#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/98/7009889.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_7009889
loop_
_publ_author_name
'Helgard G. Raubenheimer'
'Eugene K. Marais'
'Stephanie Cronje'
'Catharine Esterhuysen (neé Thompson)'
'Gert J. Kruger'
_publ_section_title
;
 Synthesis and crystallographic characterization of
 thiazole-2-dithiocarboxylate methyl ester complexes of chromium,
 tungsten and iron carbonyls
;
_journal_issue                   17
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3016
_journal_page_last               3021
_journal_paper_doi               10.1039/b004251j
_journal_year                    2000
_chemical_formula_moiety         'C10 H7 Cr N O4 S3'
_chemical_formula_sum            'C10 H7 Cr N O4 S3'
_chemical_formula_weight         353.35
_chemical_name_systematic
;
  Tetracarbonyl(4-methylthiazole-2-carbodithiomethylester)Cr(0)
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.854(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.948(2)
_cell_length_b                   16.647(3)
_cell_length_c                   9.4732(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      12
_cell_volume                     1397.9(5)
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'XTAL3.4 (Hall, King & Stewart,1995)'
_computing_structure_solution    'XTAL3.4 (Hall, King & Stewart,1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'ENRAF-NONIUS CAD4F'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_av_sigmaI/netI    0.009
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2535
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.27
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via psi scan (North et al.,1968)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.44
_refine_diff_density_rms         0.07
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_obs          0.037
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
   w=1/[σ²(Fo²)+(0.0220P)²+0.7200P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.036
_refine_ls_wR_factor_obs         0.036
_reflns_number_total             1941
_cod_data_source_file            b004251j.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 2~1~/n'
_cod_original_formula_sum        'C10 H7 Cr1 N1 O4 S3'
_cod_database_code               7009889
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_thermal_displace_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr Cr 0.27806(5) 0.34655(3) 0.31414(5) 0.0415(2) Uani 1 1 d . . .
S1 S 0.05724(9) 0.39446(6) 0.17785(10) 0.0543(3) Uani 1 1 d . . .
S2 S -0.10308(11) 0.39693(6) 0.58109(11) 0.0632(3) Uani 1 1 d . . .
S3 S -0.23864(10) 0.44590(7) 0.26990(14) 0.0743(4) Uani 1 1 d . . .
N N 0.1394(3) 0.36122(15) 0.4790(3) 0.0419(6) Uani 1 1 d . . .
O1 O 0.5729(3) 0.28691(18) 0.4658(3) 0.0706(7) Uani 1 1 d . . .
O2 O 0.4239(3) 0.3279(2) 0.0505(3) 0.0809(9) Uani 1 1 d . . .
O3 O 0.1985(3) 0.17976(17) 0.3079(3) 0.0745(8) Uani 1 1 d . . .
O4 O 0.4264(3) 0.5108(2) 0.3347(4) 0.090(1) Uani 1 1 d . . .
C1 C 0.4573(4) 0.3111(2) 0.4144(4) 0.0486(8) Uani 1 1 d . . .
C2 C 0.3656(4) 0.3347(2) 0.1518(4) 0.0539(9) Uani 1 1 d . . .
C3 C 0.2218(4) 0.2368(2) 0.3066(4) 0.0490(8) Uani 1 1 d . . .
C4 C 0.3650(4) 0.4510(2) 0.3308(4) 0.0557(9) Uani 1 1 d . . .
C5 C 0.0003(4) 0.38944(18) 0.4418(4) 0.0450(8) Uani 1 1 d . . .
C6 C 0.0461(4) 0.3608(2) 0.6922(4) 0.0611(10) Uani 1 1 d . . .
H6 H 0.04643 0.3532 0.7905 0.07337 Uiso 1 1 calc R . .
C7 C 0.1649(4) 0.3443(2) 0.6226(4) 0.0507(9) Uani 1 1 d . . .
C8 C 0.3111(5) 0.3107(3) 0.691(10) 0.0755(12) Uani 1 1 d . . .
H8A H 0.3776 0.3040 0.6201 0.075 Uiso 1 1 calc R . .
H8B H 0.2941 0.2596 0.7326 0.075 Uiso 1 1 calc R . .
H8C H 0.3561 0.3468 0.7634 0.075 Uiso 1 1 calc R . .
C9 C -0.0567(3) 0.4093(2) 0.2987(4) 0.0300(16) Uani 1 1 d . . .
C10 C -0.2650(5) 0.4708(3) 0.0866(5) 0.053(2) Uani 1 1 d . . .
H10A H -0.3646 0.4920 0.0605 0.135 Uiso 1 1 calc R . .
H10B H -0.2528 0.4235 0.0313 0.135 Uiso 1 1 calc R . .
H10C H -0.1918 0.5103 0.0684 0.135 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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
C2 Cr C1 87.49(15) . . ?
C2 Cr C3 90.34(15) . . ?
C1 Cr C3 85.35(15) . . ?
C2 Cr C4 87.22(16) . . ?
C1 Cr C4 86.11(15) . . ?
C3 Cr C4 171.21(14) . . ?
C2 Cr N 169.96(13) . . ?
C1 Cr N 102.19(13) . . ?
C3 Cr N 87.72(12) . . ?
C4 Cr N 96.11(13) . . ?
C2 Cr S1 89.95(11) . . ?
C1 Cr S1 177.02(11) . . ?
C3 Cr S1 96.19(11) . . ?
C4 Cr S1 92.25(11) . . ?
N Cr S1 80.45(8) . . ?
C9 S1 Cr 102.85(13) . . ?
C6 S2 C5 89.44(17) . . ?
C9 S3 C10 103.5(2) . . ?
C5 N C7 110.8(3) . . ?
C5 N Cr 117.5(2) . . ?
C7 N Cr 131.6(2) . . ?
O1 C1 Cr 174.0(3) . . ?
O2 C2 Cr 178.5(3) . . ?
O3 C3 Cr 174.8(3) . . ?
O4 C4 Cr 174.11(3) . . ?
N C5 C9 122.3(3) . . ?
N C5 S2 113.9(3) . . ?
C9 C5 S2 123.8(2) . . ?
C7 C6 S2 112.0(3) . . ?
C7 C6 H6 124.02 . . ?
S2 C6 H6 124.02 . . ?
C6 C7 N 113.9(3) . . ?
C6 C7 C8 124.59(4) . . ?
N C7 C8 121.5(3) . . ?
C7 C8 H8A 109.47 . . ?
C7 C8 H8B 109.47 . . ?
H8A C8 H8B 109.47 . . ?
C7 C8 H8C 109.47 . . ?
H8A C8 H8C 109.47 . . ?
H8B C8 H8C 109.47 . . ?
C5 C9 S1 116.9(2) . . ?
C5 C9 S3 116.1(3) . . ?
S1 C9 S3 127.0(2) . . ?
S3 C10 H10A 109.47 . . ?
S3 C10 H10B 109.47 . . ?
H10A C10 H10B 109.47 . . ?
S3 C10 H10C 109.47 . . ?
H10A C10 H10C 109.47 . . ?
H10B C10 H10C 109.47 . . ?
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
Cr C2 1.830(4) . ?
Cr C1 1.845(4) . ?
Cr C3 1.895(4) . ?
Cr C4 1.902(4) . ?
Cr N 2.137(3) . ?
Cr S1 2.3474(11) . ?
S1 C9 1.652(4) . ?
S2 C6 1.694(4) . ?
S2 C5 1.716(3) . ?
S3 C9 1.725(3) . ?
S3 C10 1.770(5) . ?
N C5 1.333(4) . ?
N C7 1.377(4) . ?
O1 C1 1.154(4) . ?
O2 C2 1.158(4) . ?
O3 C3 1.135(4) . ?
O4 C4 1.136(4) . ?
C5 C9 1.421(5) . ?
C6 C7 1.353(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.487(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
