#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:55:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179161 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/22/4312220.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_4312220
loop_
_publ_author_name
'Richard D. Adams'
'Shaobin Miao'
_publ_section_title
;
 Metal Carbonyl Derivatives of Sulfur-Containing Quinones and
 Hydroquinones: Synthesis, Structures, and Electrochemical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8414
_journal_page_last               8426
_journal_paper_doi               10.1021/ic048880w
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C20 H19 Mn Mo O8 S2'
_chemical_formula_weight         602.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.4970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7934(4)
_cell_length_b                   21.9625(9)
_cell_length_c                   12.7233(6)
_cell_measurement_reflns_used    9253
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.34
_cell_volume                     2436.18(19)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18524
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0267
_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)+(0.0283P)²+1.1244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                5353
_reflns_number_total             6049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048880wsi20040816_124320.cif
_cod_data_source_block           miaoii1s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4312220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mo1 Mo 0.473378(18) 0.318971(9) 0.487960(13) 0.04394(6) Uani 1 1 d . . .
Mn1 Mn 0.23968(3) 0.378022(12) 0.56889(2) 0.03867(7) Uani 1 1 d . . .
S1 S 0.29932(5) 0.27683(2) 0.60846(3) 0.03887(10) Uani 1 1 d . . .
S2 S 0.20855(5) 0.33656(2) 0.39853(3) 0.03995(10) Uani 1 1 d . . .
O10 O 0.3374(2) 0.41984(10) 0.78697(15) 0.0872(6) Uani 1 1 d . . .
O11 O 0.2013(3) 0.50452(8) 0.4937(2) 0.0952(7) Uani 1 1 d . . .
O12 O -0.08088(19) 0.37419(9) 0.60670(16) 0.0745(5) Uani 1 1 d . . .
O20 O 0.63198(18) 0.37759(10) 0.69902(13) 0.0737(5) Uani 1 1 d . . .
O21 O 0.5027(3) 0.44963(11) 0.39151(18) 0.0965(7) Uani 1 1 d . . .
O32 O -0.02542(18) 0.26096(8) 0.24377(11) 0.0531(4) Uani 1 1 d . . .
O35 O 0.1465(2) 0.15749(7) 0.63724(11) 0.0543(4) Uani 1 1 d . . .
C1 C 0.4981(4) 0.23558(16) 0.3781(2) 0.0781(9) Uani 1 1 d . . .
C2 C 0.5663(4) 0.21895(15) 0.4790(3) 0.0773(8) Uani 1 1 d . . .
C3 C 0.6915(3) 0.25818(16) 0.5095(3) 0.0783(9) Uani 1 1 d . . .
C4 C 0.7007(3) 0.2986(2) 0.4262(3) 0.0864(10) Uani 1 1 d . . .
C5 C 0.5810(4) 0.2846(2) 0.3452(2) 0.0848(10) Uani 1 1 d . . .
C10 C 0.3011(2) 0.40370(10) 0.70190(18) 0.0535(5) Uani 1 1 d . . .
C11 C 0.2197(3) 0.45553(10) 0.52243(19) 0.0576(5) Uani 1 1 d . . .
C12 C 0.0441(2) 0.37572(9) 0.59210(16) 0.0466(4) Uani 1 1 d . . .
C20 C 0.5680(2) 0.35799(11) 0.62280(17) 0.0536(5) Uani 1 1 d . . .
C21 C 0.4900(3) 0.40323(13) 0.4299(2) 0.0650(6) Uani 1 1 d . . .
C30 C 0.1661(2) 0.23659(8) 0.51546(13) 0.0361(3) Uani 1 1 d . . .
C31 C 0.12444(19) 0.26422(8) 0.41762(13) 0.0348(3) Uani 1 1 d . . .
C32 C 0.0227(2) 0.23604(9) 0.34047(14) 0.0394(4) Uani 1 1 d . . .
C33 C -0.0376(3) 0.17963(9) 0.36346(16) 0.0483(5) Uani 1 1 d . . .
C34 C 0.0028(3) 0.15268(9) 0.46077(16) 0.0499(5) Uani 1 1 d . . .
C35 C 0.1056(2) 0.18116(8) 0.53826(14) 0.0416(4) Uani 1 1 d . . .
H1 H 0.415(4) 0.2185(14) 0.341(2) 0.090(10) Uiso 1 1 d . . .
H2 H 0.530(3) 0.1885(12) 0.513(2) 0.062(8) Uiso 1 1 d . . .
H3 H 0.752(4) 0.2581(14) 0.567(3) 0.092(10) Uiso 1 1 d . . .
H4 H 0.768(5) 0.3303(16) 0.426(3) 0.113(13) Uiso 1 1 d . . .
H5 H 0.568(4) 0.3034(16) 0.283(3) 0.105(12) Uiso 1 1 d . . .
H32 H 0.027(3) 0.2852(11) 0.2272(19) 0.051(7) Uiso 1 1 d . . .
H33 H -0.106(3) 0.1604(10) 0.3109(18) 0.050(6) Uiso 1 1 d . . .
H34 H -0.042(3) 0.1158(11) 0.4786(18) 0.061(7) Uiso 1 1 d . . .
H35 H 0.119(3) 0.1259(12) 0.640(2) 0.066(9) Uiso 1 1 d . . .
C50 C -0.1673(8) 0.0696(3) 0.7088(6) 0.186(3) Uani 1 1 d . . .
H50A H -0.1312 0.1102 0.7243 0.279 Uiso 1 1 calc R . .
H50B H -0.2422 0.0591 0.7543 0.279 Uiso 1 1 calc R . .
H50C H -0.2130 0.0673 0.6362 0.279 Uiso 1 1 calc R . .
C51 C -0.0409(8) 0.0279(3) 0.7262(5) 0.174(3) Uani 1 1 d . . .
H51A H 0.0050 0.0302 0.7996 0.208 Uiso 1 1 calc R . .
H51B H -0.0780 -0.0133 0.7125 0.208 Uiso 1 1 calc R . .
C52 C 0.1961(8) 0.00183(18) 0.6705(5) 0.176(3) Uani 1 1 d . . .
H52A H 0.1606 -0.0392 0.6534 0.212 Uiso 1 1 calc R . .
H52B H 0.2439 0.0021 0.7437 0.212 Uiso 1 1 calc R . .
C53 C 0.3088(10) 0.0186(4) 0.6023(7) 0.228(4) Uani 1 1 d . . .
H53A H 0.2616 0.0189 0.5299 0.342 Uiso 1 1 calc R . .
H53B H 0.3913 -0.0103 0.6104 0.342 Uiso 1 1 calc R . .
H53C H 0.3481 0.0585 0.6213 0.342 Uiso 1 1 calc R . .
O50 O 0.0712(4) 0.04129(9) 0.65958(18) 0.1064(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
C20 Mo1 C21 83.01(10) . . ?
C20 Mo1 C5 130.91(11) . . ?
C21 Mo1 C5 87.39(14) . . ?
C20 Mo1 C4 95.40(10) . . ?
C21 Mo1 C4 86.86(14) . . ?
C5 Mo1 C4 35.89(11) . . ?
C20 Mo1 C3 84.27(10) . . ?
C21 Mo1 C3 118.38(12) . . ?
C5 Mo1 C3 58.84(12) . . ?
C4 Mo1 C3 35.17(13) . . ?
C20 Mo1 C1 142.20(10) . . ?
C21 Mo1 C1 119.18(12) . . ?
C5 Mo1 C1 35.18(13) . . ?
C4 Mo1 C1 59.06(13) . . ?
C3 Mo1 C1 58.61(10) . . ?
C20 Mo1 C2 109.49(11) . . ?
C21 Mo1 C2 143.31(12) . . ?
C5 Mo1 C2 57.99(14) . . ?
C4 Mo1 C2 58.36(14) . . ?
C3 Mo1 C2 35.14(11) . . ?
C1 Mo1 C2 34.59(11) . . ?
C20 Mo1 S1 81.43(7) . . ?
C21 Mo1 S1 130.69(8) . . ?
C5 Mo1 S1 136.15(11) . . ?
C4 Mo1 S1 140.96(12) . . ?
C3 Mo1 S1 106.19(10) . . ?
C1 Mo1 S1 100.99(10) . . ?
C2 Mo1 S1 85.86(9) . . ?
C20 Mo1 S2 125.91(6) . . ?
C21 Mo1 S2 78.27(7) . . ?
C5 Mo1 S2 98.51(9) . . ?
C4 Mo1 S2 133.03(9) . . ?
C3 Mo1 S2 148.55(8) . . ?
C1 Mo1 S2 90.16(8) . . ?
C2 Mo1 S2 115.71(9) . . ?
S1 Mo1 S2 73.998(15) . . ?
C20 Mo1 Mn1 73.95(6) . . ?
C21 Mo1 Mn1 78.22(8) . . ?
C5 Mo1 Mn1 149.76(9) . . ?
C4 Mo1 Mn1 162.51(11) . . ?
C3 Mo1 Mn1 151.05(8) . . ?
C1 Mo1 Mn1 136.88(8) . . ?
C2 Mo1 Mn1 137.93(9) . . ?
S1 Mo1 Mn1 52.532(13) . . ?
S2 Mo1 Mn1 52.767(13) . . ?
C12 Mn1 C10 91.77(10) . . ?
C12 Mn1 C11 91.50(10) . . ?
C10 Mn1 C11 90.97(11) . . ?
C12 Mn1 S1 97.60(7) . . ?
C10 Mn1 S1 93.69(7) . . ?
C11 Mn1 S1 169.63(8) . . ?
C12 Mn1 S2 98.28(7) . . ?
C10 Mn1 S2 168.67(7) . . ?
C11 Mn1 S2 93.97(8) . . ?
S1 Mn1 S2 79.856(18) . . ?
C12 Mn1 Mo1 146.62(7) . . ?
C10 Mn1 Mo1 110.72(7) . . ?
C11 Mn1 Mo1 111.67(8) . . ?
S1 Mn1 Mo1 57.988(14) . . ?
S2 Mn1 Mo1 57.961(14) . . ?
C30 S1 Mn1 102.69(6) . . ?
C30 S1 Mo1 100.33(6) . . ?
Mn1 S1 Mo1 69.480(15) . . ?
C31 S2 Mn1 102.80(6) . . ?
C31 S2 Mo1 100.35(6) . . ?
Mn1 S2 Mo1 69.272(14) . . ?
C2 C1 C5 107.5(3) . . ?
C2 C1 Mo1 73.52(16) . . ?
C5 C1 Mo1 70.52(16) . . ?
C1 C2 C3 108.7(3) . . ?
C1 C2 Mo1 71.88(18) . . ?
C3 C2 Mo1 71.33(17) . . ?
C4 C3 C2 107.5(3) . . ?
C4 C3 Mo1 70.91(16) . . ?
C2 C3 Mo1 73.52(16) . . ?
C3 C4 C5 107.8(3) . . ?
C3 C4 Mo1 73.92(16) . . ?
C5 C4 Mo1 71.96(16) . . ?
C1 C5 C4 108.6(3) . . ?
C1 C5 Mo1 74.30(16) . . ?
C4 C5 Mo1 72.15(16) . . ?
O10 C10 Mn1 178.7(2) . . ?
O11 C11 Mn1 177.4(2) . . ?
O12 C12 Mn1 179.8(3) . . ?
O20 C20 Mo1 174.6(2) . . ?
O21 C21 Mo1 175.7(3) . . ?
C35 C30 C31 120.77(16) . . ?
C35 C30 S1 122.45(13) . . ?
C31 C30 S1 116.78(13) . . ?
C32 C31 C30 120.66(16) . . ?
C32 C31 S2 122.88(13) . . ?
C30 C31 S2 116.46(12) . . ?
O32 C32 C31 123.80(17) . . ?
O32 C32 C33 117.69(16) . . ?
C31 C32 C33 118.48(17) . . ?
C34 C33 C32 120.70(18) . . ?
C33 C34 C35 120.66(18) . . ?
O35 C35 C30 117.96(17) . . ?
O35 C35 C34 123.29(18) . . ?
C30 C35 C34 118.73(17) . . ?
O50 C51 C50 111.2(4) . . ?
O50 C52 C53 112.0(5) . . ?
C52 O50 C51 114.5(4) . . ?
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
Mo1 C20 1.999(2) . ?
Mo1 C21 2.005(3) . ?
Mo1 C5 2.283(3) . ?
Mo1 C4 2.285(3) . ?
Mo1 C3 2.324(3) . ?
Mo1 C1 2.331(3) . ?
Mo1 C2 2.352(3) . ?
Mo1 S1 2.4824(5) . ?
Mo1 S2 2.4851(5) . ?
Mo1 Mn1 2.7418(3) . ?
Mn1 C12 1.783(2) . ?
Mn1 C10 1.799(2) . ?
Mn1 C11 1.803(2) . ?
Mn1 S1 2.3236(5) . ?
Mn1 S2 2.3341(5) . ?
S1 C30 1.7866(17) . ?
S2 C31 1.7826(17) . ?
O10 C10 1.144(3) . ?
O11 C11 1.141(3) . ?
O12 C12 1.139(3) . ?
O20 C20 1.140(2) . ?
O21 C21 1.142(3) . ?
O32 C32 1.363(2) . ?
O35 C35 1.366(2) . ?
C1 C2 1.392(4) . ?
C1 C5 1.395(5) . ?
C2 C3 1.412(5) . ?
C3 C4 1.393(5) . ?
C4 C5 1.407(4) . ?
C30 C35 1.375(2) . ?
C30 C31 1.390(2) . ?
C31 C32 1.385(2) . ?
C32 C33 1.393(3) . ?
C33 C34 1.377(3) . ?
C34 C35 1.396(3) . ?
C50 C51 1.434(8) . ?
C51 O50 1.412(6) . ?
C52 O50 1.392(6) . ?
C52 C53 1.447(9) . ?
