#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:54:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179160 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/21/4312195.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_4312195
loop_
_publ_author_name
'David V. Partyka'
'R. H. Holm'
_publ_section_title
;
 Oxygen/Sulfur Substitution Reactions of Tetraoxometalates Effected by
 Electrophilic Carbon and Silicon Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8609
_journal_page_last               8616
_journal_paper_doi               10.1021/ic040097g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C22 H44 Mo N2 O3 S2'
_chemical_formula_weight         544.65
_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                104.87(3)
_cell_angle_beta                 95.78(3)
_cell_angle_gamma                116.56(3)
_cell_formula_units_Z            2
_cell_length_a                   9.815(2)
_cell_length_b                   10.689(2)
_cell_length_c                   15.045(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1321.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8883
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.678
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0546P)²+0.1739P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                4876
_reflns_number_total             6178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040097g_2.cif
_cod_data_source_block           tri1a
_cod_original_cell_volume        1321.7(5)
_cod_database_code               4312195
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
Mo1 Mo 0.81309(3) 0.57952(3) 0.737916(18) 0.03770(10) Uani 1 1 d . . .
S2 S 0.66486(12) 0.49658(10) 0.86045(6) 0.0503(2) Uani 1 1 d . . .
S1 S 0.69314(12) 0.29919(10) 0.67349(6) 0.0511(2) Uani 1 1 d . . .
O1 O 0.6889(3) 0.6196(3) 0.67520(17) 0.0505(6) Uani 1 1 d . . .
O2 O 0.9360(3) 0.7377(3) 0.83772(16) 0.0502(6) Uani 1 1 d . . .
N2 N 0.2189(3) 0.4136(3) 0.59702(17) 0.0361(5) Uani 1 1 d . . .
N1 N 0.1502(3) 0.8930(3) 0.11517(17) 0.0407(6) Uani 1 1 d . . .
O3 O 0.9415(3) 0.5657(3) 0.66757(18) 0.0572(6) Uani 1 1 d . . .
C21 C 0.0475(4) 0.3087(4) 0.5902(2) 0.0459(8) Uani 1 1 d . . .
H21A H 0.0432 0.2363 0.6193 0.055 Uiso 1 1 calc R . .
H21B H 0.0053 0.3656 0.6266 0.055 Uiso 1 1 calc R . .
C1 C 0.5481(4) 0.2174(4) 0.7317(2) 0.0476(8) Uani 1 1 d . . .
C2 C 0.5353(4) 0.3045(4) 0.8145(2) 0.0461(8) Uani 1 1 d . . .
C19 C 0.2257(4) 0.5386(3) 0.5647(2) 0.0414(7) Uani 1 1 d . . .
H19A H 0.1704 0.4973 0.4982 0.050 Uiso 1 1 calc R . .
H19B H 0.1701 0.5809 0.6001 0.050 Uiso 1 1 calc R . .
C9 C -0.0214(4) 0.7750(4) 0.0711(2) 0.0527(9) Uani 1 1 d . . .
H9A H -0.0864 0.8201 0.0868 0.063 Uiso 1 1 calc R . .
H9B H -0.0385 0.7421 0.0026 0.063 Uiso 1 1 calc R . .
C17 C 0.2892(4) 0.3356(4) 0.5353(3) 0.0494(8) Uani 1 1 d . . .
H17A H 0.4013 0.4027 0.5485 0.059 Uiso 1 1 calc R . .
H17B H 0.2437 0.3143 0.4693 0.059 Uiso 1 1 calc R . .
C22 C -0.0572(4) 0.2261(4) 0.4898(3) 0.0590(10) Uani 1 1 d . . .
H22A H -0.0437 0.2957 0.4574 0.088 Uiso 1 1 calc R . .
H22B H -0.1651 0.1751 0.4922 0.088 Uiso 1 1 calc R . .
H22C H -0.0291 0.1553 0.4565 0.088 Uiso 1 1 calc R . .
C15 C 0.3121(4) 0.4725(4) 0.6995(2) 0.0484(8) Uani 1 1 d . . .
H15A H 0.2925 0.3887 0.7204 0.058 Uiso 1 1 calc R . .
H15B H 0.4232 0.5247 0.7019 0.058 Uiso 1 1 calc R . .
C3 C 0.4217(5) 0.2353(5) 0.8611(3) 0.0585(9) Uani 1 1 d . . .
H3 H 0.4120 0.2923 0.9157 0.070 Uiso 1 1 calc R . .
C20 C 0.3893(4) 0.6621(4) 0.5766(3) 0.0533(9) Uani 1 1 d . . .
H20A H 0.4373 0.7183 0.6428 0.080 Uiso 1 1 calc R . .
H20B H 0.3834 0.7263 0.5437 0.080 Uiso 1 1 calc R . .
H20C H 0.4512 0.6203 0.5507 0.080 Uiso 1 1 calc R . .
C13 C 0.1754(4) 1.0178(4) 0.0775(2) 0.0456(8) Uani 1 1 d . . .
H13A H 0.1451 0.9776 0.0087 0.055 Uiso 1 1 calc R . .
H13B H 0.1060 1.0554 0.0977 0.055 Uiso 1 1 calc R . .
C16 C 0.2743(5) 0.5763(5) 0.7685(3) 0.0652(11) Uani 1 1 d . . .
H16A H 0.3061 0.6659 0.7537 0.098 Uiso 1 1 calc R . .
H16B H 0.3296 0.6001 0.8321 0.098 Uiso 1 1 calc R . .
H16C H 0.1631 0.5286 0.7635 0.098 Uiso 1 1 calc R . .
C11 C 0.2585(5) 0.8322(4) 0.0899(2) 0.0555(9) Uani 1 1 d . . .
H11A H 0.2308 0.7465 0.1100 0.067 Uiso 1 1 calc R . .
H11B H 0.3652 0.9070 0.1254 0.067 Uiso 1 1 calc R . .
C7 C 0.1842(5) 0.9460(4) 0.2232(2) 0.0528(9) Uani 1 1 d . . .
H7A H 0.1767 0.8653 0.2443 0.063 Uiso 1 1 calc R . .
H7B H 0.2917 1.0268 0.2486 0.063 Uiso 1 1 calc R . .
C8 C 0.0774(5) 0.9986(4) 0.2651(3) 0.0631(10) Uani 1 1 d . . .
H8A H 0.0828 1.0782 0.2445 0.095 Uiso 1 1 calc R . .
H8B H 0.1105 1.0332 0.3331 0.095 Uiso 1 1 calc R . .
H8C H -0.0288 0.9178 0.2442 0.095 Uiso 1 1 calc R . .
C18 C 0.2651(5) 0.1920(4) 0.5484(3) 0.0636(10) Uani 1 1 d . . .
H18A H 0.3081 0.2111 0.6137 0.095 Uiso 1 1 calc R . .
H18B H 0.3172 0.1522 0.5090 0.095 Uiso 1 1 calc R . .
H18C H 0.1547 0.1217 0.5309 0.095 Uiso 1 1 calc R . .
C4 C 0.3236(5) 0.0820(5) 0.8263(4) 0.0699(12) Uani 1 1 d . . .
H4 H 0.2497 0.0369 0.8582 0.084 Uiso 1 1 calc R . .
C5 C 0.3352(5) -0.0033(5) 0.7449(3) 0.0689(12) Uani 1 1 d . . .
H5 H 0.2687 -0.1057 0.7216 0.083 Uiso 1 1 calc R . .
C12 C 0.2553(5) 0.7865(5) -0.0150(3) 0.0668(11) Uani 1 1 d . . .
H12A H 0.1491 0.7178 -0.0515 0.100 Uiso 1 1 calc R . .
H12B H 0.3190 0.7400 -0.0258 0.100 Uiso 1 1 calc R . .
H12C H 0.2959 0.8729 -0.0339 0.100 Uiso 1 1 calc R . .
C6 C 0.4461(5) 0.0633(4) 0.6977(3) 0.0609(10) Uani 1 1 d . . .
H6 H 0.4530 0.0050 0.6426 0.073 Uiso 1 1 calc R . .
C14 C 0.3408(5) 1.1455(4) 0.1086(3) 0.0712(12) Uani 1 1 d . . .
H14A H 0.3724 1.1865 0.1767 0.107 Uiso 1 1 calc R . .
H14B H 0.3457 1.2206 0.0831 0.107 Uiso 1 1 calc R . .
H14C H 0.4100 1.1110 0.0859 0.107 Uiso 1 1 calc R . .
C10 C -0.0754(7) 0.6400(5) 0.1027(3) 0.0920(17) Uani 1 1 d . . .
H10A H -0.0088 0.5971 0.0904 0.138 Uiso 1 1 calc R . .
H10B H -0.1820 0.5679 0.0683 0.138 Uiso 1 1 calc R . .
H10C H -0.0696 0.6696 0.1695 0.138 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 O2 107.80(12) . . ?
O1 Mo1 O3 106.26(12) . . ?
O2 Mo1 O3 103.84(12) . . ?
O1 Mo1 S1 105.73(10) . . ?
O2 Mo1 S1 143.28(8) . . ?
O3 Mo1 S1 80.41(9) . . ?
O1 Mo1 S2 101.46(8) . . ?
O2 Mo1 S2 81.92(9) . . ?
O3 Mo1 S2 148.12(9) . . ?
S1 Mo1 S2 77.15(4) . . ?
C2 S2 Mo1 109.65(13) . . ?
C1 S1 Mo1 109.68(12) . . ?
C17 N2 C19 109.1(2) . . ?
C17 N2 C15 108.3(3) . . ?
C19 N2 C15 111.1(2) . . ?
C17 N2 C21 111.7(3) . . ?
C19 N2 C21 107.9(2) . . ?
C15 N2 C21 108.6(2) . . ?
C11 N1 C13 111.8(3) . . ?
C11 N1 C9 111.4(3) . . ?
C13 N1 C9 105.5(2) . . ?
C11 N1 C7 106.2(2) . . ?
C13 N1 C7 111.4(3) . . ?
C9 N1 C7 110.6(3) . . ?
C22 C21 N2 114.8(3) . . ?
C6 C1 C2 118.9(4) . . ?
C6 C1 S1 120.4(3) . . ?
C2 C1 S1 120.7(3) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 S2 120.8(3) . . ?
C1 C2 S2 119.9(3) . . ?
C20 C19 N2 115.1(3) . . ?
C10 C9 N1 114.7(3) . . ?
N2 C17 C18 114.8(3) . . ?
C16 C15 N2 114.8(3) . . ?
C4 C3 C2 120.4(4) . . ?
C14 C13 N1 114.9(3) . . ?
N1 C11 C12 114.9(3) . . ?
C8 C7 N1 115.7(3) . . ?
C5 C4 C3 120.4(4) . . ?
C4 C5 C6 120.0(4) . . ?
C5 C6 C1 121.0(4) . . ?
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 1.733(2) . ?
Mo1 O2 1.754(3) . ?
Mo1 O3 1.757(2) . ?
Mo1 S1 2.5357(14) . ?
Mo1 S2 2.5548(12) . ?
S2 C2 1.752(4) . ?
S1 C1 1.757(4) . ?
N2 C17 1.511(4) . ?
N2 C19 1.512(4) . ?
N2 C15 1.521(4) . ?
N2 C21 1.522(4) . ?
N1 C11 1.506(4) . ?
N1 C13 1.511(4) . ?
N1 C9 1.521(4) . ?
N1 C7 1.524(4) . ?
C21 C22 1.519(5) . ?
C1 C6 1.403(5) . ?
C1 C2 1.406(5) . ?
C2 C3 1.403(5) . ?
C19 C20 1.509(5) . ?
C9 C10 1.520(5) . ?
C17 C18 1.513(5) . ?
C15 C16 1.517(5) . ?
C3 C4 1.391(6) . ?
C13 C14 1.502(5) . ?
C11 C12 1.520(5) . ?
C7 C8 1.512(5) . ?
C4 C5 1.376(6) . ?
C5 C6 1.385(6) . ?
