#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318900.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_4318900
loop_
_publ_author_name
'Richard D. Adams'
'O-Sung Kwon'
'Mark D. Smith'
_publ_section_title
;
 Disulfides of Manganese Carbonyl. Synthesis of Mn2(CO)7(μ-S2) and Its
 Reactions with Tertiary Phosphines and Arsines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6281
_journal_page_last               6290
_journal_paper_doi               10.1021/ic0203670
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C22 H11 As Mn4 O14 S4'
_chemical_formula_weight         922.23
_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                 91.4490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0561(4)
_cell_length_b                   25.9062(11)
_cell_length_c                   13.7699(6)
_cell_measurement_reflns_used    6292
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.38
_cell_volume                     3229.5(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      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24722
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    2.866
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.852364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0334
_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)+(0.0369P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                6440
_reflns_number_total             7988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203670_07.cif
_cod_data_source_block           Mn4(CO)14S4(AsMe2Ph)
_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               4318900
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 0.77751(4) 0.168063(13) 0.95487(3) 0.02847(9) Uani 1 1 d . . .
Mn2 Mn 0.45896(4) 0.160859(13) 0.80447(3) 0.02880(9) Uani 1 1 d . . .
Mn3 Mn 0.81368(4) 0.224610(13) 0.68495(3) 0.02986(9) Uani 1 1 d . . .
Mn4 Mn 0.72444(4) 0.022230(13) 0.82808(3) 0.02911(9) Uani 1 1 d . . .
S1 S 0.68912(6) 0.11430(2) 0.82592(4) 0.02683(12) Uani 1 1 d . . .
S2 S 0.58429(7) 0.22207(2) 0.90087(4) 0.03023(13) Uani 1 1 d . . .
S3 S 0.87395(6) 0.15985(2) 0.80008(4) 0.02767(13) Uani 1 1 d . . .
S4 S 0.57954(7) 0.23439(2) 0.75184(4) 0.03073(13) Uani 1 1 d . . .
As1 As 0.81989(3) 0.016484(9) 0.663883(19) 0.03500(7) Uani 1 1 d . . .
C1 C 0.9651(3) 0.06613(10) 0.6226(2) 0.0512(8) Uani 1 1 d . . .
H1A H 1.0466 0.0667 0.6686 0.077 Uiso 1 1 calc R . .
H1B H 0.9209 0.0998 0.6189 0.077 Uiso 1 1 calc R . .
H1C H 0.9999 0.0565 0.5599 0.077 Uiso 1 1 calc R . .
C2 C 0.6770(4) 0.01661(14) 0.5568(2) 0.0654(9) Uani 1 1 d . . .
H2A H 0.7272 0.0123 0.4968 0.098 Uiso 1 1 calc R . .
H2B H 0.6245 0.0488 0.5558 0.098 Uiso 1 1 calc R . .
H2C H 0.6084 -0.0112 0.5648 0.098 Uiso 1 1 calc R . .
C3 C 0.9244(3) -0.04786(10) 0.6471(2) 0.0439(7) Uani 1 1 d . . .
C4 C 0.8510(4) -0.09101(11) 0.6111(2) 0.0590(9) Uani 1 1 d . . .
H4 H 0.7526 -0.0886 0.5907 0.071 Uiso 1 1 calc R . .
C5 C 0.9238(6) -0.13745(12) 0.6058(3) 0.0827(15) Uani 1 1 d . . .
H5 H 0.8743 -0.1663 0.5813 0.099 Uiso 1 1 calc R . .
C6 C 1.0659(6) -0.14160(14) 0.6355(3) 0.0939(17) Uani 1 1 d . . .
H6 H 1.1135 -0.1733 0.6313 0.113 Uiso 1 1 calc R . .
C7 C 1.1417(5) -0.09954(16) 0.6720(3) 0.0851(13) Uani 1 1 d . . .
H7 H 1.2399 -0.1026 0.6926 0.102 Uiso 1 1 calc R . .
C8 C 1.0684(4) -0.05192(12) 0.6777(3) 0.0618(9) Uani 1 1 d . . .
H8 H 1.1180 -0.0231 0.7023 0.074 Uiso 1 1 calc R . .
C10 C 0.8739(3) 0.22260(10) 1.00693(19) 0.0379(6) Uani 1 1 d . . .
C11 C 0.6654(3) 0.15763(10) 1.0597(2) 0.0419(6) Uani 1 1 d . . .
C12 C 0.9121(3) 0.12473(10) 1.0100(2) 0.0394(6) Uani 1 1 d . . .
C20 C 0.2923(3) 0.19777(10) 0.8104(2) 0.0396(6) Uani 1 1 d . . .
C21 C 0.3955(3) 0.12848(10) 0.6951(2) 0.0414(6) Uani 1 1 d . . .
C22 C 0.3821(3) 0.11512(9) 0.8884(2) 0.0372(6) Uani 1 1 d . . .
C30 C 0.8849(3) 0.27477(10) 0.7737(2) 0.0380(6) Uani 1 1 d . . .
C31 C 0.7696(3) 0.27600(10) 0.5979(2) 0.0383(6) Uani 1 1 d . . .
C32 C 0.9957(3) 0.21459(10) 0.63504(19) 0.0382(6) Uani 1 1 d . . .
C33 C 0.7267(3) 0.17733(10) 0.6005(2) 0.0378(6) Uani 1 1 d . . .
C40 C 0.5330(3) 0.01516(9) 0.7789(2) 0.0407(6) Uani 1 1 d . . .
C41 C 0.7282(3) -0.04836(10) 0.8344(2) 0.0387(6) Uani 1 1 d . . .
C42 C 0.9239(3) 0.02603(10) 0.8653(2) 0.0394(6) Uani 1 1 d . . .
C43 C 0.6683(3) 0.02708(9) 0.9556(2) 0.0369(6) Uani 1 1 d . . .
O10 O 0.9346(2) 0.25780(8) 1.03809(17) 0.0594(6) Uani 1 1 d . . .
O11 O 0.5970(3) 0.15127(10) 1.12693(17) 0.0724(7) Uani 1 1 d . . .
O12 O 0.9915(3) 0.09807(9) 1.05116(18) 0.0679(7) Uani 1 1 d . . .
O20 O 0.1878(2) 0.22215(9) 0.81932(17) 0.0629(6) Uani 1 1 d . . .
O21 O 0.3525(3) 0.10853(9) 0.62589(17) 0.0695(7) Uani 1 1 d . . .
O22 O 0.3319(3) 0.08665(8) 0.94141(17) 0.0611(6) Uani 1 1 d . . .
O30 O 0.9244(3) 0.30588(8) 0.82435(17) 0.0620(6) Uani 1 1 d . . .
O31 O 0.7417(3) 0.30743(8) 0.54372(16) 0.0567(6) Uani 1 1 d . . .
O32 O 1.1092(2) 0.20758(9) 0.60434(16) 0.0585(6) Uani 1 1 d . . .
O33 O 0.6719(3) 0.14963(8) 0.54766(16) 0.0609(6) Uani 1 1 d . . .
O40 O 0.4183(2) 0.00762(8) 0.74796(19) 0.0648(6) Uani 1 1 d . . .
O41 O 0.7225(3) -0.09197(7) 0.83619(16) 0.0582(6) Uani 1 1 d . . .
O42 O 1.0448(2) 0.02603(9) 0.88530(19) 0.0692(7) Uani 1 1 d . . .
O43 O 0.6389(3) 0.03125(8) 1.03396(15) 0.0557(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'
As As 0.0499 2.0058 '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
C10 Mn1 C11 94.34(13) . . ?
C10 Mn1 C12 90.30(12) . . ?
C11 Mn1 C12 87.58(12) . . ?
C10 Mn1 S3 104.26(9) . . ?
C11 Mn1 S3 161.34(9) . . ?
C12 Mn1 S3 93.62(9) . . ?
C10 Mn1 S2 90.48(9) . . ?
C11 Mn1 S2 85.00(9) . . ?
C12 Mn1 S2 172.58(9) . . ?
S3 Mn1 S2 93.34(2) . . ?
C10 Mn1 S1 155.12(9) . . ?
C11 Mn1 S1 108.89(9) . . ?
C12 Mn1 S1 99.22(8) . . ?
S3 Mn1 S1 52.53(2) . . ?
S2 Mn1 S1 83.02(2) . . ?
C20 Mn2 C21 92.03(12) . . ?
C20 Mn2 C22 88.98(12) . . ?
C21 Mn2 C22 96.28(13) . . ?
C20 Mn2 S4 88.84(9) . . ?
C21 Mn2 S4 105.25(9) . . ?
C22 Mn2 S4 158.42(9) . . ?
C20 Mn2 S2 90.55(9) . . ?
C21 Mn2 S2 157.92(9) . . ?
C22 Mn2 S2 105.69(9) . . ?
S4 Mn2 S2 52.87(2) . . ?
C20 Mn2 S1 170.14(9) . . ?
C21 Mn2 S1 97.19(9) . . ?
C22 Mn2 S1 86.53(8) . . ?
S4 Mn2 S1 92.10(2) . . ?
S2 Mn2 S1 82.23(2) . . ?
C32 Mn3 C31 92.35(11) . . ?
C32 Mn3 C33 92.50(12) . . ?
C31 Mn3 C33 89.29(12) . . ?
C32 Mn3 C30 92.56(12) . . ?
C31 Mn3 C30 89.34(12) . . ?
C33 Mn3 C30 174.80(12) . . ?
C32 Mn3 S4 177.83(8) . . ?
C31 Mn3 S4 89.67(8) . . ?
C33 Mn3 S4 86.76(8) . . ?
C30 Mn3 S4 88.22(8) . . ?
C32 Mn3 S3 87.48(8) . . ?
C31 Mn3 S3 178.47(9) . . ?
C33 Mn3 S3 92.24(8) . . ?
C30 Mn3 S3 89.15(8) . . ?
S4 Mn3 S3 90.52(2) . . ?
C41 Mn4 C43 91.59(11) . . ?
C41 Mn4 C40 86.26(12) . . ?
C43 Mn4 C40 94.42(12) . . ?
C41 Mn4 C42 91.32(12) . . ?
C43 Mn4 C42 91.31(12) . . ?
C40 Mn4 C42 173.84(12) . . ?
C41 Mn4 S1 173.07(8) . . ?
C43 Mn4 S1 84.52(7) . . ?
C40 Mn4 S1 88.32(8) . . ?
C42 Mn4 S1 94.50(8) . . ?
C41 Mn4 As1 88.67(8) . . ?
C43 Mn4 As1 175.28(9) . . ?
C40 Mn4 As1 90.29(9) . . ?
C42 Mn4 As1 83.98(9) . . ?
S1 Mn4 As1 95.675(19) . . ?
S3 S1 Mn1 62.60(2) . . ?
S3 S1 Mn4 117.12(3) . . ?
Mn1 S1 Mn4 121.93(3) . . ?
S3 S1 Mn2 112.93(3) . . ?
Mn1 S1 Mn2 94.11(2) . . ?
Mn4 S1 Mn2 127.54(3) . . ?
S4 S2 Mn2 63.02(3) . . ?
S4 S2 Mn1 113.67(3) . . ?
Mn2 S2 Mn1 97.04(2) . . ?
S1 S3 Mn1 64.87(2) . . ?
S1 S3 Mn3 110.09(3) . . ?
Mn1 S3 Mn3 117.57(3) . . ?
S2 S4 Mn2 64.11(2) . . ?
S2 S4 Mn3 112.02(3) . . ?
Mn2 S4 Mn3 118.09(3) . . ?
C3 As1 C1 101.50(12) . . ?
C3 As1 C2 103.31(14) . . ?
C1 As1 C2 102.80(15) . . ?
C3 As1 Mn4 110.40(8) . . ?
C1 As1 Mn4 119.33(9) . . ?
C2 As1 Mn4 117.29(11) . . ?
C8 C3 C4 119.6(3) . . ?
C8 C3 As1 119.8(2) . . ?
C4 C3 As1 120.4(3) . . ?
C5 C4 C3 119.9(4) . . ?
C6 C5 C4 120.7(4) . . ?
C5 C6 C7 120.9(3) . . ?
C6 C7 C8 118.9(4) . . ?
C3 C8 C7 120.0(4) . . ?
O10 C10 Mn1 178.5(2) . . ?
O11 C11 Mn1 178.7(3) . . ?
O12 C12 Mn1 174.8(3) . . ?
O20 C20 Mn2 176.2(3) . . ?
O21 C21 Mn2 178.5(3) . . ?
O22 C22 Mn2 179.1(2) . . ?
O30 C30 Mn3 177.4(3) . . ?
O31 C31 Mn3 179.4(3) . . ?
O32 C32 Mn3 179.0(2) . . ?
O33 C33 Mn3 178.1(2) . . ?
O40 C40 Mn4 175.6(2) . . ?
O41 C41 Mn4 176.1(3) . . ?
O42 C42 Mn4 176.5(3) . . ?
O43 C43 Mn4 177.3(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 C10 1.800(3) . ?
Mn1 C11 1.806(3) . ?
Mn1 C12 1.810(3) . ?
Mn1 S3 2.3336(7) . ?
Mn1 S2 2.3466(7) . ?
Mn1 S1 2.3795(7) . ?
Mn2 C20 1.791(3) . ?
Mn2 C21 1.805(3) . ?
Mn2 C22 1.807(3) . ?
Mn2 S4 2.3208(7) . ?
Mn2 S2 2.3428(7) . ?
Mn2 S1 2.4198(7) . ?
Mn3 C32 1.821(3) . ?
Mn3 C31 1.829(3) . ?
Mn3 C33 1.851(3) . ?
Mn3 C30 1.886(3) . ?
Mn3 S4 2.3468(7) . ?
Mn3 S3 2.3625(7) . ?
Mn4 C41 1.831(3) . ?
Mn4 C43 1.844(3) . ?
Mn4 C40 1.855(3) . ?
Mn4 C42 1.868(3) . ?
Mn4 S1 2.4065(6) . ?
Mn4 As1 2.4454(5) . ?
S1 S3 2.0860(8) . ?
S2 S4 2.0762(9) . ?
As1 C3 1.934(3) . ?
As1 C1 1.935(3) . ?
As1 C2 1.937(3) . ?
C3 C8 1.364(5) . ?
C3 C4 1.386(4) . ?
C4 C5 1.375(5) . ?
C5 C6 1.344(6) . ?
C6 C7 1.377(6) . ?
C7 C8 1.404(4) . ?
C10 O10 1.143(3) . ?
C11 O11 1.139(3) . ?
C12 O12 1.138(3) . ?
C20 O20 1.146(3) . ?
C21 O21 1.144(3) . ?
C22 O22 1.140(3) . ?
C30 O30 1.119(3) . ?
C31 O31 1.128(3) . ?
C32 O32 1.135(3) . ?
C33 O33 1.128(3) . ?
C40 O40 1.129(3) . ?
C41 O41 1.131(3) . ?
C42 O42 1.122(3) . ?
C43 O43 1.123(3) . ?
