#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313652.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_4313652
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            'C18 H5 Mn3 Mo O13 S2'
_chemical_formula_weight         754.10
_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                 103.5760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4646(5)
_cell_length_b                   15.8502(9)
_cell_length_c                   16.9337(9)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.56
_cell_volume                     2469.3(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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15852
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0346
_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)+(0.0324P)²+0.3820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4180
_reflns_number_total             4870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030034i_03.cif
_cod_data_source_block           miaocpms
_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               4313652
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 0.51606(5) 0.16177(3) 0.29956(3) 0.02233(13) Uani 1 1 d . . .
Mn2 Mn 0.44855(5) 0.37467(3) 0.14324(3) 0.02035(12) Uani 1 1 d . . .
Mn3 Mn 0.77220(5) 0.24754(3) 0.31500(3) 0.02189(13) Uani 1 1 d . . .
Mo1 Mo 0.44255(3) 0.295746(18) 0.392735(16) 0.01997(9) Uani 1 1 d . . .
S1 S 0.54286(8) 0.30197(5) 0.26986(5) 0.01816(17) Uani 1 1 d . . .
S2 S 0.66770(9) 0.21251(5) 0.41805(5) 0.02235(18) Uani 1 1 d . . .
O10 O 0.4478(3) 0.00683(18) 0.38002(19) 0.0537(8) Uani 1 1 d . . .
O11 O 0.6925(4) 0.06191(18) 0.21200(19) 0.0554(8) Uani 1 1 d . . .
O12 O 0.2745(3) 0.13298(18) 0.15771(16) 0.0483(8) Uani 1 1 d . . .
O20 O 0.3430(3) 0.14471(18) 0.48878(17) 0.0444(7) Uani 1 1 d . . .
O21 O 0.1402(3) 0.2545(2) 0.27729(16) 0.0483(8) Uani 1 1 d . . .
O30 O 0.5116(3) 0.21962(18) 0.05472(16) 0.0445(7) Uani 1 1 d . . .
O31 O 0.7569(3) 0.43237(18) 0.15878(16) 0.0426(7) Uani 1 1 d . . .
O32 O 0.3409(3) 0.47476(16) -0.00678(14) 0.0368(6) Uani 1 1 d . . .
O33 O 0.3881(3) 0.52560(18) 0.23669(16) 0.0487(8) Uani 1 1 d . . .
O34 O 0.1396(3) 0.31724(17) 0.12160(15) 0.0373(6) Uani 1 1 d . . .
O40 O 0.8450(3) 0.24024(19) 0.15455(16) 0.0432(7) Uani 1 1 d . . .
O41 O 1.0106(3) 0.13240(18) 0.38822(18) 0.0489(8) Uani 1 1 d . . .
O42 O 0.9630(3) 0.39135(19) 0.37125(19) 0.0533(8) Uani 1 1 d . . .
C1 C 0.4736(4) 0.3601(2) 0.5165(2) 0.0315(8) Uani 1 1 d . . .
H1 H 0.4918 0.3268 0.5644 0.038 Uiso 1 1 calc R . .
C2 C 0.3344(4) 0.3820(2) 0.4683(2) 0.0357(9) Uani 1 1 d . . .
H2 H 0.2432 0.3672 0.4786 0.043 Uiso 1 1 calc R . .
C3 C 0.3570(4) 0.4301(2) 0.4020(2) 0.0353(9) Uani 1 1 d . . .
H3 H 0.2831 0.4525 0.3591 0.042 Uiso 1 1 calc R . .
C4 C 0.5080(4) 0.4391(2) 0.4105(2) 0.0316(8) Uani 1 1 d . . .
H4 H 0.5535 0.4690 0.3746 0.038 Uiso 1 1 calc R . .
C5 C 0.5799(4) 0.3962(2) 0.4811(2) 0.0301(8) Uani 1 1 d . . .
H5 H 0.6821 0.3922 0.5014 0.036 Uiso 1 1 calc R . .
C10 C 0.4760(4) 0.0674(2) 0.3503(2) 0.0334(9) Uani 1 1 d . . .
C11 C 0.6308(4) 0.1039(2) 0.2480(2) 0.0353(9) Uani 1 1 d . . .
C12 C 0.3665(4) 0.1449(2) 0.2142(2) 0.0313(8) Uani 1 1 d . . .
C20 C 0.3806(4) 0.1970(2) 0.4532(2) 0.0291(8) Uani 1 1 d . . .
C21 C 0.2538(4) 0.2678(3) 0.3170(2) 0.0331(9) Uani 1 1 d . . .
C30 C 0.4875(4) 0.2778(2) 0.0879(2) 0.0276(8) Uani 1 1 d . . .
C31 C 0.6413(4) 0.4115(2) 0.1532(2) 0.0281(8) Uani 1 1 d . . .
C32 C 0.3835(4) 0.4353(2) 0.0494(2) 0.0268(8) Uani 1 1 d . . .
C33 C 0.4115(4) 0.4683(2) 0.2026(2) 0.0306(8) Uani 1 1 d . . .
C34 C 0.2567(4) 0.3369(2) 0.1324(2) 0.0268(8) Uani 1 1 d . . .
C40 C 0.8170(4) 0.2446(2) 0.2173(2) 0.0289(8) Uani 1 1 d . . .
C41 C 0.9187(4) 0.1768(2) 0.3582(2) 0.0311(8) Uani 1 1 d . . .
C42 C 0.8867(4) 0.3357(2) 0.3485(2) 0.0321(9) 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 C11 89.14(18) . . ?
C12 Mn1 C10 92.62(16) . . ?
C11 Mn1 C10 91.54(17) . . ?
C12 Mn1 S1 94.28(11) . . ?
C11 Mn1 S1 106.02(12) . . ?
C10 Mn1 S1 161.20(13) . . ?
C12 Mn1 S2 164.10(13) . . ?
C11 Mn1 S2 105.99(13) . . ?
C10 Mn1 S2 91.82(12) . . ?
S1 Mn1 S2 77.12(3) . . ?
C12 Mn1 Mn3 131.77(12) . . ?
C11 Mn1 Mn3 71.17(12) . . ?
C10 Mn1 Mn3 130.15(12) . . ?
S1 Mn1 Mn3 53.27(2) . . ?
S2 Mn1 Mn3 52.49(3) . . ?
C12 Mn1 Mo1 108.13(12) . . ?
C11 Mn1 Mo1 155.55(12) . . ?
C10 Mn1 Mo1 104.43(13) . . ?
S1 Mn1 Mo1 56.78(2) . . ?
S2 Mn1 Mo1 55.97(2) . . ?
Mn3 Mn1 Mo1 84.385(18) . . ?
C32 Mn2 C33 89.03(15) . . ?
C32 Mn2 C34 87.88(15) . . ?
C33 Mn2 C34 90.36(16) . . ?
C32 Mn2 C30 93.50(15) . . ?
C33 Mn2 C30 177.45(15) . . ?
C34 Mn2 C30 89.40(16) . . ?
C32 Mn2 C31 92.05(15) . . ?
C33 Mn2 C31 90.31(16) . . ?
C34 Mn2 C31 179.32(16) . . ?
C30 Mn2 C31 89.93(15) . . ?
C32 Mn2 S1 176.61(11) . . ?
C33 Mn2 S1 88.74(10) . . ?
C34 Mn2 S1 94.69(10) . . ?
C30 Mn2 S1 88.76(10) . . ?
C31 Mn2 S1 85.41(10) . . ?
C42 Mn3 C41 90.35(16) . . ?
C42 Mn3 C40 93.24(17) . . ?
C41 Mn3 C40 91.87(16) . . ?
C42 Mn3 S2 106.85(13) . . ?
C41 Mn3 S2 88.16(11) . . ?
C40 Mn3 S2 159.91(12) . . ?
C42 Mn3 S1 105.61(12) . . ?
C41 Mn3 S1 161.50(12) . . ?
C40 Mn3 S1 96.42(11) . . ?
S2 Mn3 S1 78.40(3) . . ?
C42 Mn3 Mn1 151.70(13) . . ?
C41 Mn3 Mn1 108.05(12) . . ?
C40 Mn3 Mn1 107.05(11) . . ?
S2 Mn3 Mn1 54.23(3) . . ?
S1 Mn3 Mn1 53.66(2) . . ?
C21 Mo1 C20 80.31(14) . . ?
C21 Mo1 C2 92.40(15) . . ?
C20 Mo1 C2 87.63(15) . . ?
C21 Mo1 C1 126.36(14) . . ?
C20 Mo1 C1 82.66(14) . . ?
C2 Mo1 C1 36.29(13) . . ?
C21 Mo1 C3 88.43(15) . . ?
C20 Mo1 C3 122.15(15) . . ?
C2 Mo1 C3 36.04(13) . . ?
C1 Mo1 C3 59.69(13) . . ?
C21 Mo1 C4 117.81(15) . . ?
C20 Mo1 C4 141.04(13) . . ?
C2 Mo1 C4 59.19(14) . . ?
C1 Mo1 C4 58.62(13) . . ?
C3 Mo1 C4 35.26(13) . . ?
C21 Mo1 C5 146.94(15) . . ?
C20 Mo1 C5 112.45(13) . . ?
C2 Mo1 C5 59.35(14) . . ?
C1 Mo1 C5 35.23(13) . . ?
C3 Mo1 C5 58.74(13) . . ?
C4 Mo1 C5 34.71(12) . . ?
C21 Mo1 S2 127.15(12) . . ?
C20 Mo1 S2 80.75(10) . . ?
C2 Mo1 S2 135.35(10) . . ?
C1 Mo1 S2 99.21(9) . . ?
C3 Mo1 S2 142.31(10) . . ?
C4 Mo1 S2 107.71(10) . . ?
C5 Mo1 S2 85.72(9) . . ?
C21 Mo1 S1 86.03(10) . . ?
C20 Mo1 S1 131.72(11) . . ?
C2 Mo1 S1 139.34(10) . . ?
C1 Mo1 S1 139.27(10) . . ?
C3 Mo1 S1 103.33(10) . . ?
C4 Mo1 S1 85.85(9) . . ?
C5 Mo1 S1 104.07(9) . . ?
S2 Mo1 S1 71.40(3) . . ?
C21 Mo1 Mn1 76.97(11) . . ?
C20 Mo1 Mn1 80.82(10) . . ?
C2 Mo1 Mn1 165.42(11) . . ?
C1 Mo1 Mn1 148.29(9) . . ?
C3 Mo1 Mn1 150.59(9) . . ?
C4 Mo1 Mn1 134.71(10) . . ?
C5 Mo1 Mn1 133.67(9) . . ?
S2 Mo1 Mn1 51.48(2) . . ?
S1 Mo1 Mn1 50.94(2) . . ?
Mn3 S1 Mn1 73.07(3) . . ?
Mn3 S1 Mn2 126.83(4) . . ?
Mn1 S1 Mn2 128.13(4) . . ?
Mn3 S1 Mo1 102.93(3) . . ?
Mn1 S1 Mo1 72.28(3) . . ?
Mn2 S1 Mo1 128.97(4) . . ?
Mn3 S2 Mn1 73.28(3) . . ?
Mn3 S2 Mo1 104.56(3) . . ?
Mn1 S2 Mo1 72.55(3) . . ?
C5 C1 C2 108.4(3) . . ?
C5 C1 Mo1 75.1(2) . . ?
C2 C1 Mo1 71.3(2) . . ?
C3 C2 C1 107.2(3) . . ?
C3 C2 Mo1 72.9(2) . . ?
C1 C2 Mo1 72.4(2) . . ?
C4 C3 C2 108.2(3) . . ?
C4 C3 Mo1 74.6(2) . . ?
C2 C3 Mo1 71.1(2) . . ?
C5 C4 C3 108.3(3) . . ?
C5 C4 Mo1 72.7(2) . . ?
C3 C4 Mo1 70.1(2) . . ?
C4 C5 C1 107.9(3) . . ?
C4 C5 Mo1 72.6(2) . . ?
C1 C5 Mo1 69.7(2) . . ?
O10 C10 Mn1 177.7(4) . . ?
O11 C11 Mn1 173.2(4) . . ?
O12 C12 Mn1 177.2(4) . . ?
O20 C20 Mo1 176.7(3) . . ?
O21 C21 Mo1 175.0(3) . . ?
O30 C30 Mn2 179.7(4) . . ?
O31 C31 Mn2 178.9(4) . . ?
O32 C32 Mn2 177.3(3) . . ?
O33 C33 Mn2 178.4(3) . . ?
O34 C34 Mn2 175.6(3) . . ?
O40 C40 Mn3 178.0(3) . . ?
O41 C41 Mn3 177.6(3) . . ?
O42 C42 Mn3 178.4(3) . . ?
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 1.790(4) . ?
Mn1 C11 1.797(4) . ?
Mn1 C10 1.808(4) . ?
Mn1 S1 2.3054(9) . ?
Mn1 S2 2.3195(9) . ?
Mn1 Mn3 2.7379(7) . ?
Mn1 Mo1 2.8280(6) . ?
Mn2 C32 1.836(4) . ?
Mn2 C33 1.871(4) . ?
Mn2 C34 1.879(4) . ?
Mn2 C30 1.880(4) . ?
Mn2 C31 1.885(4) . ?
Mn2 S1 2.4132(9) . ?
Mn3 C42 1.777(4) . ?
Mn3 C41 1.800(4) . ?
Mn3 C40 1.802(4) . ?
Mn3 S2 2.2675(10) . ?
Mn3 S1 2.2936(9) . ?
Mo1 C21 1.989(4) . ?
Mo1 C20 2.031(4) . ?
Mo1 C2 2.273(4) . ?
Mo1 C1 2.286(3) . ?
Mo1 C3 2.297(4) . ?
Mo1 C4 2.355(4) . ?
Mo1 C5 2.356(3) . ?
Mo1 S2 2.4569(9) . ?
Mo1 S1 2.4836(8) . ?
O10 C10 1.145(4) . ?
O11 C11 1.150(5) . ?
O12 C12 1.148(4) . ?
O20 C20 1.129(4) . ?
O21 C21 1.146(4) . ?
O30 C30 1.130(4) . ?
O31 C31 1.126(4) . ?
O32 C32 1.130(4) . ?
O33 C33 1.126(4) . ?
O34 C34 1.125(4) . ?
O40 C40 1.157(4) . ?
O41 C41 1.141(4) . ?
O42 C42 1.148(4) . ?
C1 C5 1.407(5) . ?
C1 C2 1.420(5) . ?
C2 C3 1.414(5) . ?
C3 C4 1.410(5) . ?
C4 C5 1.405(5) . ?
