#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313650.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_4313650
loop_
_publ_author_name
'Richard D. Adams'
'Burjor Captain'
'O-Sung Kwon'
'Shaobin Miao'
_publ_section_title
;
 New Disulfido Molybdenum-Manganese Complexes Exhibit Facile Addition of
 Small Molecules to the Sulfur Atoms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3356
_journal_page_last               3365
_journal_paper_doi               10.1021/ic030034i
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H5 Mn Mo O5 S2'
_chemical_formula_weight         420.14
_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                 98.005(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0575(11)
_cell_length_b                   8.2471(8)
_cell_length_c                   14.5820(15)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.21
_cell_measurement_theta_min      2.49
_cell_volume                     1316.8(2)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7693
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.877902
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0403
_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)+(0.0291P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                1721
_reflns_number_total             2327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030034i_01.cif
_cod_data_source_block           miaomoms
_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               4313650
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
Mn1 Mn 0.70839(7) 0.54802(9) 0.36786(6) 0.0366(2) Uani 1 1 d . . .
Mo1 Mo 0.72800(4) 0.72167(5) 0.53764(3) 0.03368(15) Uani 1 1 d . . .
S1 S 0.65194(14) 0.81400(17) 0.38147(11) 0.0440(4) Uani 1 1 d . . .
S2 S 0.54459(13) 0.64437(18) 0.43264(11) 0.0440(4) Uani 1 1 d . . .
C1 C 0.6728(6) 0.9715(7) 0.5967(5) 0.0567(17) Uani 1 1 d . . .
H1 H 0.6397 1.0559 0.5590 0.068 Uiso 1 1 calc R . .
C2 C 0.6062(6) 0.8538(8) 0.6353(5) 0.0588(18) Uani 1 1 d . . .
H2 H 0.5216 0.8448 0.6280 0.071 Uiso 1 1 calc R . .
C3 C 0.6898(8) 0.7508(8) 0.6873(4) 0.067(2) Uani 1 1 d . . .
H3 H 0.6707 0.6609 0.7210 0.081 Uiso 1 1 calc R . .
C4 C 0.8077(7) 0.8073(9) 0.6798(5) 0.068(2) Uani 1 1 d . . .
H4 H 0.8805 0.7615 0.7077 0.082 Uiso 1 1 calc R . .
C5 C 0.7965(6) 0.9442(8) 0.6230(5) 0.0620(19) Uani 1 1 d . . .
H5 H 0.8603 1.0057 0.6059 0.074 Uiso 1 1 calc R . .
C10 C 0.7181(5) 0.3372(7) 0.3941(4) 0.0459(15) Uani 1 1 d . . .
C11 C 0.8556(6) 0.5486(7) 0.3307(4) 0.0490(16) Uani 1 1 d . . .
C12 C 0.6364(5) 0.5048(7) 0.2538(5) 0.0497(16) Uani 1 1 d . . .
C20 C 0.8972(5) 0.7145(7) 0.5068(4) 0.0443(14) Uani 1 1 d . . .
C21 C 0.7614(5) 0.4926(7) 0.5724(4) 0.0421(14) Uani 1 1 d . . .
O10 O 0.7227(4) 0.2007(5) 0.4097(3) 0.0731(14) Uani 1 1 d . . .
O11 O 0.9500(4) 0.5450(6) 0.3057(3) 0.0784(15) Uani 1 1 d . . .
O12 O 0.5907(4) 0.4732(6) 0.1800(4) 0.0809(16) Uani 1 1 d . . .
O20 O 0.9981(4) 0.7183(6) 0.4968(3) 0.0683(13) Uani 1 1 d . . .
O21 O 0.7813(4) 0.3646(5) 0.6017(3) 0.0543(11) 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'
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
C12 Mn1 C10 90.6(3) . . ?
C12 Mn1 C11 91.4(3) . . ?
C10 Mn1 C11 92.2(3) . . ?
C12 Mn1 S1 100.41(19) . . ?
C10 Mn1 S1 157.4(2) . . ?
C11 Mn1 S1 107.09(19) . . ?
C12 Mn1 S2 100.26(19) . . ?
C10 Mn1 S2 106.06(19) . . ?
C11 Mn1 S2 158.08(19) . . ?
S1 Mn1 S2 52.77(6) . . ?
C12 Mn1 Mo1 152.39(19) . . ?
C10 Mn1 Mo1 108.05(19) . . ?
C11 Mn1 Mo1 107.50(19) . . ?
S1 Mn1 Mo1 55.40(4) . . ?
S2 Mn1 Mo1 55.71(4) . . ?
C21 Mo1 C20 83.2(2) . . ?
C21 Mo1 C4 91.6(3) . . ?
C20 Mo1 C4 87.5(3) . . ?
C21 Mo1 C5 126.2(3) . . ?
C20 Mo1 C5 84.0(2) . . ?
C4 Mo1 C5 35.8(2) . . ?
C21 Mo1 C3 84.7(2) . . ?
C20 Mo1 C3 121.5(3) . . ?
C4 Mo1 C3 36.0(2) . . ?
C5 Mo1 C3 59.2(2) . . ?
C21 Mo1 C1 142.5(2) . . ?
C20 Mo1 C1 114.3(2) . . ?
C4 Mo1 C1 58.3(2) . . ?
C5 Mo1 C1 34.8(2) . . ?
C3 Mo1 C1 57.8(2) . . ?
C21 Mo1 C2 112.8(2) . . ?
C20 Mo1 C2 141.8(2) . . ?
C4 Mo1 C2 58.8(3) . . ?
C5 Mo1 C2 58.3(2) . . ?
C3 Mo1 C2 35.0(2) . . ?
C1 Mo1 C2 34.2(2) . . ?
C21 Mo1 S1 124.48(18) . . ?
C20 Mo1 S1 90.64(17) . . ?
C4 Mo1 S1 143.4(2) . . ?
C5 Mo1 S1 107.6(2) . . ?
C3 Mo1 S1 140.5(2) . . ?
C1 Mo1 S1 89.72(17) . . ?
C2 Mo1 S1 105.56(19) . . ?
C21 Mo1 S2 91.17(17) . . ?
C20 Mo1 S2 125.12(17) . . ?
C4 Mo1 S2 147.3(2) . . ?
C5 Mo1 S2 137.06(19) . . ?
C3 Mo1 S2 112.1(2) . . ?
C1 Mo1 S2 102.88(17) . . ?
C2 Mo1 S2 90.29(18) . . ?
S1 Mo1 S2 49.40(5) . . ?
C21 Mo1 Mn1 74.40(18) . . ?
C20 Mo1 Mn1 75.39(16) . . ?
C4 Mo1 Mn1 158.92(19) . . ?
C5 Mo1 Mn1 149.08(19) . . ?
C3 Mo1 Mn1 151.68(18) . . ?
C1 Mo1 Mn1 140.36(17) . . ?
C2 Mo1 Mn1 141.08(18) . . ?
S1 Mo1 Mn1 50.87(4) . . ?
S2 Mo1 Mn1 50.82(4) . . ?
S2 S1 Mn1 63.65(6) . . ?
S2 S1 Mo1 65.61(6) . . ?
Mn1 S1 Mo1 73.73(5) . . ?
S1 S2 Mn1 63.58(6) . . ?
S1 S2 Mo1 64.99(6) . . ?
Mn1 S2 Mo1 73.47(5) . . ?
C2 C1 C5 109.5(6) . . ?
C2 C1 Mo1 73.4(3) . . ?
C5 C1 Mo1 70.2(3) . . ?
C1 C2 C3 107.3(6) . . ?
C1 C2 Mo1 72.4(3) . . ?
C3 C2 Mo1 70.0(3) . . ?
C2 C3 C4 107.9(6) . . ?
C2 C3 Mo1 75.1(4) . . ?
C4 C3 Mo1 70.3(4) . . ?
C5 C4 C3 108.0(6) . . ?
C5 C4 Mo1 73.5(4) . . ?
C3 C4 Mo1 73.7(4) . . ?
C1 C5 C4 107.3(6) . . ?
C1 C5 Mo1 75.0(4) . . ?
C4 C5 Mo1 70.7(4) . . ?
O10 C10 Mn1 178.7(6) . . ?
O11 C11 Mn1 178.2(5) . . ?
O12 C12 Mn1 178.4(6) . . ?
O20 C20 Mo1 173.4(5) . . ?
O21 C21 Mo1 173.1(5) . . ?
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
Mn1 C12 1.776(7) . ?
Mn1 C10 1.780(6) . ?
Mn1 C11 1.785(7) . ?
Mn1 S1 2.2968(16) . ?
Mn1 S2 2.2981(16) . ?
Mn1 Mo1 2.8421(10) . ?
Mo1 C21 1.977(6) . ?
Mo1 C20 1.985(6) . ?
Mo1 C4 2.250(7) . ?
Mo1 C5 2.286(6) . ?
Mo1 C3 2.293(6) . ?
Mo1 C1 2.346(6) . ?
Mo1 C2 2.358(6) . ?
Mo1 S1 2.4372(16) . ?
Mo1 S2 2.4492(16) . ?
S1 S2 2.042(2) . ?
C1 C2 1.384(8) . ?
C1 C5 1.387(8) . ?
C2 C3 1.398(9) . ?
C3 C4 1.403(9) . ?
C4 C5 1.395(9) . ?
C10 O10 1.148(6) . ?
C11 O11 1.153(6) . ?
C12 O12 1.154(7) . ?
C20 O20 1.145(6) . ?
C21 O21 1.149(6) . ?
