#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:51:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179266 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/86/4318692.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_4318692
loop_
_publ_author_name
'Richard D. Adams'
'O.-Sung Kwon'
'Mark D. Smith'
_publ_section_title
;
 Reactions of Thioethers with Mn2(CO)7(μ-S2) Proceed with CO Displacement
 and Insertion of the Sulfur Atom into the Mn-Mn Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5525
_journal_page_last               5529
_journal_paper_doi               10.1021/ic020408s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H18 Mn2 O6 S5'
_chemical_formula_weight         564.47
_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                106.943(2)
_cell_angle_beta                 91.098(2)
_cell_angle_gamma                106.817(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2793(10)
_cell_length_b                   10.4560(10)
_cell_length_c                   11.1034(11)
_cell_measurement_reflns_used    6531
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      26.392
_cell_measurement_theta_min      2.397
_cell_volume                     1085.78(18)
_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      190(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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10061
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_T_max  0.862022
_exptl_absorpt_correction_T_min  0.684510
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0288
_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
  [0.00000+1.00000exp(0.90(sinθ/λ)²)]/
    [σ²(Fo²)+0.0000+0.0000*P+(0.0332P)²+0.0000sinθ/λ]
  where P = 0.33333Fo² + 0.66667Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                3633
_reflns_number_total             4428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020408s_4.cif
_cod_data_source_block           kw12s3s
_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               4318692
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 -0.00771(3) 0.25463(4) 0.13380(3) 0.02062(9) Uani 1 1 d . . .
Mn2 Mn 0.18506(3) 0.30238(4) 0.41005(3) 0.02065(9) Uani 1 1 d . . .
S1 S -0.05057(6) 0.21828(6) 0.33147(6) 0.02468(14) Uani 1 1 d . . .
S2 S 0.07289(6) 0.11519(6) 0.22995(6) 0.02454(13) Uani 1 1 d . . .
S31 S 0.18301(5) 0.42649(6) 0.26506(5) 0.01996(13) Uani 1 1 d . . .
S32 S 0.34300(6) 0.93298(6) 0.39007(6) 0.02766(14) Uani 1 1 d . . .
S33 S 0.53740(6) 0.73558(6) 0.10815(6) 0.02756(14) Uani 1 1 d . . .
C10 C 0.0696(2) 0.2462(2) -0.0119(2) 0.0243(5) Uani 1 1 d . . .
C11 C -0.1026(2) 0.3661(3) 0.1055(2) 0.0262(5) Uani 1 1 d . . .
C12 C -0.1504(2) 0.1030(3) 0.0518(2) 0.0246(5) Uani 1 1 d . . .
C20 C 0.3632(2) 0.3110(2) 0.4155(2) 0.0253(5) Uani 1 1 d . . .
C21 C 0.2114(2) 0.4530(3) 0.5483(2) 0.0259(5) Uani 1 1 d . . .
C22 C 0.1574(2) 0.1909(2) 0.5110(2) 0.0250(5) Uani 1 1 d . . .
C31 C 0.1667(2) 0.5980(2) 0.3457(2) 0.0237(5) Uani 1 1 d . . .
H31A H 0.0905 0.5852 0.3987 0.028 Uiso 1 1 calc R . .
H31B H 0.2515 0.6544 0.4035 0.028 Uiso 1 1 calc R . .
C32 C 0.1412(3) 0.6815(2) 0.2620(2) 0.0285(5) Uani 1 1 d . . .
H32A H 0.0461 0.6399 0.2201 0.034 Uiso 1 1 calc R . .
H32B H 0.2039 0.6776 0.1954 0.034 Uiso 1 1 calc R . .
C33 C 0.1645(2) 0.8343(2) 0.3412(2) 0.0272(5) Uani 1 1 d . . .
H33A H 0.1160 0.8361 0.4176 0.033 Uiso 1 1 calc R . .
H33B H 0.1242 0.8808 0.2913 0.033 Uiso 1 1 calc R . .
C34 C 0.3893(3) 0.9664(3) 0.2426(2) 0.0293(5) Uani 1 1 d . . .
H34A H 0.3443 0.8809 0.1708 0.035 Uiso 1 1 calc R . .
H34B H 0.3551 1.0427 0.2332 0.035 Uiso 1 1 calc R . .
C35 C 0.5432(3) 1.0080(3) 0.2371(3) 0.0332(6) Uani 1 1 d . . .
H35A H 0.5629 1.0317 0.1580 0.040 Uiso 1 1 calc R . .
H35B H 0.5875 1.0936 0.3091 0.040 Uiso 1 1 calc R . .
C36 C 0.6065(2) 0.8949(2) 0.2419(2) 0.0286(5) Uani 1 1 d . . .
H36A H 0.5891 0.8721 0.3217 0.034 Uiso 1 1 calc R . .
H36B H 0.7067 0.9312 0.2417 0.034 Uiso 1 1 calc R . .
C37 C 0.5719(2) 0.6096(2) 0.1772(2) 0.0262(5) Uani 1 1 d . . .
H37A H 0.5767 0.5266 0.1083 0.031 Uiso 1 1 calc R . .
H37B H 0.6620 0.6527 0.2290 0.031 Uiso 1 1 calc R . .
C38 C 0.4633(2) 0.5613(3) 0.2600(2) 0.0262(5) Uani 1 1 d . . .
H38A H 0.4966 0.5101 0.3097 0.031 Uiso 1 1 calc R . .
H38B H 0.4469 0.6444 0.3202 0.031 Uiso 1 1 calc R . .
C39 C 0.3306(2) 0.4664(2) 0.1795(2) 0.0233(5) Uani 1 1 d . . .
H39A H 0.3450 0.3767 0.1308 0.028 Uiso 1 1 calc R . .
H39B H 0.3092 0.5111 0.1176 0.028 Uiso 1 1 calc R . .
O10 O 0.11635(18) 0.24071(19) -0.10512(16) 0.0341(4) Uani 1 1 d . . .
O11 O -0.16686(19) 0.43014(19) 0.08107(18) 0.0395(5) Uani 1 1 d . . .
O12 O -0.24004(18) 0.00578(19) -0.00014(17) 0.0372(4) Uani 1 1 d . . .
O20 O 0.47522(17) 0.31391(18) 0.42085(17) 0.0334(4) Uani 1 1 d . . .
O21 O 0.2271(2) 0.5468(2) 0.63740(17) 0.0411(5) Uani 1 1 d . . .
O22 O 0.13935(18) 0.12376(19) 0.57757(17) 0.0351(4) 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'
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 90.50(10) . . ?
C12 Mn1 C11 89.04(11) . . ?
C10 Mn1 C11 92.58(11) . . ?
C12 Mn1 S31 169.15(8) . . ?
C10 Mn1 S31 95.37(7) . . ?
C11 Mn1 S31 99.77(8) . . ?
C12 Mn1 S2 89.52(8) . . ?
C10 Mn1 S2 106.90(8) . . ?
C11 Mn1 S2 160.48(8) . . ?
S31 Mn1 S2 80.06(2) . . ?
C12 Mn1 S1 91.97(7) . . ?
C10 Mn1 S1 158.14(8) . . ?
C11 Mn1 S1 109.17(8) . . ?
S31 Mn1 S1 79.22(2) . . ?
S2 Mn1 S1 51.43(2) . . ?
C21 Mn2 C20 94.11(11) . . ?
C21 Mn2 C22 89.34(11) . . ?
C20 Mn2 C22 89.67(10) . . ?
C21 Mn2 S2 159.54(8) . . ?
C20 Mn2 S2 106.24(8) . . ?
C22 Mn2 S2 92.82(8) . . ?
C21 Mn2 S31 94.85(8) . . ?
C20 Mn2 S31 98.56(8) . . ?
C22 Mn2 S31 170.46(7) . . ?
S2 Mn2 S31 80.30(2) . . ?
C21 Mn2 S1 108.25(8) . . ?
C20 Mn2 S1 157.61(8) . . ?
C22 Mn2 S1 91.53(7) . . ?
S2 Mn2 S1 51.38(2) . . ?
S31 Mn2 S1 79.03(2) . . ?
S2 S1 Mn1 63.98(2) . . ?
S2 S1 Mn2 63.47(2) . . ?
Mn1 S1 Mn2 93.39(2) . . ?
S1 S2 Mn2 65.15(3) . . ?
S1 S2 Mn1 64.60(3) . . ?
Mn2 S2 Mn1 94.58(2) . . ?
C31 S31 C39 103.45(11) . . ?
C31 S31 Mn2 110.08(8) . . ?
C39 S31 Mn2 119.10(8) . . ?
C31 S31 Mn1 118.12(8) . . ?
C39 S31 Mn1 112.41(8) . . ?
Mn2 S31 Mn1 94.45(2) . . ?
C33 S32 C34 98.90(12) . . ?
C37 S33 C36 99.18(12) . . ?
O10 C10 Mn1 178.8(2) . . ?
O11 C11 Mn1 175.8(2) . . ?
O12 C12 Mn1 179.2(2) . . ?
O20 C20 Mn2 178.1(2) . . ?
O21 C21 Mn2 178.6(2) . . ?
O22 C22 Mn2 178.0(2) . . ?
C32 C31 S31 116.28(16) . . ?
C31 C32 C33 110.1(2) . . ?
C32 C33 S32 113.32(17) . . ?
C35 C34 S32 112.27(18) . . ?
C36 C35 C34 114.1(2) . . ?
C35 C36 S33 111.96(18) . . ?
C38 C37 S33 112.86(17) . . ?
C39 C38 C37 110.81(19) . . ?
C38 C39 S31 115.83(16) . . ?
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 1.805(2) . ?
Mn1 C10 1.806(2) . ?
Mn1 C11 1.807(2) . ?
Mn1 S31 2.3499(6) . ?
Mn1 S2 2.3503(7) . ?
Mn1 S1 2.3627(7) . ?
Mn2 C21 1.800(3) . ?
Mn2 C20 1.806(2) . ?
Mn2 C22 1.811(2) . ?
Mn2 S2 2.3418(7) . ?
Mn2 S31 2.3469(6) . ?
Mn2 S1 2.3750(7) . ?
S1 S2 2.0448(9) . ?
S31 C31 1.813(2) . ?
S31 C39 1.816(2) . ?
S32 C33 1.807(2) . ?
S32 C34 1.816(2) . ?
S33 C37 1.816(2) . ?
S33 C36 1.821(2) . ?
C10 O10 1.143(3) . ?
C11 O11 1.146(3) . ?
C12 O12 1.145(3) . ?
C20 O20 1.143(3) . ?
C21 O21 1.141(3) . ?
C22 O22 1.142(3) . ?
C31 C32 1.513(3) . ?
C32 C33 1.529(3) . ?
C34 C35 1.523(3) . ?
C35 C36 1.517(3) . ?
C37 C38 1.526(3) . ?
C38 C39 1.516(3) . ?
