#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:38:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179254 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317416.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_4317416
loop_
_publ_author_name
'SeChin Chang'
'Vivek V. Karambelkar'
'Roger D. Sommer'
'Arnold L. Rheingold'
'David P. Goldberg'
_publ_section_title
;
 New Monomeric Cobalt(II) and Zinc(II) Complexes of a Mixed
 N,S(alkylthiolate) Ligand: Model Complexes of (His)(His)(Cys)
 Metalloprotein Active Sites
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              239
_journal_page_last               248
_journal_paper_doi               10.1021/ic010321r
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C12 H19 Br Co N2 S'
_chemical_formula_weight         362.19
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.096(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1867(7)
_cell_length_b                   14.9939(13)
_cell_length_c                   11.9478(10)
_cell_measurement_reflns_used    5347
_cell_measurement_temperature    173(2)
_cell_volume                     1466.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6073
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    4.018
_exptl_absorpt_correction_T_max  0.4718
_exptl_absorpt_correction_T_min  0.2831
_exptl_absorpt_correction_type   'Empirical from SADABS'
_exptl_crystal_colour            parallelepiped
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blue
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0516
_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/[σ²(Fo²)+(0.1099P)²+0.6002P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                3066
_reflns_number_total             3307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010321r_1.cif
_cod_data_source_block           (PATH)CoBr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317416
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
Co1 Co 0.31291(4) 0.18707(2) 0.36758(3) 0.01792(15) Uani 1 1 d . . .
Br1 Br 0.16719(4) 0.12632(2) 0.21096(3) 0.03680(16) Uani 1 1 d . . .
N1 N 0.5143(3) 0.10794(16) 0.38145(18) 0.0200(4) Uani 1 1 d . . .
N2 N 0.4234(3) 0.31110(15) 0.34352(19) 0.0193(5) Uani 1 1 d . . .
S1 S 0.19005(9) 0.23460(5) 0.52178(6) 0.02594(19) Uani 1 1 d . . .
C1 C 0.5017(4) 0.01994(19) 0.3582(2) 0.0239(5) Uani 1 1 d . . .
H1A H 0.3984 -0.0031 0.3351 0.029 Uiso 1 1 calc R . .
C2 C 0.6326(4) -0.0379(2) 0.3665(2) 0.0304(6) Uani 1 1 d . . .
H2A H 0.6200 -0.0995 0.3501 0.037 Uiso 1 1 calc R . .
C3 C 0.7832(4) -0.0034(2) 0.3996(3) 0.0341(7) Uani 1 1 d . . .
H3A H 0.8755 -0.0415 0.4070 0.041 Uiso 1 1 calc R . .
C4 C 0.7981(4) 0.0863(2) 0.4216(2) 0.0298(6) Uani 1 1 d . . .
H4A H 0.9012 0.1107 0.4428 0.036 Uiso 1 1 calc R . .
C5 C 0.6606(3) 0.1417(2) 0.4125(2) 0.0219(5) Uani 1 1 d . . .
C6 C 0.6718(3) 0.2400(2) 0.4372(3) 0.0259(6) Uani 1 1 d . . .
H6A H 0.7878 0.2554 0.4522 0.031 Uiso 1 1 calc R . .
H6B H 0.6109 0.2525 0.5063 0.031 Uiso 1 1 calc R . .
C7 C 0.6057(3) 0.30076(19) 0.3439(2) 0.0245(6) Uani 1 1 d . . .
H7A H 0.6565 0.3604 0.3521 0.029 Uiso 1 1 calc R . .
H7B H 0.6385 0.2762 0.2708 0.029 Uiso 1 1 calc R . .
C8 C 0.3717(4) 0.3506(2) 0.2343(2) 0.0288(6) Uani 1 1 d . . .
H8A H 0.4251 0.4085 0.2249 0.043 Uiso 1 1 calc R . .
H8B H 0.2529 0.3587 0.2327 0.043 Uiso 1 1 calc R . .
H8C H 0.4029 0.3106 0.1735 0.043 Uiso 1 1 calc R . .
C9 C 0.3772(3) 0.37140(18) 0.4379(2) 0.0224(5) Uani 1 1 d . . .
H9A H 0.3805 0.4338 0.4107 0.027 Uiso 1 1 calc R . .
H9B H 0.4609 0.3656 0.4983 0.027 Uiso 1 1 calc R . .
C10 C 0.2087(3) 0.3545(2) 0.4881(2) 0.0220(5) Uani 1 1 d . . .
C11 C 0.2034(4) 0.4075(2) 0.5978(2) 0.0320(7) Uani 1 1 d . . .
H11A H 0.2133 0.4713 0.5816 0.048 Uiso 1 1 calc R . .
H11B H 0.2940 0.3888 0.6473 0.048 Uiso 1 1 calc R . .
H11C H 0.0995 0.3962 0.6347 0.048 Uiso 1 1 calc R . .
C12 C 0.0667(4) 0.3844(2) 0.4123(3) 0.0301(6) Uani 1 1 d . . .
H12A H 0.0783 0.4480 0.3952 0.045 Uiso 1 1 calc R . .
H12B H -0.0366 0.3745 0.4505 0.045 Uiso 1 1 calc R . .
H12C H 0.0672 0.3500 0.3426 0.045 Uiso 1 1 calc R . .
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'
Br Br -0.2901 2.4595 '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
N1 Co1 N2 100.24(9) . . ?
N1 Co1 S1 119.72(7) . . ?
N2 Co1 S1 91.86(6) . . ?
N1 Co1 Br1 103.53(7) . . ?
N2 Co1 Br1 116.36(6) . . ?
S1 Co1 Br1 122.94(3) . . ?
C5 N1 C1 119.2(2) . . ?
C5 N1 Co1 121.24(19) . . ?
C1 N1 Co1 119.58(19) . . ?
C8 N2 C9 110.3(2) . . ?
C8 N2 C7 108.1(2) . . ?
C9 N2 C7 109.0(2) . . ?
C8 N2 Co1 110.98(18) . . ?
C9 N2 Co1 108.49(15) . . ?
C7 N2 Co1 109.93(16) . . ?
C10 S1 Co1 95.18(8) . . ?
N1 C1 C2 122.8(3) . . ?
C1 C2 C3 118.1(3) . . ?
C4 C3 C2 119.6(3) . . ?
C3 C4 C5 119.8(3) . . ?
N1 C5 C4 120.5(3) . . ?
N1 C5 C6 118.2(2) . . ?
C4 C5 C6 121.3(3) . . ?
C5 C6 C7 114.9(2) . . ?
N2 C7 C6 113.7(2) . . ?
N2 C9 C10 115.8(2) . . ?
C12 C10 C11 108.7(2) . . ?
C12 C10 C9 113.5(2) . . ?
C11 C10 C9 106.8(2) . . ?
C12 C10 S1 110.5(2) . . ?
C11 C10 S1 108.3(2) . . ?
C9 C10 S1 108.92(19) . . ?
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
Co1 N1 2.036(2) . ?
Co1 N2 2.090(2) . ?
Co1 S1 2.2327(7) . ?
Co1 Br1 2.3810(5) . ?
N1 C5 1.346(4) . ?
N1 C1 1.352(4) . ?
N2 C8 1.487(3) . ?
N2 C9 1.499(3) . ?
N2 C7 1.500(3) . ?
S1 C10 1.849(3) . ?
C1 C2 1.380(4) . ?
C2 C3 1.387(5) . ?
C3 C4 1.375(5) . ?
C4 C5 1.401(4) . ?
C5 C6 1.507(4) . ?
C6 C7 1.530(4) . ?
C9 C10 1.536(4) . ?
C10 C12 1.528(4) . ?
C10 C11 1.535(4) . ?
