#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:38:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179254 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317417.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_4317417
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            'C13 H19 Co N3 S2'
_chemical_formula_weight         340.36
_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                 102.072(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8132(18)
_cell_length_b                   14.733(3)
_cell_length_c                   14.012(4)
_cell_measurement_reflns_used    3327
_cell_measurement_temperature    176(2)
_cell_volume                     1577.3(7)
_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      176(2)
_diffrn_measured_fraction_theta_full 0.860
_diffrn_measured_fraction_theta_max 0.860
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7219
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.7388
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   'Empirical From SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0455P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                2527
_reflns_number_total             3371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010321r_2.cif
_cod_data_source_block           (PATH)CoNCS
_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_original_cell_volume        1577.3(6)
_cod_database_code               4317417
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 0.18795(3) 0.391025(18) 0.67226(2) 0.02673(10) Uani 1 1 d . . .
N1 N 0.3424(2) 0.38070(12) 0.57487(14) 0.0315(4) Uani 1 1 d . . .
N2 N 0.3691(2) 0.36954(11) 0.80224(14) 0.0259(4) Uani 1 1 d . . .
N3 N 0.0182(2) 0.29311(12) 0.64729(16) 0.0388(5) Uani 1 1 d . . .
S1 S 0.12226(7) 0.53064(4) 0.71473(4) 0.03139(15) Uani 1 1 d . . .
S2 S -0.22853(8) 0.15539(4) 0.63531(5) 0.03998(17) Uani 1 1 d . . .
C1 C 0.2743(3) 0.35967(17) 0.4807(2) 0.0432(6) Uani 1 1 d . . .
H1A H 0.1529 0.3463 0.4629 0.052 Uiso 1 1 calc R . .
C2 C 0.3702(4) 0.35645(17) 0.4095(2) 0.0487(7) Uani 1 1 d . . .
H2A H 0.3168 0.3415 0.3441 0.058 Uiso 1 1 calc R . .
C3 C 0.5461(4) 0.37556(15) 0.4354(2) 0.0436(7) Uani 1 1 d . . .
H3A H 0.6167 0.3741 0.3878 0.052 Uiso 1 1 calc R . .
C4 C 0.6191(3) 0.39696(15) 0.5312(2) 0.0377(6) Uani 1 1 d . . .
H4A H 0.7407 0.4100 0.5496 0.045 Uiso 1 1 calc R . .
C5 C 0.5176(3) 0.39955(13) 0.60021(18) 0.0285(5) Uani 1 1 d . . .
C6 C 0.5903(3) 0.42411(16) 0.70500(17) 0.0331(5) Uani 1 1 d . . .
H6A H 0.5450 0.4847 0.7177 0.040 Uiso 1 1 calc R . .
H6B H 0.7192 0.4291 0.7145 0.040 Uiso 1 1 calc R . .
C7 C 0.5479(3) 0.35753(15) 0.78078(17) 0.0312(5) Uani 1 1 d . . .
H7A H 0.5581 0.2949 0.7571 0.037 Uiso 1 1 calc R . .
H7B H 0.6361 0.3648 0.8422 0.037 Uiso 1 1 calc R . .
C8 C 0.3312(3) 0.28678(15) 0.85579(19) 0.0389(6) Uani 1 1 d . . .
H8A H 0.4201 0.2803 0.9161 0.058 Uiso 1 1 calc R . .
H8B H 0.3331 0.2332 0.8146 0.058 Uiso 1 1 calc R . .
H8C H 0.2154 0.2926 0.8718 0.058 Uiso 1 1 calc R . .
C9 C 0.3639(3) 0.45203(13) 0.86478(17) 0.0269(5) Uani 1 1 d . . .
H9A H 0.4557 0.4948 0.8540 0.032 Uiso 1 1 calc R . .
H9B H 0.3934 0.4332 0.9341 0.032 Uiso 1 1 calc R . .
C10 C 0.1873(3) 0.50284(13) 0.84636(16) 0.0261(5) Uani 1 1 d . . .
C11 C 0.2167(3) 0.59150(14) 0.9056(2) 0.0366(6) Uani 1 1 d . . .
H11A H 0.2506 0.5772 0.9753 0.055 Uiso 1 1 calc R . .
H11B H 0.1083 0.6270 0.8934 0.055 Uiso 1 1 calc R . .
H11C H 0.3098 0.6267 0.8858 0.055 Uiso 1 1 calc R . .
C12 C 0.0412(3) 0.44833(15) 0.87741(18) 0.0320(5) Uani 1 1 d . . .
H12A H 0.0753 0.4339 0.9471 0.048 Uiso 1 1 calc R . .
H12B H 0.0216 0.3919 0.8397 0.048 Uiso 1 1 calc R . .
H12C H -0.0667 0.4843 0.8653 0.048 Uiso 1 1 calc R . .
C13 C -0.0849(3) 0.23569(14) 0.64255(16) 0.0277(5) Uani 1 1 d . . .
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'
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 Co1 N1 107.85(8) . . ?
N3 Co1 N2 111.00(8) . . ?
N1 Co1 N2 100.81(8) . . ?
N3 Co1 S1 123.13(6) . . ?
N1 Co1 S1 117.11(5) . . ?
N2 Co1 S1 93.39(5) . . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Co1 120.76(17) . . ?
C5 N1 Co1 121.26(16) . . ?
C8 N2 C7 107.19(16) . . ?
C8 N2 C9 109.54(18) . . ?
C7 N2 C9 110.63(16) . . ?
C8 N2 Co1 113.15(14) . . ?
C7 N2 Co1 109.49(14) . . ?
C9 N2 Co1 106.87(12) . . ?
C13 N3 Co1 172.8(2) . . ?
C10 S1 Co1 91.79(7) . . ?
N1 C1 C2 123.8(2) . . ?
C1 C2 C3 118.1(3) . . ?
C2 C3 C4 119.3(3) . . ?
C5 C4 C3 120.6(2) . . ?
N1 C5 C4 120.4(2) . . ?
N1 C5 C6 117.1(2) . . ?
C4 C5 C6 122.5(2) . . ?
C5 C6 C7 115.48(19) . . ?
N2 C7 C6 114.16(17) . . ?
N2 C9 C10 115.28(17) . . ?
C12 C10 C11 109.14(19) . . ?
C12 C10 C9 113.05(17) . . ?
C11 C10 C9 107.12(17) . . ?
C12 C10 S1 109.46(14) . . ?
C11 C10 S1 109.15(15) . . ?
C9 C10 S1 108.85(15) . . ?
N3 C13 S2 179.7(2) . . ?
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 N3 1.9414(18) . ?
Co1 N1 2.008(2) . ?
Co1 N2 2.0839(18) . ?
Co1 S1 2.2307(8) . ?
N1 C1 1.352(3) . ?
N1 C5 1.369(3) . ?
N2 C8 1.493(3) . ?
N2 C7 1.499(3) . ?
N2 C9 1.504(3) . ?
N3 C13 1.160(3) . ?
S1 C10 1.854(2) . ?
S2 C13 1.619(2) . ?
C1 C2 1.367(4) . ?
C2 C3 1.375(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.374(3) . ?
C5 C6 1.504(3) . ?
C6 C7 1.532(3) . ?
C9 C10 1.543(3) . ?
C10 C12 1.531(3) . ?
C10 C11 1.539(3) . ?
