#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321994.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_4321994
loop_
_publ_author_name
'C. Simonnet-Jégat'
'E. Cadusseau'
'R. Dessapt'
'F. Sécheresse'
_publ_section_title
;
 Synthesis and Structural Characterizations of New Mononuclear and
 Dinuclear Molybdenum(V) Anions Containing Trithiocarbonate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2335
_journal_page_last               2339
_journal_paper_doi               10.1021/ic980907m
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H60 Mo N3 S12'
_chemical_formula_weight         919.45
_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                 102.9510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5249(5)
_cell_length_b                   11.8058(4)
_cell_length_c                   20.2942(5)
_cell_measurement_reflns_used    11176
_cell_measurement_temperature    296(2)
_cell_volume                     4325.5(2)
_computing_cell_refinement       'Bruker AXS SMART'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SMART'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device
'three-circle diffractometer with CCD area detector'
_diffrn_measurement_method       '3D profiles from 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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29192
_diffrn_reflns_theta_max         29.76
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  59.64
_exptl_absorpt_correction_T_min  3
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          .86
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0007(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   1.020
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         11176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         -0.271
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0906P)²+2.1768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1663
_refine_ls_wR_factor_obs         0.1416
_reflns_number_observed          7518
_reflns_number_total             11176
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980907m_1.cif
_cod_data_source_block           (NEt4)3[Mo(CS3)4]_compound1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+2.1768P] 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^)+(0.0906P)^2^+2.1768P] 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               4321994
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
Mo1 Mo 0.52050(2) 0.31527(3) 0.246121(15) 0.03946(11) Uani 1 d . .
S4 S 0.64158(6) 0.31755(10) 0.20718(6) 0.0560(3) Uani 1 d . .
S7 S 0.47954(6) 0.43503(9) 0.14319(5) 0.0497(2) Uani 1 d . .
S2 S 0.50812(6) 0.17271(9) 0.14948(5) 0.0503(2) Uani 1 d . .
S1 S 0.39813(6) 0.21859(10) 0.21944(6) 0.0547(3) Uani 1 d . .
S8 S 0.43604(6) 0.47753(10) 0.26345(6) 0.0592(3) Uani 1 d . .
S10 S 0.57835(7) 0.14384(11) 0.30922(6) 0.0638(3) Uani 1 d . .
S11 S 0.49727(8) 0.30028(12) 0.36424(6) 0.0689(3) Uani 1 d . .
S5 S 0.60906(6) 0.46166(10) 0.30356(6) 0.0588(3) Uani 1 d . .
S3 S 0.35862(8) 0.06537(12) 0.09814(6) 0.0745(4) Uani 1 d . .
S6 S 0.75321(6) 0.49909(12) 0.26317(7) 0.0709(4) Uani 1 d . .
S9 S 0.38218(8) 0.63702(12) 0.14731(8) 0.0795(4) Uani 1 d . .
S12 S 0.54681(11) 0.0917(2) 0.44572(7) 0.1065(6) Uani 1 d . .
C1 C 0.4179(2) 0.1465(3) 0.1525(2) 0.0496(9) Uani 1 d . .
C2 C 0.6731(2) 0.4300(3) 0.2583(2) 0.0503(9) Uani 1 d . .
C4 C 0.5427(3) 0.1734(4) 0.3772(2) 0.0671(13) Uani 1 d . .
C3 C 0.4296(2) 0.5245(3) 0.1818(2) 0.0516(9) Uani 1 d . .
N1 N 0.3716(2) 0.2710(3) -0.0957(2) 0.0478(7) Uani 1 d . .
C12 C 0.4045(3) 0.3226(4) -0.1528(2) 0.0633(12) Uani 1 d . .
N2 N 0.1567(2) 0.3656(3) 0.1722(2) 0.0597(9) Uani 1 d . .
C10 C 0.4009(3) 0.1506(4) -0.0787(3) 0.0648(12) Uani 1 d . .
C11 C 0.3941(3) 0.3435(4) -0.0329(2) 0.0657(12) Uani 1 d . .
C22 C 0.2155(2) 0.3809(5) 0.2364(2) 0.0652(12) Uani 1 d . .
C13 C 0.2872(2) 0.2659(5) -0.1212(2) 0.0635(11) Uani 1 d . .
C21 C 0.1808(4) 0.4222(5) 0.1117(3) 0.086(2) Uani 1 d . .
C23 C 0.0847(3) 0.4269(5) 0.1767(4) 0.102(2) Uani 1 d . .
C130 C 0.2459(3) 0.2265(6) -0.0679(3) 0.0799(15) Uani 1 d . .
C220 C 0.2379(3) 0.5009(5) 0.2547(3) 0.083(2) Uani 1 d . .
C110 C 0.3650(4) 0.4639(5) -0.0407(3) 0.086(2) Uani 1 d . .
C20 C 0.1488(4) 0.2385(5) 0.1632(3) 0.087(2) Uani 1 d . .
C200 C 0.0892(7) 0.2041(7) 0.0996(5) 0.180(5) Uani 1 d . .
C100 C 0.4849(3) 0.1409(6) -0.0593(4) 0.093(2) Uani 1 d . .
C120 C 0.3909(4) 0.2513(6) -0.2170(3) 0.090(2) Uani 1 d . .
C210 C 0.2533(4) 0.3785(7) 0.0994(3) 0.107(2) Uani 1 d . .
N3 N 0.6958(2) 0.6991(3) 0.4777(2) 0.0546(8) Uani 1 d . .
C30 C 0.3405(5) 0.2539(7) -0.4067(4) 0.077(2) Uani 0.67 d P .
C31 C 0.2792(4) 0.7939(9) -0.0086(4) 0.081(2) Uani 0.67 d P .
C230 C 0.0509(4) 0.3830(7) 0.2368(5) 0.134(3) Uani 1 d . .
C32 C 0.6725(5) 0.5759(7) 0.4798(4) 0.073(2) Uani 0.67 d P .
C310 C 0.3185(4) 0.8437(7) -0.0556(4) 0.115(3) Uani 1 d . .
C330 C 0.6881(4) 0.7356(8) 0.6021(3) 0.111(2) Uani 1 d . .
C33 C 0.6656(5) 0.7692(8) 0.5304(4) 0.083(2) Uani 0.67 d P .
C300 C 0.3178(5) 0.1398(7) -0.3907(4) 0.125(3) Uani 1 d . .
C320 C 0.5962(5) 0.5516(8) 0.4791(4) 0.134(3) Uani 1 d . .
C301 C 0.3062(14) 0.1775(23) -0.4540(16) 0.135(10) Uani 0.33 d P .
C311 C 0.2467(10) 0.8720(17) -0.0557(11) 0.090(5) Uani 0.33 d P .
C331 C 0.7286(11) 0.6976(17) 0.5580(10) 0.091(6) Uani 0.33 d P .
C321 C 0.6232(12) 0.6433(29) 0.4643(11) 0.127(10) Uani 0.33 d P .
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'
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
S5 Mo1 S1 153.48(4) . . ?
S5 Mo1 S7 92.49(4) . . ?
S1 Mo1 S7 89.23(4) . . ?
S5 Mo1 S10 99.22(4) . . ?
S1 Mo1 S10 90.30(4) . . ?
S7 Mo1 S10 154.29(4) . . ?
S5 Mo1 S11 80.75(4) . . ?
S1 Mo1 S11 80.46(4) . . ?
S7 Mo1 S11 138.33(4) . . ?
S10 Mo1 S11 66.66(4) . . ?
S5 Mo1 S4 66.57(4) . . ?
S1 Mo1 S4 139.69(4) . . ?
S7 Mo1 S4 81.81(4) . . ?
S10 Mo1 S4 82.01(4) . . ?
S11 Mo1 S4 130.08(4) . . ?
S5 Mo1 S8 76.92(4) . . ?
S1 Mo1 S8 79.47(4) . . ?
S7 Mo1 S8 66.96(4) . . ?
S10 Mo1 S8 137.99(4) . . ?
S11 Mo1 S8 71.47(4) . . ?
S4 Mo1 S8 130.36(4) . . ?
S5 Mo1 S2 138.94(4) . . ?
S1 Mo1 S2 67.04(3) . . ?
S7 Mo1 S2 76.85(4) . . ?
S10 Mo1 S2 79.32(4) . . ?
S11 Mo1 S2 132.44(4) . . ?
S4 Mo1 S2 72.65(3) . . ?
S8 Mo1 S2 130.47(4) . . ?
C2 S4 Mo1 91.40(14) . . ?
C3 S7 Mo1 93.5(2) . . ?
C1 S2 Mo1 90.70(14) . . ?
C1 S1 Mo1 93.12(14) . . ?
C3 S8 Mo1 91.24(14) . . ?
C4 S10 Mo1 92.9(2) . . ?
C4 S11 Mo1 91.4(2) . . ?
C2 S5 Mo1 93.50(14) . . ?
S3 C1 S1 125.7(3) . . ?
S3 C1 S2 125.6(3) . . ?
S1 C1 S2 108.8(2) . . ?
S6 C2 S5 125.3(3) . . ?
S6 C2 S4 126.3(3) . . ?
S5 C2 S4 108.4(2) . . ?
S12 C4 S10 127.0(4) . . ?
S12 C4 S11 124.0(3) . . ?
S10 C4 S11 108.9(2) . . ?
S9 C3 S7 126.4(3) . . ?
S9 C3 S8 125.4(3) . . ?
S7 C3 S8 108.3(2) . . ?
C11 N1 C10 108.5(3) . . ?
C11 N1 C13 112.0(3) . . ?
C10 N1 C13 108.8(3) . . ?
C11 N1 C12 109.1(3) . . ?
C10 N1 C12 110.7(3) . . ?
C13 N1 C12 107.8(3) . . ?
C120 C12 N1 113.9(4) . . ?
C22 N2 C20 104.7(4) . . ?
C22 N2 C23 111.2(4) . . ?
C20 N2 C23 114.3(4) . . ?
C22 N2 C21 110.6(4) . . ?
C20 N2 C21 111.6(4) . . ?
C23 N2 C21 104.6(4) . . ?
C100 C10 N1 114.7(4) . . ?
N1 C11 C110 114.6(4) . . ?
C220 C22 N2 115.6(4) . . ?
C130 C13 N1 113.9(4) . . ?
C210 C21 N2 114.1(5) . . ?
N2 C23 C230 113.0(5) . . ?
N2 C20 C200 113.0(5) . . ?
C321 N3 C31 156.4(15) . 4_676 ?
C321 N3 C32 47.3(14) . . ?
C31 N3 C32 109.4(6) 4_676 . ?
C321 N3 C311 107.5(13) . 4_676 ?
C31 N3 C311 53.4(8) 4_676 4_676 ?
C32 N3 C311 72.1(9) . 4_676 ?
C321 N3 C301 114.3(17) . 3_665 ?
C31 N3 C301 87.6(10) 4_676 3_665 ?
C32 N3 C301 158.6(12) . 3_665 ?
C311 N3 C301 110.9(13) 4_676 3_665 ?
C321 N3 C30 78.5(12) . 3_665 ?
C31 N3 C30 111.3(5) 4_676 3_665 ?
C32 N3 C30 107.5(5) . 3_665 ?
C311 N3 C30 88.0(9) 4_676 3_665 ?
C301 N3 C30 52.6(13) 3_665 3_665 ?
C321 N3 C33 84.9(10) . . ?
C31 N3 C33 110.9(5) 4_676 . ?
C32 N3 C33 110.1(5) . . ?
C311 N3 C33 162.0(9) 4_676 . ?
C301 N3 C33 73.9(12) 3_665 . ?
C30 N3 C33 107.6(5) 3_665 . ?
C321 N3 C331 107.8(12) . . ?
C31 N3 C331 71.0(8) 4_676 . ?
C32 N3 C331 90.4(8) . . ?
C311 N3 C331 108.2(11) 4_676 . ?
C301 N3 C331 107.9(15) 3_665 . ?
C30 N3 C331 159.1(8) 3_665 . ?
C33 N3 C331 54.6(9) . . ?
C301 C30 C300 55.8(11) . . ?
C301 C30 N3 63.0(9) . 3_665 ?
C300 C30 N3 116.6(7) . 3_665 ?
C301 C30 C321 99.3(13) . 3_665 ?
C300 C30 C321 151.1(10) . 3_665 ?
N3 C30 C321 48.8(7) 3_665 3_665 ?
C311 C31 C310 58.2(9) . . ?
C311 C31 N3 64.1(8) . 4_575 ?
C310 C31 N3 120.1(7) . 4_575 ?
C311 C31 C331 105.3(11) . 4_575 ?
C310 C31 C331 152.8(10) . 4_575 ?
N3 C31 C331 56.9(6) 4_575 4_575 ?
C321 C32 C320 56.0(13) . . ?
C321 C32 N3 64.0(11) . . ?
C320 C32 N3 118.3(7) . . ?
C321 C32 C311 105.9(14) . 4_676 ?
C320 C32 C311 154.4(10) . 4_676 ?
N3 C32 C311 54.2(7) . 4_676 ?
C311 C310 C31 57.9(9) . . ?
C331 C330 C33 61.1(8) . . ?
C331 C33 C330 55.8(9) . . ?
C331 C33 N3 64.6(9) . . ?
C330 C33 N3 118.1(7) . . ?
C331 C33 C301 99.7(12) . 3_665 ?
C330 C33 C301 147.9(11) . 3_665 ?
N3 C33 C301 52.6(9) . 3_665 ?
C331 C33 C321 89.2(13) . . ?
C330 C33 C321 115.8(11) . . ?
N3 C33 C321 45.8(6) . . ?
C301 C33 C321 80.6(13) 3_665 . ?
C301 C300 C30 58.2(14) . . ?
C321 C320 C32 52.2(13) . . ?
C300 C301 C30 66.0(17) . . ?
C300 C301 N3 127.5(26) . 3_665 ?
C30 C301 N3 64.4(13) . 3_665 ?
C300 C301 C33 155.0(19) . 3_665 ?
C30 C301 C33 101.0(15) . 3_665 ?
N3 C301 C33 53.5(8) 3_665 3_665 ?
C31 C311 C310 63.9(10) . . ?
C31 C311 N3 62.5(9) . 4_575 ?
C310 C311 N3 124.0(14) . 4_575 ?
C31 C311 C32 102.0(12) . 4_575 ?
C310 C311 C32 155.7(16) . 4_575 ?
N3 C311 C32 53.7(6) 4_575 4_575 ?
C330 C331 C33 63.1(11) . . ?
C330 C331 N3 121.5(14) . . ?
C33 C331 N3 60.8(7) . . ?
C330 C331 C31 157.2(15) . 4_676 ?
C33 C331 C31 100.7(11) . 4_676 ?
N3 C331 C31 52.0(7) . 4_676 ?
C32 C321 C320 71.7(23) . . ?
C32 C321 N3 68.7(10) . . ?
C320 C321 N3 137.7(27) . . ?
C32 C321 C30 103.3(13) . 3_665 ?
C320 C321 C30 155.2(15) . 3_665 ?
N3 C321 C30 52.7(9) . 3_665 ?
C32 C321 C33 98.8(11) . . ?
C320 C321 C33 125.9(16) . . ?
N3 C321 C33 49.3(7) . . ?
C30 C321 C33 78.6(10) 3_665 . ?
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 S5 2.4860(11) . ?
Mo1 S1 2.4868(10) . ?
Mo1 S7 2.4956(10) . ?
Mo1 S10 2.5038(12) . ?
Mo1 S11 2.5348(11) . ?
Mo1 S4 2.5400(11) . ?
Mo1 S8 2.5471(11) . ?
Mo1 S2 2.5553(10) . ?
S4 C2 1.705(4) . ?
S7 C3 1.706(4) . ?
S2 C1 1.714(4) . ?
S1 C1 1.711(4) . ?
S8 C3 1.726(5) . ?
S10 C4 1.694(5) . ?
S11 C4 1.710(6) . ?
S5 C2 1.696(4) . ?
S3 C1 1.672(4) . ?
S6 C2 1.677(4) . ?
S9 C3 1.658(4) . ?
S12 C4 1.680(5) . ?
N1 C11 1.514(5) . ?
N1 C10 1.534(6) . ?
N1 C13 1.534(5) . ?
N1 C12 1.550(5) . ?
C12 C120 1.524(8) . ?
N2 C22 1.511(5) . ?
N2 C20 1.515(7) . ?
N2 C23 1.536(7) . ?
N2 C21 1.550(6) . ?
C10 C100 1.522(7) . ?
C11 C110 1.516(7) . ?
C22 C220 1.499(8) . ?
C13 C130 1.532(7) . ?
C21 C210 1.512(9) . ?
C23 C230 1.578(10) . ?
C20 C200 1.552(9) . ?
N3 C321 1.47(2) . ?
N3 C31 1.510(8) 4_676 ?
N3 C32 1.521(8) . ?
N3 C311 1.53(2) 4_676 ?
N3 C301 1.53(2) 3_665 ?
N3 C30 1.551(8) 3_665 ?
N3 C33 1.551(8) . ?
N3 C331 1.61(2) . ?
C30 C301 1.37(3) . ?
C30 C300 1.469(12) . ?
C30 N3 1.551(8) 3_665 ?
C30 C321 1.91(3) 3_665 ?
C31 C311 1.37(2) . ?
C31 C310 1.448(11) . ?
C31 N3 1.510(8) 4_575 ?
C31 C331 1.81(2) 4_575 ?
C32 C321 1.20(3) . ?
C32 C320 1.440(12) . ?
C32 C311 1.80(2) 4_676 ?
C310 C311 1.37(2) . ?
C330 C331 1.37(2) . ?
C330 C33 1.475(11) . ?
C33 C331 1.45(2) . ?
C33 C301 1.85(3) 3_665 ?
C33 C321 2.04(2) . ?
C300 C301 1.33(3) . ?
C320 C321 1.26(3) . ?
C301 N3 1.53(2) 3_665 ?
C301 C33 1.85(3) 3_665 ?
C311 N3 1.53(2) 4_575 ?
C311 C32 1.80(2) 4_575 ?
C331 C31 1.81(2) 4_676 ?
C321 C30 1.91(3) 3_665 ?
