#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319894.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_4319894
loop_
_publ_author_name
'Wen-Feng Liaw'
'Chien-Kuo Hsieh'
'Ging-Yi Lin'
'Gene-Hsiang Lee'
_publ_section_title
;
 Syntheses, Reactivity, and π-Donating Ligand Metathesis Reaction of
 Five-Coordinate Sixteen-Electron Manganese(I) Complexes: Crystal
 Structures of [Mn(CO)3(-TeC6H4-o-NH-)]-,
 [(Mn(CO)3)2(μ-SC6H4-o-S-S-C6H4-o-μ-S-)], [(CO)3Mn(μ-SC6H4-o-NH2-)]2,
 and [(CO)3Mn(μ-SC8N2H4-o-S-)]22-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3468
_journal_page_last               3475
_journal_paper_doi               10.1021/ic000795a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C18 H8 Mn2 O6 S4'
_chemical_formula_weight         558.36
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.703(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6320(1)
_cell_length_b                   12.4082(3)
_cell_length_c                   16.6646(2)
_cell_measurement_reflns_used    4797
_cell_measurement_temperature    295(2)
_cell_volume                     2191.06(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'ω 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10980
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_obs          0.0319
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0229P)²+0.8488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0728
_refine_ls_wR_factor_obs         0.0665
_reflns_number_observed          3871
_reflns_number_total             4842
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000795a_5.cif
_cod_data_source_block           ic6078
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.8488P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.8488P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319894
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn 0.76989(3) 0.66434(3) 0.06261(2) 0.04014(11) Uani 1 d . .
Mn2 Mn 0.54952(3) 0.74760(3) -0.08816(2) 0.03942(11) Uani 1 d . .
S1 S 0.76312(6) 0.68870(5) -0.08191(4) 0.0439(2) Uani 1 d . .
S2 S 0.63825(5) 0.90121(5) -0.02861(3) 0.03731(14) Uani 1 d . .
S3 S 0.71678(5) 0.84058(5) 0.09056(3) 0.03698(14) Uani 1 d . .
S4 S 0.54786(6) 0.64523(5) 0.03544(4) 0.04175(15) Uani 1 d . .
C1 C 0.9394(2) 0.6914(2) 0.07050(15) 0.0514(6) Uani 1 d . .
C2 C 0.7672(2) 0.6375(2) 0.1691(2) 0.0462(6) Uani 1 d . .
C3 C 0.7958(3) 0.5208(3) 0.0467(2) 0.0639(8) Uani 1 d . .
C4 C 0.5595(2) 0.8110(2) -0.18496(15) 0.0455(6) Uani 1 d . .
C5 C 0.3899(2) 0.7956(2) -0.0774(2) 0.0508(6) Uani 1 d . .
C6 C 0.4890(3) 0.6281(3) -0.1420(2) 0.0594(7) Uani 1 d . .
C7 C 0.8420(2) 0.8134(2) -0.09412(13) 0.0422(6) Uani 1 d . .
C8 C 0.9594(2) 0.8191(3) -0.12622(15) 0.0525(7) Uani 1 d . .
H8A H 0.9996(2) 0.7563(3) -0.14069(15) 0.063 Uiso 1 calc R .
C9 C 1.0156(2) 0.9181(3) -0.1364(2) 0.0616(8) Uani 1 d . .
H9A H 1.0926(2) 0.9214(3) -0.1591(2) 0.074 Uiso 1 calc R .
C10 C 0.9593(2) 1.0118(3) -0.1134(2) 0.0587(7) Uani 1 d . .
H10A H 0.9982(2) 1.0777(3) -0.1211(2) 0.070 Uiso 1 calc R .
C11 C 0.8446(2) 1.0087(2) -0.07867(15) 0.0477(6) Uani 1 d . .
H11A H 0.8080(2) 1.0716(2) -0.06103(15) 0.057 Uiso 1 calc R .
C12 C 0.7864(2) 0.9096(2) -0.07104(13) 0.0387(5) Uani 1 d . .
C13 C 0.5684(2) 0.8255(2) 0.13165(13) 0.0366(5) Uani 1 d . .
C14 C 0.5274(2) 0.9016(2) 0.18527(15) 0.0455(6) Uani 1 d . .
H14A H 0.5776(2) 0.9607(2) 0.20060(15) 0.055 Uiso 1 calc R .
C15 C 0.4106(3) 0.8879(2) 0.2154(2) 0.0540(7) Uani 1 d . .
H15A H 0.3828(3) 0.9371(2) 0.2522(2) 0.065 Uiso 1 calc R .
C16 C 0.3356(2) 0.8012(3) 0.1907(2) 0.0550(7) Uani 1 d . .
H16A H 0.2575(2) 0.7927(3) 0.2111(2) 0.066 Uiso 1 calc R .
C17 C 0.3745(2) 0.7270(2) 0.1362(2) 0.0482(6) Uani 1 d . .
H17A H 0.3222(2) 0.6697(2) 0.1197(2) 0.058 Uiso 1 calc R .
C18 C 0.4932(2) 0.7380(2) 0.10579(13) 0.0378(5) Uani 1 d . .
O1 O 1.0452(2) 0.7083(2) 0.07392(13) 0.0776(7) Uani 1 d . .
O2 O 0.7677(2) 0.6189(2) 0.23676(12) 0.0678(6) Uani 1 d . .
O3 O 0.8113(3) 0.4303(2) 0.0400(2) 0.1102(10) Uani 1 d . .
O4 O 0.5646(2) 0.8472(2) -0.24807(11) 0.0660(6) Uani 1 d . .
O5 O 0.2900(2) 0.8256(2) -0.06953(14) 0.0798(7) Uani 1 d . .
O6 O 0.4493(3) 0.5568(2) -0.17959(15) 0.0976(9) Uani 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
C2 Mn1 C3 88.73(13) . . ?
C2 Mn1 C1 93.35(11) . . ?
C3 Mn1 C1 91.73(14) . . ?
C2 Mn1 S3 87.29(9) . . ?
C3 Mn1 S3 173.31(10) . . ?
C1 Mn1 S3 93.86(9) . . ?
C2 Mn1 S4 94.18(8) . . ?
C3 Mn1 S4 91.96(10) . . ?
C1 Mn1 S4 171.69(9) . . ?
S3 Mn1 S4 82.99(2) . . ?
C2 Mn1 S1 175.68(9) . . ?
C3 Mn1 S1 88.27(10) . . ?
C1 Mn1 S1 89.84(8) . . ?
S3 Mn1 S1 95.41(2) . . ?
S4 Mn1 S1 82.82(2) . . ?
C4 Mn2 C5 93.95(11) . . ?
C4 Mn2 C6 87.63(12) . . ?
C5 Mn2 C6 91.19(13) . . ?
C4 Mn2 S2 88.43(8) . . ?
C5 Mn2 S2 92.21(9) . . ?
C6 Mn2 S2 174.97(10) . . ?
C4 Mn2 S1 92.70(8) . . ?
C5 Mn2 S1 171.76(8) . . ?
C6 Mn2 S1 93.94(10) . . ?
S2 Mn2 S1 83.12(2) . . ?
C4 Mn2 S4 173.52(8) . . ?
C5 Mn2 S4 90.93(9) . . ?
C6 Mn2 S4 88.01(9) . . ?
S2 Mn2 S4 95.65(2) . . ?
S1 Mn2 S4 82.83(2) . . ?
C7 S1 Mn2 100.64(8) . . ?
C7 S1 Mn1 104.26(8) . . ?
Mn2 S1 Mn1 91.85(2) . . ?
C12 S2 S3 95.45(8) . . ?
C12 S2 Mn2 102.74(8) . . ?
S3 S2 Mn2 102.39(3) . . ?
C13 S3 S2 95.72(7) . . ?
C13 S3 Mn1 102.49(8) . . ?
S2 S3 Mn1 102.71(3) . . ?
C18 S4 Mn1 100.57(8) . . ?
C18 S4 Mn2 104.33(8) . . ?
Mn1 S4 Mn2 91.91(2) . . ?
O1 C1 Mn1 178.7(2) . . ?
O2 C2 Mn1 178.4(2) . . ?
O3 C3 Mn1 177.2(3) . . ?
O4 C4 Mn2 177.1(2) . . ?
O5 C5 Mn2 179.1(2) . . ?
O6 C6 Mn2 176.1(3) . . ?
C8 C7 C12 118.2(2) . . ?
C8 C7 S1 122.1(2) . . ?
C12 C7 S1 119.8(2) . . ?
C9 C8 C7 120.0(3) . . ?
C10 C9 C8 120.9(2) . . ?
C9 C10 C11 120.6(3) . . ?
C12 C11 C10 118.3(3) . . ?
C11 C12 C7 121.9(2) . . ?
C11 C12 S2 120.3(2) . . ?
C7 C12 S2 117.8(2) . . ?
C14 C13 C18 121.6(2) . . ?
C14 C13 S3 120.5(2) . . ?
C18 C13 S3 117.8(2) . . ?
C15 C14 C13 119.0(2) . . ?
C16 C15 C14 119.9(2) . . ?
C17 C16 C15 121.3(2) . . ?
C16 C17 C18 120.0(2) . . ?
C13 C18 C17 118.2(2) . . ?
C13 C18 S4 119.9(2) . . ?
C17 C18 S4 121.9(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 C2 1.808(3) . ?
Mn1 C3 1.825(3) . ?
Mn1 C1 1.828(3) . ?
Mn1 S3 2.3154(7) . ?
Mn1 S4 2.3787(7) . ?
Mn1 S1 2.4226(7) . ?
Mn2 C4 1.805(3) . ?
Mn2 C5 1.821(3) . ?
Mn2 C6 1.823(3) . ?
Mn2 S2 2.3139(7) . ?
Mn2 S1 2.3799(7) . ?
Mn2 S4 2.4214(7) . ?
S1 C7 1.780(3) . ?
S2 C12 1.782(2) . ?
S2 S3 2.2216(8) . ?
S3 C13 1.780(2) . ?
S4 C18 1.774(2) . ?
C1 O1 1.141(3) . ?
C2 O2 1.150(3) . ?
C3 O3 1.142(4) . ?
C4 O4 1.149(3) . ?
C5 O5 1.144(3) . ?
C6 O6 1.145(3) . ?
C7 C8 1.400(3) . ?
C7 C12 1.399(3) . ?
C8 C9 1.382(4) . ?
C9 C10 1.377(4) . ?
C10 C11 1.392(4) . ?
C11 C12 1.388(3) . ?
C13 C14 1.395(3) . ?
C13 C18 1.396(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.382(4) . ?
C16 C17 1.379(4) . ?
C17 C18 1.404(3) . ?
