#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/98/7009890.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_7009890
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         'C12 H7 Fe N O3 S3'
_chemical_formula_sum            'C12 H7 Fe N O3 S3'
_chemical_formula_weight         365.23
_chemical_name_systematic
;
  Tricarbonyl(benzothiazole-2-carbodithiomethylester)Fe(0)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.38(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.312(2)
_cell_length_b                   7.317(3)
_cell_length_c                   10.741(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      12
_cell_volume                     729.7(4)
_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  0.033
_diffrn_reflns_av_sigmaI/netI    0.014
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2752
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via psi scan (North et al.,1968)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.07
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_obs          0.034
_refine_ls_shift/esd_max         0.011
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
   w=1/[σ²(Fo²)+(0.0220P)²+0.72P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.031
_reflns_number_total             1845
_cod_data_source_file            b004251j.txt
_cod_data_source_block           2
_cod_original_cell_volume        729.6(4)
_cod_original_sg_symbol_H-M      'P 2~1~'
_cod_original_formula_sum        'C12 H7 Fe1 N1 O3 S3'
_cod_database_code               7009890
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.7510(1) 0.2449(1) 0.7534(1) 0.07328 Uani 1 d . . .
S1 S 0.9358(1) 0.2473(2) 0.8925(1) 0.08489 Uani 1 d . . .
S2 S 1.1580(1) 0.2452(2) 0.5605(1) 0.06561 Uani 1 d . . .
S3 S 1.2553(2) 0.2383(1) 0.8571(1) 0.09193 Uani 1 d . . .
O1 O 0.5797(4) -0.0542(3) 0.6337(4) 0.13060 Uani 1 d . . .
O2 O 0.5884(3) 0.2794(3) 0.9718(3) 0.14476 Uani 1 d . . .
O3 O 0.5897(3) 0.5545(3) 0.6546(4) 0.10467 Uani 1 d . . .
N N 0.8980(4) 0.2540(4) 0.6326(4) 0.05604 Uani 1 d . . .
C1 C 0.6504(4) 0.0548(3) 0.6802(4) 0.08135 Uani 1 d . . .
C2 C 0.6481(4) 0.2635(4) 0.8835(5) 0.11202 Uani 1 d . . .
C3 C 0.6521(5) 0.4304(4) 0.6899(5) 0.09206 Uani 1 d . . .
C4 C 1.0370(4) 0.2511(4) 0.6744(4) 0.05545 Uani 1 d . . .
C5 C 1.0145(4) 0.2452(3) 0.4480(5) 0.06283 Uani 1 d . . .
C6 C 0.8834(5) 0.2448(4) 0.5018(5) 0.05444 Uani 1 d . . .
C7 C 0.7553(4) 0.2544(4) 0.4263(4) 0.06472 Uani 1 d . . .
H7 H 0.6676 0.2689 0.4611 0.07767 Uiso 1 calc R . .
C8 C 0.7615(4) 0.2421(3) 0.2999(4) 0.08008 Uani 1 d . . .
H8 H 0.6781 0.2185 0.2492 0.09609 Uiso 1 calc R . .
C9 C 0.8924(5) 0.2648(4) 0.2462(5) 0.04930 Uani 1 d . . .
H9 H 0.8931 0.2823 0.1605 0.05916 Uiso 1 calc R . .
C10 C 1.0204(4) 0.2614(3) 0.3195(5) 0.06989 Uani 1 d . . .
H10 H 1.1082 0.2697 0.2841 0.08386 Uiso 1 calc R . .
C11 C 1.0750(5) 0.2470(3) 0.8020(5) 0.06499 Uani 1 d . . .
C12 C 1.2462(4) 0.2585(4) 1.0184(5) 0.10961 Uani 1 d . . .
H12A H 1.3366 0.2227 1.0602 0.16442 Uiso 1 calc R . .
H12B H 1.1711 0.1809 1.0447 0.16442 Uiso 1 calc R . .
H12C H 1.2259 0.3831 1.0389 0.16442 Uiso 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'
Fe Fe 0.3463 0.8444 '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
C3 Fe C2 87.0(5) . . ?
C3 Fe C1 100.8(3) . . ?
C1 Fe C2 96.2(5) . . ?
C3 Fe N 95.1(4) . . ?
C2 Fe N 167.1(9) . . ?
C1 Fe N 95.9(3) . . ?
C3 Fe S1 128.5(8) . . ?
C2 Fe S1 84.5(2) . . ?
C1 Fe S1 130.7(7) . . ?
N Fe S1 84.2(1) . . ?
C11 S1 Fe 101.9(2) . . ?
C11 S3 C12 102.5(3) . . ?
C4 S2 C5 89.08(18) . . ?
C4 N C6 110.7(3) . . ?
C4 N Fe 119.0(3) . . ?
C6 N Fe 130.0(3) . . ?
C4 C11 S1 114.9(3) . . ?
C4 C11 S3 120.2(3) . . ?
S1 C11 S3 124.9(2) . . ?
S3 C12 H12A 109.47 . . ?
S3 C12 H12B 109.47 . . ?
H1 C12 H12B 109.47 . . ?
S3 C12 H12C 109.47 . . ?
H12A C12 H12C 109.47 . . ?
H12B C12 H12C 109.47 . . ?
N C4 C11 119.9(4) . . ?
N C4 S3 115.5(3) . . ?
C11 C4 S3 124.6(3) . . ?
C6 C5 C10 121.0(4) . . ?
C6 C5 S3 111.4(2) . . ?
C10 C5 S3 127.3(5) . . ?
C5 C6 C7 119.9(3) . . ?
C5 C6 N 113.3(3) . . ?
C7 C6 N 126.5(4) . . ?
C8 C7 C6 118.4(5) . . ?
C8 C7 H7 120.78 . . ?
C6 C7 H7 120.78 . . ?
C7 C8 C9 120.4(5) . . ?
C7 C8 H8 119.78 . . ?
C9 C8 H8 119.78 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.81 . . ?
C8 C9 H9 119.81 . . ?
C9 C10 C5 118.1(5) . . ?
C9 C10 H10 120.96 . . ?
C5 C10 H10 120.96 . . ?
O1 C1 Fe 174.9(7) . . ?
O2 C2 Fe 176.0(10) . . ?
O3 C3 Fe 176.5(7) . . ?
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
Fe C3 1.750(2) . ?
Fe C2 1.759(8) . ?
Fe C1 1.820(2) . ?
Fe N 1.958(4) . ?
Fe S1 2.191(1) . ?
S1 C11 1.678(5) . ?
S3 C11 1.738(4) . ?
S3 C12 1.747(6) . ?
S2 C4 1.726(5) . ?
S2 C5 1.732(5) . ?
O2 C2 1.141(6) . ?
O1 C1 1.126(5) . ?
O3 C3 1.128(6) . ?
N C4 1.337(5) . ?
N C6 1.402(6) . ?
C11 C4 1.389(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C5 C6 1.390(6) . ?
C5 C10 1.391(5) . ?
C6 C7 1.392(6) . ?
C7 C8 1.366(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.398(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.378(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
