#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313659.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_4313659
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            'C21 H21 Mn Mo O9 S2'
_chemical_formula_weight         632.38
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.7140(10)
_cell_angle_beta                 66.0920(10)
_cell_angle_gamma                74.8760(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2318(7)
_cell_length_b                   11.8012(8)
_cell_length_c                   12.0221(8)
_cell_measurement_reflns_used    4734
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.43
_cell_volume                     1218.05(14)
_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      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10985
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.917899
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0258
_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)+(0.0341P)²+0.3140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                4275
_reflns_number_total             4801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030034i_10.cif
_cod_data_source_block           ksmomnds
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4313659
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_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 0.45988(4) 0.84062(3) 0.23911(3) 0.03403(9) Uani 1 1 d . . .
Mo1 Mo 0.68054(2) 0.767831(17) 0.329668(17) 0.03108(7) Uani 1 1 d . . .
S1 S 0.70094(6) 0.84843(5) 0.10082(5) 0.03361(13) Uani 1 1 d . . .
S2 S 0.55641(6) 0.62952(5) 0.30156(5) 0.03538(13) Uani 1 1 d . . .
C1 C 0.8274(3) 0.7797(3) 0.4258(2) 0.0461(6) Uani 1 1 d . . .
C2 C 0.7979(3) 0.6559(3) 0.4776(3) 0.0527(7) Uani 1 1 d . . .
C3 C 0.8591(3) 0.6012(2) 0.3782(3) 0.0492(6) Uani 1 1 d . . .
C4 C 0.9272(3) 0.6903(2) 0.2645(3) 0.0436(6) Uani 1 1 d . . .
C5 C 0.9062(2) 0.8031(2) 0.2924(2) 0.0404(5) Uani 1 1 d . . .
C10 C 0.4146(3) 1.0050(2) 0.1966(2) 0.0417(6) Uani 1 1 d . . .
C11 C 0.2898(3) 0.8299(3) 0.3669(3) 0.0475(6) Uani 1 1 d . . .
C12 C 0.3856(3) 0.8275(2) 0.1331(3) 0.0451(6) Uani 1 1 d . . .
C20 C 0.6203(3) 0.9446(3) 0.3161(3) 0.0477(6) Uani 1 1 d . . .
C21 C 0.5076(3) 0.7499(3) 0.4911(3) 0.0464(6) Uani 1 1 d . . .
C31 C 0.7997(3) 0.8669(4) 0.5002(3) 0.0755(11) Uani 1 1 d . . .
H31A H 0.7188 0.8461 0.5777 0.113 Uiso 1 1 calc R . .
H31B H 0.7794 0.9501 0.4493 0.113 Uiso 1 1 calc R . .
H31C H 0.8834 0.8601 0.5207 0.113 Uiso 1 1 calc R . .
C32 C 0.7331(4) 0.5865(4) 0.6180(3) 0.0926(14) Uani 1 1 d . . .
H32A H 0.8088 0.5389 0.6507 0.139 Uiso 1 1 calc R . .
H32B H 0.6707 0.5324 0.6283 0.139 Uiso 1 1 calc R . .
H32C H 0.6788 0.6443 0.6643 0.139 Uiso 1 1 calc R . .
C33 C 0.8608(4) 0.4684(3) 0.3938(4) 0.0846(12) Uani 1 1 d . . .
H33A H 0.8795 0.4599 0.3122 0.127 Uiso 1 1 calc R . .
H33B H 0.7689 0.4421 0.4517 0.127 Uiso 1 1 calc R . .
H33C H 0.9348 0.4183 0.4275 0.127 Uiso 1 1 calc R . .
C34 C 1.0225(3) 0.6678(3) 0.1396(3) 0.0658(9) Uani 1 1 d . . .
H34A H 1.1205 0.6455 0.1375 0.099 Uiso 1 1 calc R . .
H34B H 1.0158 0.7415 0.0703 0.099 Uiso 1 1 calc R . .
H34C H 0.9922 0.6019 0.1312 0.099 Uiso 1 1 calc R . .
C35 C 0.9727(3) 0.9177(3) 0.2009(3) 0.0659(8) Uani 1 1 d . . .
H35A H 0.9154 0.9879 0.2269 0.099 Uiso 1 1 calc R . .
H35B H 0.9768 0.9281 0.1164 0.099 Uiso 1 1 calc R . .
H35C H 1.0684 0.9104 0.2007 0.099 Uiso 1 1 calc R . .
C41 C 1.0025(3) 0.8049(3) -0.2627(2) 0.0541(7) Uani 1 1 d . . .
H41A H 0.9790 0.7481 -0.2896 0.081 Uiso 1 1 calc R . .
H41B H 1.1015 0.7848 -0.2680 0.081 Uiso 1 1 calc R . .
H41C H 0.9876 0.8874 -0.3173 0.081 Uiso 1 1 calc R . .
C42 C 0.8272(2) 0.7069(2) -0.0721(2) 0.0355(5) Uani 1 1 d . . .
C43 C 0.7351(2) 0.7096(2) 0.0595(2) 0.0326(5) Uani 1 1 d . . .
C44 C 0.6717(2) 0.6140(2) 0.1488(2) 0.0328(5) Uani 1 1 d . . .
C45 C 0.6911(3) 0.4903(2) 0.1324(2) 0.0374(5) Uani 1 1 d . . .
C46 C 0.5797(4) 0.3586(3) 0.1024(3) 0.0645(9) Uani 1 1 d . . .
H46A H 0.6451 0.3605 0.0178 0.097 Uiso 1 1 calc R . .
H46B H 0.4855 0.3488 0.1110 0.097 Uiso 1 1 calc R . .
H46C H 0.6130 0.2906 0.1642 0.097 Uiso 1 1 calc R . .
O4 O 0.91136(18) 0.79642(15) -0.13247(15) 0.0422(4) Uani 1 1 d . . .
O5 O 0.8235(2) 0.63388(17) -0.11753(17) 0.0508(5) Uani 1 1 d . . .
O6 O 0.7962(2) 0.41771(17) 0.1312(2) 0.0583(5) Uani 1 1 d . . .
O7 O 0.57317(19) 0.47305(16) 0.12390(18) 0.0481(4) Uani 1 1 d . . .
O10 O 0.3824(2) 1.10975(18) 0.1738(2) 0.0638(6) Uani 1 1 d . . .
O11 O 0.1784(2) 0.8304(2) 0.4454(2) 0.0739(6) Uani 1 1 d . . .
O12 O 0.3372(2) 0.8187(2) 0.0667(2) 0.0715(6) Uani 1 1 d . . .
O20 O 0.5960(3) 1.04528(19) 0.3155(2) 0.0741(7) Uani 1 1 d . . .
O21 O 0.4144(2) 0.7397(2) 0.58530(19) 0.0684(6) 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
C11 Mn1 C10 87.54(12) . . ?
C11 Mn1 C12 92.23(12) . . ?
C10 Mn1 C12 93.10(12) . . ?
C11 Mn1 S1 169.36(9) . . ?
C10 Mn1 S1 94.31(8) . . ?
C12 Mn1 S1 98.12(8) . . ?
C11 Mn1 S2 97.49(9) . . ?
C10 Mn1 S2 169.36(8) . . ?
C12 Mn1 S2 96.06(9) . . ?
S1 Mn1 S2 79.06(2) . . ?
C11 Mn1 Mo1 111.17(9) . . ?
C10 Mn1 Mo1 110.90(8) . . ?
C12 Mn1 Mo1 146.50(8) . . ?
S1 Mn1 Mo1 58.410(17) . . ?
S2 Mn1 Mo1 58.539(16) . . ?
C20 Mo1 C21 81.56(12) . . ?
C20 Mo1 C5 86.35(10) . . ?
C21 Mo1 C5 128.83(9) . . ?
C20 Mo1 C1 83.79(10) . . ?
C21 Mo1 C1 92.84(10) . . ?
C5 Mo1 C1 36.27(9) . . ?
C20 Mo1 C2 114.99(11) . . ?
C21 Mo1 C2 81.39(10) . . ?
C5 Mo1 C2 59.51(9) . . ?
C1 Mo1 C2 35.54(10) . . ?
C20 Mo1 C4 120.28(10) . . ?
C21 Mo1 C4 138.93(10) . . ?
C5 Mo1 C4 36.01(9) . . ?
C1 Mo1 C4 59.37(9) . . ?
C2 Mo1 C4 58.24(9) . . ?
C20 Mo1 C3 141.75(10) . . ?
C21 Mo1 C3 106.42(11) . . ?
C5 Mo1 C3 59.12(9) . . ?
C1 Mo1 C3 58.87(10) . . ?
C2 Mo1 C3 34.90(10) . . ?
C4 Mo1 C3 34.55(9) . . ?
C20 Mo1 S1 81.78(8) . . ?
C21 Mo1 S1 131.40(8) . . ?
C5 Mo1 S1 95.08(6) . . ?
C1 Mo1 S1 130.00(7) . . ?
C2 Mo1 S1 146.42(7) . . ?
C4 Mo1 S1 88.23(7) . . ?
C3 Mo1 S1 114.73(7) . . ?
C20 Mo1 S2 127.31(8) . . ?
C21 Mo1 S2 80.49(7) . . ?
C5 Mo1 S2 141.10(6) . . ?
C1 Mo1 S2 146.02(8) . . ?
C2 Mo1 S2 110.60(8) . . ?
C4 Mo1 S2 105.34(6) . . ?
C3 Mo1 S2 90.91(7) . . ?
S1 Mo1 S2 74.324(19) . . ?
C20 Mo1 Mn1 73.68(8) . . ?
C21 Mo1 Mn1 77.75(8) . . ?
C5 Mo1 Mn1 144.44(7) . . ?
C1 Mo1 Mn1 156.55(7) . . ?
C2 Mo1 Mn1 155.94(7) . . ?
C4 Mo1 Mn1 138.94(6) . . ?
C3 Mo1 Mn1 144.31(7) . . ?
S1 Mo1 Mn1 53.777(16) . . ?
S2 Mo1 Mn1 54.222(16) . . ?
C43 S1 Mn1 100.56(7) . . ?
C43 S1 Mo1 102.65(7) . . ?
Mn1 S1 Mo1 67.813(17) . . ?
C44 S2 Mn1 99.99(8) . . ?
C44 S2 Mo1 101.94(7) . . ?
Mn1 S2 Mo1 67.239(18) . . ?
C2 C1 C5 107.9(2) . . ?
C2 C1 C31 126.5(3) . . ?
C5 C1 C31 125.1(3) . . ?
C2 C1 Mo1 74.05(14) . . ?
C5 C1 Mo1 71.65(13) . . ?
C31 C1 Mo1 126.45(19) . . ?
C1 C2 C3 108.5(2) . . ?
C1 C2 C32 126.1(3) . . ?
C3 C2 C32 124.7(3) . . ?
C1 C2 Mo1 70.41(14) . . ?
C3 C2 Mo1 74.13(15) . . ?
C32 C2 Mo1 128.6(2) . . ?
C4 C3 C2 108.1(2) . . ?
C4 C3 C33 126.0(3) . . ?
C2 C3 C33 125.8(3) . . ?
C4 C3 Mo1 71.86(14) . . ?
C2 C3 Mo1 70.96(15) . . ?
C33 C3 Mo1 126.41(19) . . ?
C3 C4 C5 108.2(2) . . ?
C3 C4 C34 126.2(3) . . ?
C5 C4 C34 125.2(3) . . ?
C3 C4 Mo1 73.59(14) . . ?
C5 C4 Mo1 69.28(13) . . ?
C34 C4 Mo1 128.99(18) . . ?
C1 C5 C4 107.2(2) . . ?
C1 C5 C35 126.9(2) . . ?
C4 C5 C35 125.5(2) . . ?
C1 C5 Mo1 72.08(13) . . ?
C4 C5 Mo1 74.71(13) . . ?
C35 C5 Mo1 124.85(19) . . ?
O10 C10 Mn1 177.6(2) . . ?
O11 C11 Mn1 175.9(3) . . ?
O12 C12 Mn1 179.3(3) . . ?
O20 C20 Mo1 172.1(2) . . ?
O21 C21 Mo1 176.5(2) . . ?
O5 C42 O4 124.9(2) . . ?
O5 C42 C43 123.6(2) . . ?
O4 C42 C43 111.49(19) . . ?
C44 C43 C42 122.6(2) . . ?
C44 C43 S1 117.30(17) . . ?
C42 C43 S1 120.05(16) . . ?
C43 C44 C45 124.5(2) . . ?
C43 C44 S2 118.96(17) . . ?
C45 C44 S2 116.49(16) . . ?
O6 C45 O7 125.5(2) . . ?
O6 C45 C44 124.2(2) . . ?
O7 C45 C44 110.3(2) . . ?
C42 O4 C41 116.26(19) . . ?
C45 O7 C46 115.9(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
Mn1 C11 1.790(3) . ?
Mn1 C10 1.792(3) . ?
Mn1 C12 1.795(3) . ?
Mn1 S1 2.3526(7) . ?
Mn1 S2 2.3757(7) . ?
Mn1 Mo1 2.7003(4) . ?
Mo1 C20 1.978(3) . ?
Mo1 C21 2.011(3) . ?
Mo1 C5 2.286(2) . ?
Mo1 C1 2.292(2) . ?
Mo1 C2 2.339(3) . ?
Mo1 C4 2.358(2) . ?
Mo1 C3 2.380(3) . ?
Mo1 S1 2.4841(6) . ?
Mo1 S2 2.4978(6) . ?
S1 C43 1.798(2) . ?
S2 C44 1.784(2) . ?
C1 C2 1.414(4) . ?
C1 C5 1.425(3) . ?
C1 C31 1.510(4) . ?
C2 C3 1.416(4) . ?
C2 C32 1.513(4) . ?
C3 C4 1.407(4) . ?
C3 C33 1.503(4) . ?
C4 C5 1.437(3) . ?
C4 C34 1.502(4) . ?
C5 C35 1.499(4) . ?
C10 O10 1.147(3) . ?
C11 O11 1.149(3) . ?
C12 O12 1.142(3) . ?
C20 O20 1.146(3) . ?
C21 O21 1.134(3) . ?
C41 O4 1.441(3) . ?
C42 O5 1.197(3) . ?
C42 O4 1.331(3) . ?
C42 C43 1.485(3) . ?
C43 C44 1.321(3) . ?
C44 C45 1.498(3) . ?
C45 O6 1.186(3) . ?
C45 O7 1.324(3) . ?
C46 O7 1.449(3) . ?
