#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310061.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_4310061
loop_
_publ_author_name
'Rosa Llusar'
'Sonia Triguero'
'Cristian Vicent'
'Maxim N. Sokolov'
'Benoît Domercq'
'Marc Fourmigué'
_publ_contact_author             'Llusar Barelles Rosa'
_publ_contact_author_address
;
Departament de Ciències Experimentals
Universitat Jaume I, Campus de Riu Sec, P. O. Box 224. Castelló, Spain
;
_publ_contact_author_email       llusar@exp.uji.es
_publ_contact_author_phone       '+34 964 728086'
_publ_section_title
;
A Family of Oxo-Chalcogenide Molybdenum and Tungsten Complexes,
(n-Bu4N)2[M2O2(μ-Q)2(1,3-dithiole-2-thione-4,5-dithiolate)2] (M = Mo, W; Q
= S, Se): New Synthetic Entries, Structure, and Gas-Phase Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8937
_journal_page_last               8946
_journal_paper_doi               10.1021/ic0508728
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C38 H72 Mo2 N2 O4 S10'
_chemical_formula_weight         1133.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 121.029(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.770(5)
_cell_length_b                   13.988(3)
_cell_length_c                   19.668(4)
_cell_measurement_reflns_used    647
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.59
_cell_measurement_theta_min      2.54
_cell_volume                     5368(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0993
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12335
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3734
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0516
_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 w=1/[σ²(Fo²)+(0.0628P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                2056
_reflns_number_total             3734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0508728si20050603_113343_6.cif
_cod_data_source_block           (n-Bu4N)2[Mo2O2S2(dmid)2
_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               4310061
#BEGIN Tags that were not found in dictionaries:
_ratio_of_minimum_to_maximum_apparent_transmission 0.629592
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Mo1 Mo 0.07215(4) 0.92863(5) 0.29140(4) 0.0558(3) Uani 1 1 d . . .
S1 S 0.00153(11) 0.96746(16) 0.34134(13) 0.0643(6) Uani 1 1 d . . .
S2 S 0.15349(12) 0.98917(19) 0.42089(14) 0.0802(7) Uani 1 1 d . . .
S3 S 0.15359(11) 0.98903(16) 0.25710(13) 0.0676(6) Uani 1 1 d . . .
S4 S 0.30370(13) 1.0358(2) 0.50291(16) 0.0970(9) Uani 1 1 d . . .
S5 S 0.30388(12) 1.03758(17) 0.35456(16) 0.0827(8) Uani 1 1 d . . .
O1 O 0.0851(3) 0.8110(4) 0.2976(3) 0.0764(17) Uani 1 1 d . . .
O2 O 0.4127(3) 1.0726(5) 0.4943(4) 0.109(2) Uani 1 1 d . . .
C1 C 0.2268(4) 1.0092(6) 0.3487(5) 0.065(2) Uani 1 1 d . . .
C2 C 0.2270(4) 1.0073(6) 0.4165(5) 0.067(2) Uani 1 1 d . . .
C3 C 0.3522(5) 1.0557(6) 0.4576(6) 0.087(3) Uani 1 1 d . . .
N1 N 0.4323(3) 0.7467(4) 0.4434(4) 0.0653(19) Uani 1 1 d . . .
C10 C 0.4478(4) 0.8229(6) 0.5046(5) 0.072(2) Uani 1 1 d . . .
H10A H 0.4904 0.8539 0.5173 0.087 Uiso 1 1 calc R . .
H10B H 0.4119 0.8708 0.4810 0.087 Uiso 1 1 calc R . .
C11 C 0.4540(5) 0.7893(7) 0.5807(6) 0.090(3) Uani 1 1 d . . .
H11A H 0.4905 0.7425 0.6060 0.108 Uiso 1 1 calc R . .
H11B H 0.4116 0.7589 0.5693 0.108 Uiso 1 1 calc R . .
C12 C 0.4691(5) 0.8729(7) 0.6361(6) 0.094(3) Uani 1 1 d . . .
H12A H 0.4354 0.9226 0.6080 0.112 Uiso 1 1 calc R . .
H12B H 0.4646 0.8522 0.6802 0.112 Uiso 1 1 calc R . .
C13 C 0.5383(6) 0.9131(9) 0.6673(6) 0.140(5) Uani 1 1 d . . .
H13A H 0.5444 0.9671 0.7005 0.210 Uiso 1 1 calc R . .
H13B H 0.5434 0.9330 0.6239 0.210 Uiso 1 1 calc R . .
H13C H 0.5720 0.8654 0.6978 0.210 Uiso 1 1 calc R . .
C14 C 0.4863(4) 0.6683(6) 0.4763(5) 0.068(2) Uani 1 1 d . . .
H14A H 0.4829 0.6347 0.5173 0.082 Uiso 1 1 calc R . .
H14B H 0.4751 0.6229 0.4341 0.082 Uiso 1 1 calc R . .
C15 C 0.5587(5) 0.6985(6) 0.5102(6) 0.085(3) Uani 1 1 d . . .
H15A H 0.5650 0.7199 0.4674 0.102 Uiso 1 1 calc R . .
H15B H 0.5680 0.7524 0.5454 0.102 Uiso 1 1 calc R . .
C16 C 0.6087(5) 0.6217(7) 0.5546(6) 0.094(3) Uani 1 1 d . . .
H16A H 0.6002 0.5690 0.5186 0.112 Uiso 1 1 calc R . .
H16B H 0.6008 0.5986 0.5957 0.112 Uiso 1 1 calc R . .
C17 C 0.6820(5) 0.6507(8) 0.5922(7) 0.124(4) Uani 1 1 d . . .
H17A H 0.7109 0.5969 0.6193 0.185 Uiso 1 1 calc R . .
H17B H 0.6916 0.7013 0.6295 0.185 Uiso 1 1 calc R . .
H17C H 0.6908 0.6726 0.5520 0.185 Uiso 1 1 calc R . .
C18 C 0.3632(4) 0.6983(6) 0.4165(6) 0.078(3) Uani 1 1 d . . .
H18A H 0.3561 0.6491 0.3781 0.094 Uiso 1 1 calc R . .
H18B H 0.3662 0.6665 0.4620 0.094 Uiso 1 1 calc R . .
C19 C 0.3006(5) 0.7627(8) 0.3798(7) 0.128(5) Uani 1 1 d . . .
H19A H 0.3037 0.8081 0.3445 0.154 Uiso 1 1 calc R . .
H19B H 0.2994 0.7984 0.4213 0.154 Uiso 1 1 calc R . .
C20 C 0.2313(6) 0.7016(13) 0.3310(9) 0.194(7) Uani 1 1 d D . .
H20A H 0.1923 0.7415 0.2963 0.233 Uiso 1 1 calc R . .
H20B H 0.2358 0.6507 0.3005 0.233 Uiso 1 1 calc R . .
C21 C 0.2275(8) 0.6663(15) 0.3957(11) 0.270(13) Uani 1 1 d D . .
H21A H 0.1899 0.6224 0.3768 0.405 Uiso 1 1 calc R . .
H21B H 0.2205 0.7185 0.4224 0.405 Uiso 1 1 calc R . .
H21C H 0.2694 0.6340 0.4319 0.405 Uiso 1 1 calc R . .
C22 C 0.4306(4) 0.7983(6) 0.3734(5) 0.072(3) Uani 1 1 d . . .
H22A H 0.3978 0.8503 0.3569 0.087 Uiso 1 1 calc R . .
H22B H 0.4753 0.8265 0.3922 0.087 Uiso 1 1 calc R . .
C23 C 0.4124(5) 0.7385(7) 0.3024(6) 0.097(3) Uani 1 1 d . . .
H23A H 0.3704 0.7036 0.2863 0.116 Uiso 1 1 calc R . .
H23B H 0.4486 0.6926 0.3153 0.116 Uiso 1 1 calc R . .
C24 C 0.4028(6) 0.8030(8) 0.2345(6) 0.123(4) Uani 1 1 d . . .
H24A H 0.3663 0.8482 0.2220 0.147 Uiso 1 1 calc R . .
H24B H 0.4446 0.8391 0.2520 0.147 Uiso 1 1 calc R . .
C25 C 0.3859(8) 0.7491(10) 0.1613(8) 0.181(6) Uani 1 1 d . . .
H25A H 0.3807 0.7930 0.1210 0.272 Uiso 1 1 calc R . .
H25B H 0.3439 0.7145 0.1427 0.272 Uiso 1 1 calc R . .
H25C H 0.4222 0.7049 0.1729 0.272 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
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
O1 Mo1 S1 108.1(2) . 2 ?
O1 Mo1 S1 109.47(18) . . ?
S1 Mo1 S1 99.38(8) 2 . ?
O1 Mo1 S2 105.1(2) . . ?
S1 Mo1 S2 145.43(9) 2 . ?
S1 Mo1 S2 78.13(8) . . ?
O1 Mo1 S3 103.41(18) . . ?
S1 Mo1 S3 79.58(8) 2 . ?
S1 Mo1 S3 145.52(9) . . ?
S2 Mo1 S3 83.68(8) . . ?
O1 Mo1 Mo1 98.76(18) . 2 ?
S1 Mo1 Mo1 53.09(6) 2 2 ?
S1 Mo1 Mo1 52.65(6) . 2 ?
S2 Mo1 Mo1 130.19(7) . 2 ?
S3 Mo1 Mo1 132.04(7) . 2 ?
Mo1 S1 Mo1 74.26(7) 2 . ?
C2 S2 Mo1 103.6(3) . . ?
C1 S3 Mo1 103.3(3) . . ?
C2 S4 C3 96.7(5) . . ?
C1 S5 C3 96.9(5) . . ?
C2 C1 S3 122.9(6) . . ?
C2 C1 S5 117.0(7) . . ?
S3 C1 S5 120.1(5) . . ?
C1 C2 S2 123.1(7) . . ?
C1 C2 S4 117.2(7) . . ?
S2 C2 S4 119.4(5) . . ?
O2 C3 S5 124.3(8) . . ?
O2 C3 S4 123.3(9) . . ?
S5 C3 S4 112.2(5) . . ?
C10 N1 C14 111.4(6) . . ?
C10 N1 C18 111.4(6) . . ?
C14 N1 C18 106.7(6) . . ?
C10 N1 C22 105.7(6) . . ?
C14 N1 C22 111.3(6) . . ?
C18 N1 C22 110.4(7) . . ?
C11 C10 N1 115.9(7) . . ?
C10 C11 C12 110.2(7) . . ?
C13 C12 C11 113.1(9) . . ?
C15 C14 N1 116.8(7) . . ?
C16 C15 C14 113.3(8) . . ?
C15 C16 C17 114.8(9) . . ?
C19 C18 N1 116.5(7) . . ?
C18 C19 C20 111.2(9) . . ?
C21 C20 C19 98.4(14) . . ?
C23 C22 N1 116.3(7) . . ?
C22 C23 C24 109.5(8) . . ?
C25 C24 C23 113.3(10) . . ?
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 O1 1.665(5) . ?
Mo1 S1 2.326(2) 2 ?
Mo1 S1 2.340(2) . ?
Mo1 S2 2.402(3) . ?
Mo1 S3 2.429(2) . ?
Mo1 Mo1 2.8162(15) 2 ?
S1 Mo1 2.326(2) 2 ?
S2 C2 1.740(8) . ?
S3 C1 1.734(9) . ?
S4 C2 1.743(9) . ?
S4 C3 1.762(10) . ?
S5 C1 1.744(8) . ?
S5 C3 1.755(11) . ?
O2 C3 1.204(10) . ?
C1 C2 1.331(10) . ?
N1 C10 1.506(9) . ?
N1 C14 1.521(9) . ?
N1 C18 1.535(9) . ?
N1 C22 1.536(9) . ?
C10 C11 1.505(11) . ?
C11 C12 1.511(12) . ?
C12 C13 1.475(12) . ?
C14 C15 1.487(11) . ?
C15 C16 1.479(11) . ?
C16 C17 1.493(12) . ?
C18 C19 1.518(12) . ?
C19 C20 1.605(17) . ?
C20 C21 1.409(9) . ?
C22 C23 1.493(11) . ?
C23 C24 1.530(12) . ?
C24 C25 1.490(14) . ?
