4134 0.057 Uiso 1 1 calc R . .
C3 C 0.5241(3) 0.0614(3) 0.7547(3) 0.0315(10) Uani 1 1 d . . .
H3 H 0.5689 0.0083 0.7918 0.038 Uiso 1 1 calc R . .
B1 B 0.3140(4) 0.2763(4) 0.7389(4) 0.0253(10) Uani 1 1 d . . .
C7 C 0.4314(3) 0.5247(3) 0.6408(3) 0.0291(9) Uani 1 1 d . . .
H7 H 0.4863 0.5795 0.6431 0.035 Uiso 1 1 calc R . .
C6 C 0.4292(3) 0.4413(3) 0.7072(3) 0.0255(9) Uani 1 1 d . . .
H6 H 0.4829 0.4266 0.7653 0.031 Uiso 1 1 calc R . .
C12 C -0.0678(3) 0.1354(4) 0.6000(4) 0.0390(11) Uani 1 1 d . . .
H12A H -0.139 0.1606 0.6216 0.058 Uiso 1 1 calc R . .
H12B H -0.0611 0.0581 0.612 0.058 Uiso 1 1 calc R . .
H12C H -0.0644 0.1507 0.5247 0.058 Uiso 1 1 calc R . .
C2 C 0.4413(3) 0.1171(3) 0.7919(3) 0.0307(10) Uani 1 1 d . . .
H2 H 0.4165 0.1097 0.8602 0.037 Uiso 1 1 calc R . .
C4 C 0.6189(3) 0.0639(4) 0.5869(4) 0.0390(11) Uani 1 1 d . . .
H4A H 0.6646 0.007 0.6222 0.058 Uiso 1 1 calc R . .
H4B H 0.6661 0.1258 0.5754 0.058 Uiso 1 1 calc R . .
H4C H 0.5844 0.0377 0.5186 0.058 Uiso 1 1 calc R . .
H1 H 0.325(3) 0.295(3) 0.823(3) 0.017(9) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0 0 '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'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Co1 S2 109.92(4) . . ?
S1 Co1 S3 105.43(4) . . ?
S2 Co1 S3 107.94(4) . . ?
S1 Co1 Br1 108.82(3) . . ?
S2 Co1 Br1 111.99(3) . . ?
S3 Co1 Br1 112.53(3) . . ?
C1 S1 Co1 102.90(13) . . ?
C5 S2 Co1 94.96(13) . . ?
C9 S3 Co1 93.31(13) . . ?
C5 N3 C6 107.6(3) . . ?
C5 N3 B1 133.1(3) . . ?
C6 N3 B1 119.3(3) . . ?
C9 N5 C10 108.3(3) . . ?
C9 N5 B1 132.6(3) . . ?
C10 N5 B1 118.4(3) . . ?
C9 N6 C11 108.6(3) . . ?
C9 N6 C12 125.9(3) . . ?
C11 N6 C12 125.4(3) . . ?
C1 N2 C3 109.6(3) . . ?
C1 N2 C4 124.7(3) . . ?
C3 N2 C4 125.3(4) . . ?
C5 N4 C7 109.5(3) . . ?
C5 N4 C8 125.3(3) . . ?
C7 N4 C8 125.1(3) . . ?
C1 N1 C2 107.3(3) . . ?
C1 N1 B1 131.4(3) . . ?
C2 N1 B1 120.5(3) . . ?
N4 C5 N3 107.5(3) . . ?
N4 C5 S2 122.9(3) . . ?
N3 C5 S2 129.4(3) . . ?
C11 C10 N5 107.9(4) . . ?
C10 C11 N6 107.6(3) . . ?
N5 C9 N6 107.6(3) . . ?
N5 C9 S3 129.1(3) . . ?
N6 C9 S3 123.3(3) . . ?
N2 C1 N1 107.6(3) . . ?
N2 C1 S1 122.5(3) . . ?
N1 C1 S1 129.8(3) . . ?
C2 C3 N2 107.0(4) . . ?
N5 B1 N3 111.3(3) . . ?
N5 B1 N1 114.7(3) . . ?
N3 B1 N1 110.2(3) . . ?
C6 C7 N4 106.8(3) . . ?
C7 C6 N3 108.6(3) . . ?
C3 C2 N1 108.5(3) . . ?
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
Br1 Co1 2.3943(6) . ?
Co1 S1 2.3193(11) . ?
Co1 S2 2.3279(12) . ?
Co1 S3 2.3280(11) . ?
S1 C1 1.727(4) . ?
S2 C5 1.721(4) . ?
S3 C9 1.727(4) . ?
N3 C5 1.361(5) . ?
N3 C6 1.390(5) . ?
N3 B1 1.552(5) . ?
N5 C9 1.350(5) . ?
N5 C10 1.382(5) . ?
N5 B1 1.553(5) . ?
N6 C9 1.357(5) . ?
N6 C11 1.374(5) . ?
N6 C12 1.449(5) . ?
N2 C1 1.351(5) . ?
N2 C3 1.368(5) . ?
N2 C4 1.469(5) . ?
N4 C5 1.348(5) . ?
N4 C7 1.381(5) . ?
N4 C8 1.468(5) . ?
N1 C1 1.352(5) . ?
N1 C2 1.394(5) . ?
N1 B1 1.555(6) . ?
C10 C11 1.344(6) . ?
C3 C2 1.341(6) . ?
C7 C6 1.343(5) . ?
