#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321062.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_4321062
loop_
_publ_author_name
'Mingming Miao'
'Michael W. Willer'
'R. H. Holm'
_publ_contact_author             R.H.Holm
_publ_contact_author_address
;
    Dept. of Chemistry and Chemical Biology
    Harvard University
    Cambridge, MA 02138
    USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_section_title
;
 Oxo/Sulfidotungstate(VI) as Precursors to WVIO2, WVIOS, and WVIS2
 Complexes and WIV-Dithiolene Chelate Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2843
_journal_page_last               2849
_journal_paper_doi               10.1021/ic000047l
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C71 H56 Mo N2 O2 S2 Si2'
_chemical_formula_weight         1185.42
_chemical_name_systematic
;
  [Mo(S2C2Ph2)(OSiPh3)2(Me4phen)](C5H12)
;
_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                 112.4420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0685(10)
_cell_length_b                   19.3165(10)
_cell_length_c                   17.7183(9)
_cell_measurement_temperature    213(2)
_cell_volume                     6032.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19681
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.374
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         7269
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0759P)²+9.8704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                6346
_reflns_number_total             7269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000047l_5.cif
_cod_data_source_block           compound_6
_cod_database_code               4321062
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 -1.0000 -2.034402(14) 0.7500 0.02822(10) Uani 1 2 d S . .
O1 O -0.90336(10) -2.01696(9) 0.74627(11) 0.0334(4) Uani 1 1 d . . .
S1 S -1.03662(4) -2.12276(3) 0.65586(3) 0.03227(15) Uani 1 1 d . . .
N1 N -0.96947(12) -1.94086(11) 0.83259(13) 0.0335(4) Uani 1 1 d . . .
Si1 Si -0.81276(4) -2.00277(4) 0.77619(4) 0.03161(16) Uani 1 1 d . . .
C1 C -1.01477(14) -2.20333(13) 0.70898(14) 0.0324(5) Uani 1 1 d . . .
C2 C -1.02859(16) -2.26437(13) 0.65432(15) 0.0362(5) Uani 1 1 d . . .
C3 C -1.09493(17) -2.26892(15) 0.58404(17) 0.0423(6) Uani 1 1 d . . .
H3A H -1.1322 -2.2343 0.5730 0.051 Uiso 1 1 calc R . .
C4 C -1.1062(2) -2.32411(18) 0.53042(19) 0.0552(8) Uani 1 1 d . . .
H4A H -1.1512 -2.3267 0.4837 0.066 Uiso 1 1 calc R . .
C5 C -1.0524(3) -2.37470(18) 0.5449(2) 0.0644(10) Uani 1 1 d . . .
H5A H -1.0605 -2.4121 0.5086 0.077 Uiso 1 1 calc R . .
C6 C -0.9859(3) -2.37033(18) 0.6136(2) 0.0676(10) Uani 1 1 d . . .
H6A H -0.9483 -2.4044 0.6233 0.081 Uiso 1 1 calc R . .
C7 C -0.9746(2) -2.31602(16) 0.66783(19) 0.0523(8) Uani 1 1 d . . .
H7A H -0.9296 -2.3141 0.7147 0.063 Uiso 1 1 calc R . .
C8 C -0.94169(16) -1.94136(16) 0.91344(17) 0.0403(6) Uani 1 1 d . . .
H8A H -0.9291 -1.9844 0.9399 0.048 Uiso 1 1 calc R . .
C9 C -0.92987(17) -1.88198(17) 0.96203(19) 0.0454(7) Uani 1 1 d . . .
C10 C -0.94622(16) -1.81831(16) 0.9244(2) 0.0474(7) Uani 1 1 d . . .
C11 C -0.97272(15) -1.81578(15) 0.8374(2) 0.0416(6) Uani 1 1 d . . .
C12 C -0.98506(14) -1.87875(13) 0.79399(17) 0.0344(5) Uani 1 1 d . . .
C13 C -0.98744(17) -1.75271(15) 0.7911(2) 0.0522(8) Uani 1 1 d . . .
H13A H -0.9791 -1.7095 0.8199 0.063 Uiso 1 1 d R . .
C14 C -0.9380(2) -1.7524(2) 0.9730(3) 0.0696(11) Uani 1 1 d . . .
H14A H -0.9194 -1.7634 1.0307 0.104 Uiso 1 1 calc R . .
H14B H -0.9870 -1.7298 0.9568 0.104 Uiso 1 1 calc R . .
H14C H -0.9025 -1.7217 0.9625 0.104 Uiso 1 1 calc R . .
C15 C -0.8994(2) -1.8911(2) 1.0537(2) 0.0643(10) Uani 1 1 d . . .
H15A H -0.8936 -1.8461 1.0797 0.096 Uiso 1 1 calc R . .
H15B H -0.8506 -1.9141 1.0717 0.096 Uiso 1 1 calc R . .
H15C H -0.9346 -1.9189 1.0685 0.096 Uiso 1 1 calc R . .
C16 C -0.76369(16) -2.08816(15) 0.78414(16) 0.0387(6) Uani 1 1 d . . .
C17 C -0.6855(2) -2.0924(2) 0.8097(3) 0.0681(10) Uani 1 1 d . . .
H17A H -0.6561 -2.0521 0.8273 0.082 Uiso 1 1 calc R . .
C18 C -0.6497(2) -2.1553(2) 0.8098(3) 0.0818(13) Uani 1 1 d . . .
H18A H -0.5967 -2.1570 0.8259 0.098 Uiso 1 1 calc R . .
C19 C -0.6921(3) -2.2152(2) 0.7861(3) 0.0715(11) Uani 1 1 d . . .
H19A H -0.6682 -2.2578 0.7862 0.086 Uiso 1 1 calc R . .
C20 C -0.7685(3) -2.21195(19) 0.7627(3) 0.0724(11) Uani 1 1 d . . .
H20A H -0.7975 -2.2527 0.7472 0.087 Uiso 1 1 calc R . .
C21 C -0.8047(2) -2.14873(17) 0.7612(2) 0.0544(8) Uani 1 1 d . . .
H21A H -0.8578 -2.1475 0.7443 0.065 Uiso 1 1 calc R . .
C22 C -0.77560(16) -1.95572(15) 0.87615(17) 0.0386(6) Uani 1 1 d . . .
C23 C -0.7557(2) -1.9912(2) 0.9500(2) 0.0614(9) Uani 1 1 d . . .
H23A H -0.7577 -2.0398 0.9503 0.074 Uiso 1 1 calc R . .
C24 C -0.7326(3) -1.9545(3) 1.0238(2) 0.0818(13) Uani 1 1 d . . .
H24A H -0.7199 -1.9786 1.0733 0.098 Uiso 1 1 calc R . .
C25 C -0.7282(2) -1.8835(2) 1.0244(2) 0.0725(11) Uani 1 1 d . . .
H25A H -0.7116 -1.8592 1.0741 0.087 Uiso 1 1 calc R . .
C26 C -0.7482(2) -1.8486(2) 0.9526(2) 0.0611(9) Uani 1 1 d . . .
H26A H -0.7459 -1.8000 0.9530 0.073 Uiso 1 1 calc R . .
C27 C -0.77194(18) -1.88375(16) 0.8789(2) 0.0470(7) Uani 1 1 d . . .
H27A H -0.7858 -1.8586 0.8299 0.056 Uiso 1 1 calc R . .
C28 C -0.79634(15) -1.94581(14) 0.69862(15) 0.0345(5) Uani 1 1 d . . .
C29 C -0.72395(17) -1.92563(18) 0.70670(18) 0.0485(7) Uani 1 1 d . . .
H29A H -0.6821 -1.9408 0.7523 0.058 Uiso 1 1 calc R . .
C30 C -0.71151(19) -1.88377(19) 0.6495(2) 0.0538(8) Uani 1 1 d . . .
H30A H -0.6618 -1.8714 0.6562 0.065 Uiso 1 1 calc R . .
C31 C -0.77245(19) -1.86033(18) 0.58266(19) 0.0528(8) Uani 1 1 d . . .
H31A H -0.7644 -1.8320 0.5435 0.063 Uiso 1 1 calc R . .
C32 C -0.84498(19) -1.87863(18) 0.5736(2) 0.0537(8) Uani 1 1 d . . .
H32A H -0.8867 -1.8625 0.5285 0.064 Uiso 1 1 calc R . .
C33 C -0.85668(16) -1.92114(16) 0.63146(17) 0.0429(6) Uani 1 1 d . . .
H33A H -0.9065 -1.9333 0.6247 0.051 Uiso 1 1 calc R . .
C1S C -1.0236(4) -2.5581(4) 0.6295(5) 0.0441(15) Uiso 0.50 1 d P A 1
C2S C -1.0355(6) -2.5362(5) 0.7052(7) 0.067(2) Uiso 0.50 1 d PD . 1
C1T C -1.0298(3) -2.5611(3) 0.6004(4) 0.0365(13) Uiso 0.50 1 d P . 2
C2T C -1.0302(7) -2.5462(6) 0.6767(8) 0.087(3) Uiso 0.50 1 d PD . 2
C3S C -1.0000 -2.5274(8) 0.7500 0.175(6) Uiso 1 2 d SD . .
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'
Si Si 0.0817 0.0704 '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 O1 159.57(11) . 2_356 ?
O1 Mo1 N1 82.36(8) . . ?
O1 Mo1 N1 81.32(8) 2_356 . ?
O1 Mo1 N1 81.32(8) . 2_356 ?
O1 Mo1 N1 82.36(8) 2_356 2_356 ?
N1 Mo1 N1 73.64(11) . 2_356 ?
O1 Mo1 S1 97.83(6) . . ?
O1 Mo1 S1 97.29(6) 2_356 . ?
N1 Mo1 S1 174.64(6) . . ?
N1 Mo1 S1 101.07(6) 2_356 . ?
O1 Mo1 S1 97.29(6) . 2_356 ?
O1 Mo1 S1 97.83(6) 2_356 2_356 ?
N1 Mo1 S1 101.07(6) . 2_356 ?
N1 Mo1 S1 174.64(6) 2_356 2_356 ?
S1 Mo1 S1 84.23(3) . 2_356 ?
Si1 O1 Mo1 160.61(12) . . ?
C1 S1 Mo1 108.64(8) . . ?
C8 N1 C12 118.2(2) . . ?
C8 N1 Mo1 126.38(19) . . ?
C12 N1 Mo1 115.37(17) . . ?
O1 Si1 C22 111.21(11) . . ?
O1 Si1 C16 108.30(11) . . ?
C22 Si1 C16 110.98(13) . . ?
O1 Si1 C28 108.28(11) . . ?
C22 Si1 C28 107.41(12) . . ?
C16 Si1 C28 110.64(12) . . ?
C1 C1 C2 127.06(14) 2_356 . ?
C1 C1 S1 119.20(8) 2_356 . ?
C2 C1 S1 113.66(17) . . ?
C7 C2 C3 117.9(3) . . ?
C7 C2 C1 121.6(3) . . ?
C3 C2 C1 120.4(3) . . ?
C4 C3 C2 120.5(3) . . ?
C5 C4 C3 120.7(3) . . ?
C4 C5 C6 119.4(3) . . ?
C7 C6 C5 120.3(4) . . ?
C6 C7 C2 121.2(3) . . ?
N1 C8 C9 124.3(3) . . ?
C10 C9 C8 118.7(3) . . ?
C10 C9 C15 123.2(3) . . ?
C8 C9 C15 118.1(3) . . ?
C9 C10 C11 118.3(3) . . ?
C9 C10 C14 121.4(3) . . ?
C11 C10 C14 120.2(3) . . ?
C12 C11 C10 118.4(3) . . ?
C12 C11 C13 117.8(3) . . ?
C10 C11 C13 123.8(3) . . ?
N1 C12 C11 122.0(2) . . ?
N1 C12 C12 117.74(14) . 2_356 ?
C11 C12 C12 120.29(17) . 2_356 ?
C13 C13 C11 121.88(18) 2_356 . ?
C21 C16 C17 117.7(3) . . ?
C21 C16 Si1 120.9(2) . . ?
C17 C16 Si1 121.4(2) . . ?
C16 C17 C18 121.2(4) . . ?
C19 C18 C17 120.0(4) . . ?
C20 C19 C18 119.4(3) . . ?
C19 C20 C21 120.8(4) . . ?
C16 C21 C20 121.0(3) . . ?
C27 C22 C23 117.8(3) . . ?
C27 C22 Si1 120.9(2) . . ?
C23 C22 Si1 121.2(2) . . ?
C22 C23 C24 120.1(4) . . ?
C25 C24 C23 120.6(4) . . ?
C26 C25 C24 119.6(3) . . ?
C25 C26 C27 120.9(4) . . ?
C26 C27 C22 121.0(3) . . ?
C33 C28 C29 117.3(2) . . ?
C33 C28 Si1 120.9(2) . . ?
C29 C28 Si1 121.7(2) . . ?
C30 C29 C28 122.0(3) . . ?
C31 C30 C29 119.7(3) . . ?
C32 C31 C30 119.6(3) . . ?
C31 C32 C33 120.0(3) . . ?
C28 C33 C32 121.3(3) . . ?
C3S C2S C1S 123.9(10) . . ?
C3S C2S C2S 11.7(14) . 2_356 ?
C1S C2S C2S 120.7(10) . 2_356 ?
C3S C2T C1T 153.9(11) . . ?
C2S C3S C2S 157(3) 2_356 . ?
C2S C3S C2T 143.4(17) 2_356 . ?
C2S C3S C2T 23.1(9) . . ?
C2S C3S C2T 23.1(9) 2_356 2_356 ?
C2S C3S C2T 143.4(17) . 2_356 ?
C2T C3S C2T 146.4(18) . 2_356 ?
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 1.8991(17) . ?
Mo1 O1 1.8991(17) 2_356 ?
Mo1 N1 2.257(2) . ?
Mo1 N1 2.257(2) 2_356 ?
Mo1 S1 2.3009(6) . ?
Mo1 S1 2.3009(6) 2_356 ?
O1 Si1 1.6252(18) . ?
S1 C1 1.784(3) . ?
N1 C8 1.324(3) . ?
N1 C12 1.357(3) . ?
Si1 C22 1.873(3) . ?
Si1 C16 1.875(3) . ?
Si1 C28 1.878(3) . ?
C1 C1 1.344(5) 2_356 ?
C1 C2 1.484(3) . ?
C2 C7 1.387(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.389(4) . ?
C4 C5 1.368(6) . ?
C5 C6 1.384(6) . ?
C6 C7 1.383(4) . ?
C8 C9 1.400(4) . ?
C9 C10 1.377(5) . ?
C9 C15 1.512(5) . ?
C10 C11 1.429(5) . ?
C10 C14 1.511(4) . ?
C11 C12 1.410(4) . ?
C11 C13 1.435(4) . ?
C12 C12 1.441(5) 2_356 ?
C13 C13 1.349(7) 2_356 ?
C16 C21 1.380(4) . ?
C16 C17 1.385(4) . ?
C17 C18 1.394(5) . ?
C18 C19 1.382(6) . ?
C19 C20 1.355(6) . ?
C20 C21 1.398(5) . ?
C22 C27 1.392(4) . ?
C22 C23 1.395(4) . ?
C23 C24 1.403(5) . ?
C24 C25 1.373(6) . ?
C25 C26 1.358(6) . ?
C26 C27 1.386(4) . ?
C28 C33 1.386(4) . ?
C28 C29 1.388(4) . ?
C29 C30 1.385(4) . ?
C30 C31 1.382(5) . ?
C31 C32 1.376(5) . ?
C32 C33 1.396(4) . ?
C1S C2S 1.504(12) . ?
C2S C3S 0.842(11) . ?
C2S C2S 1.65(2) 2_356 ?
C1T C2T 1.387(14) . ?
C2T C3S 1.256(14) . ?
C3S C2S 0.842(11) 2_356 ?
C3S C2T 1.256(14) 2_356 ?
