#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008119.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_7008119
loop_
_publ_author_name
'Hogarth, Graeme'
'Richards, Idris'
_publ_section_title
;
 Regioselective and reversible carbon-nitrogen bond formation:
 synthesis, structure and reactivity of ureato-bridged complexes
 [Mo2(NAr)2(mu-X){mu-ArNC(O)NAr}(S2CNR2)2](Ar = Ph, p-tol; X = S, NAr;
 R = Me, Et, Pr).
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              760
_journal_page_last               773
_journal_paper_doi               10.1039/b417234p
_journal_year                    2005
_chemical_formula_sum            'C24 H34 Mo2 N4 S7'
_chemical_formula_weight         794.85
_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                 90.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.516(4)
_cell_length_b                   12.012(2)
_cell_length_c                   14.994(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     3334.9(11)
_computing_cell_refinement       'Nicolet R3'
_computing_data_collection       'Nicolet R3'
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Nicolet R3'
_diffrn_measurement_method       omega-2theta
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2980
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0539
_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)+(0.0358P)²+29.1176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                2104
_reflns_number_total             2886
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b417234p.txt
_cod_data_source_block           str712
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7008119
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
Mo Mo 0.44152(3) 0.21377(5) 0.19142(4) 0.0492(2) Uani 1 1 d . . .
S1 S 0.41760(12) 0.1335(2) 0.04096(15) 0.0852(8) Uani 1 1 d . . .
S2 S 0.31919(10) 0.12544(18) 0.18874(14) 0.0651(5) Uani 1 1 d . . .
S3 S 0.56492(10) 0.20000(18) 0.14997(13) 0.0624(5) Uani 1 1 d . . .
S4 S 0.5323(2) 0.0566(3) 0.1920(3) 0.0645(10) Uani 0.50 1 d P . .
N1 N 0.2847(3) 0.0536(5) 0.0231(4) 0.0657(17) Uani 1 1 d . . .
N2 N 0.4253(3) 0.3540(5) 0.1743(4) 0.0604(16) Uani 1 1 d . . .
C1 C 0.3329(4) 0.0989(6) 0.0761(5) 0.0568(17) Uani 1 1 d . . .
C2 C 0.3024(5) 0.0265(7) -0.0717(5) 0.069(2) Uani 1 1 d . . .
H2A H 0.2735 -0.0350 -0.0917 0.080 Uiso 1 1 d R . .
H2B H 0.3524 0.0061 -0.0767 0.080 Uiso 1 1 d R . .
C3 C 0.2889(7) 0.1264(9) -0.1305(7) 0.113(4) Uani 1 1 d . . .
H3A H 0.3000 0.1105 -0.1917 0.080 Uiso 1 1 d R . .
H3B H 0.2389 0.1459 -0.1253 0.080 Uiso 1 1 d R . .
H3C H 0.3182 0.1873 -0.1102 0.080 Uiso 1 1 d R . .
C4 C 0.2103(4) 0.0264(9) 0.0544(7) 0.089(3) Uani 1 1 d . . .
H4A H 0.1765 0.0296 0.0059 0.080 Uiso 1 1 d R . .
H4B H 0.1923 0.0747 0.1003 0.080 Uiso 1 1 d R . .
C5 C 0.2035(6) -0.0941(11) 0.0764(8) 0.134(5) Uani 1 1 d . . .
H5A H 0.1552 -0.1126 0.0943 0.080 Uiso 1 1 d R . .
H5B H 0.2191 -0.1450 0.0310 0.080 Uiso 1 1 d R . .
H5C H 0.2353 -0.0991 0.1269 0.080 Uiso 1 1 d R . .
C10 C 0.4250(4) 0.4695(6) 0.1645(5) 0.0516(16) Uani 1 1 d . . .
C11 C 0.3703(4) 0.5346(6) 0.1982(5) 0.064(2) Uani 1 1 d . . .
H11A H 0.3306 0.4989 0.2279 0.080 Uiso 1 1 d R . .
C12 C 0.3702(5) 0.6490(7) 0.1873(6) 0.072(2) Uani 1 1 d . . .
H12A H 0.3331 0.6934 0.2144 0.080 Uiso 1 1 d R . .
C13 C 0.4247(5) 0.7000(6) 0.1405(7) 0.078(2) Uani 1 1 d . . .
C14 C 0.4793(5) 0.6366(7) 0.1072(7) 0.098(3) Uani 1 1 d . . .
H14A H 0.5181 0.6717 0.0756 0.080 Uiso 1 1 d R . .
C15 C 0.4804(5) 0.5219(7) 0.1181(7) 0.082(3) Uani 1 1 d . . .
H15A H 0.5187 0.4783 0.0929 0.080 Uiso 1 1 d R . .
C16 C 0.4248(7) 0.8248(7) 0.1265(9) 0.121(4) Uani 1 1 d . . .
H16A H 0.4662 0.8465 0.0922 0.080 Uiso 1 1 d R . .
H16B H 0.3816 0.8441 0.0946 0.080 Uiso 1 1 d R . .
H16C H 0.4255 0.8626 0.1829 0.080 Uiso 1 1 d 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'
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
N2 Mo S3 101.3(2) . . ?
N2 Mo S3 101.9(2) . 2_655 ?
S3 Mo S3 107.83(6) . 2_655 ?
N2 Mo S1 102.2(2) . . ?
S3 Mo S1 84.57(8) . . ?
S3 Mo S1 149.98(8) 2_655 . ?
N2 Mo S2 104.7(2) . . ?
S3 Mo S2 146.92(8) . . ?
S3 Mo S2 86.52(7) 2_655 . ?
S1 Mo S2 70.26(7) . . ?
N2 Mo S4 147.5(2) . . ?
S3 Mo S4 46.28(10) . . ?
S3 Mo S4 88.84(11) 2_655 . ?
S1 Mo S4 80.26(12) . . ?
S2 Mo S4 106.57(10) . . ?
N2 Mo S4 146.4(2) . 2_655 ?
S3 Mo S4 87.00(10) . 2_655 ?
S3 Mo S4 45.11(10) 2_655 2_655 ?
S1 Mo S4 110.96(12) . 2_655 ?
S2 Mo S4 82.59(11) . 2_655 ?
S4 Mo S4 48.46(17) . 2_655 ?
N2 Mo Mo 103.2(2) . 2_655 ?
S3 Mo Mo 54.41(5) . 2_655 ?
S3 Mo Mo 54.00(5) 2_655 2_655 ?
S1 Mo Mo 135.02(7) . 2_655 ?
S2 Mo Mo 135.46(6) . 2_655 ?
S4 Mo Mo 58.80(10) . 2_655 ?
S4 Mo Mo 55.69(9) 2_655 2_655 ?
C1 S1 Mo 88.6(3) . . ?
C1 S2 Mo 87.7(2) . . ?
S4 S3 Mo 71.04(13) . . ?
S4 S3 Mo 73.78(14) . 2_655 ?
Mo S3 Mo 71.59(6) . 2_655 ?
S3 S4 S4 116.50(13) . 2_655 ?
S3 S4 Mo 62.68(13) . . ?
S4 S4 Mo 67.99(14) 2_655 . ?
S3 S4 Mo 61.10(12) . 2_655 ?
S4 S4 Mo 63.54(15) 2_655 2_655 ?
Mo S4 Mo 65.51(10) . 2_655 ?
C1 N1 C4 121.8(7) . . ?
C1 N1 C2 121.0(6) . . ?
C4 N1 C2 117.2(6) . . ?
C10 N2 Mo 169.9(5) . . ?
N1 C1 S1 122.6(6) . . ?
N1 C1 S2 124.3(6) . . ?
S1 C1 S2 113.1(4) . . ?
N1 C2 C3 110.3(7) . . ?
C5 C4 N1 111.1(8) . . ?
C11 C10 C15 118.1(6) . . ?
C11 C10 N2 121.9(6) . . ?
C15 C10 N2 120.0(6) . . ?
C10 C11 C12 121.4(7) . . ?
C13 C12 C11 120.1(7) . . ?
C14 C13 C12 119.0(7) . . ?
C14 C13 C16 120.1(8) . . ?
C12 C13 C16 120.9(8) . . ?
C13 C14 C15 121.6(8) . . ?
C14 C15 C10 119.8(7) . . ?
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
Mo N2 1.731(6) . ?
Mo S3 2.3750(19) . ?
Mo S3 2.387(2) 2_655 ?
Mo S1 2.492(2) . ?
Mo S2 2.502(2) . ?
Mo S4 2.528(4) . ?
Mo S4 2.618(4) 2_655 ?
Mo Mo 2.7854(15) 2_655 ?
S1 C1 1.707(7) . ?
S2 C1 1.738(8) . ?
S3 S4 1.932(4) . ?
S3 Mo 2.387(2) 2_655 ?
S4 S4 2.114(8) 2_655 ?
S4 Mo 2.618(4) 2_655 ?
N1 C1 1.312(9) . ?
N1 C4 1.492(10) . ?
N1 C2 1.496(10) . ?
N2 C10 1.395(9) . ?
C2 C3 1.509(12) . ?
C4 C5 1.490(15) . ?
C10 C11 1.376(10) . ?
C10 C15 1.392(10) . ?
C11 C12 1.385(10) . ?
C12 C13 1.374(11) . ?
C13 C14 1.361(12) . ?
C13 C16 1.514(11) . ?
C14 C15 1.388(11) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Mo S1 C1 -97.6(3) . . . . ?
S3 Mo S1 C1 162.0(3) . . . . ?
S3 Mo S1 C1 45.3(3) 2_655 . . . ?
S2 Mo S1 C1 3.8(3) . . . . ?
S4 Mo S1 C1 115.5(3) . . . . ?
S4 Mo S1 C1 77.3(3) 2_655 . . . ?
Mo Mo S1 C1 139.2(2) 2_655 . . . ?
N2 Mo S2 C1 94.2(3) . . . . ?
S3 Mo S2 C1 -46.5(3) . . . . ?
S3 Mo S2 C1 -164.4(2) 2_655 . . . ?
S1 Mo S2 C1 -3.8(2) . . . . ?
S4 Mo S2 C1 -76.7(3) . . . . ?
S4 Mo S2 C1 -119.2(3) 2_655 . . . ?
Mo Mo S2 C1 -138.7(2) 2_655 . . . ?
N2 Mo S3 S4 176.9(3) . . . . ?
S3 Mo S3 S4 70.30(17) 2_655 . . . ?
S1 Mo S3 S4 -81.71(16) . . . . ?
S2 Mo S3 S4 -41.8(2) . . . . ?
S4 Mo S3 S4 29.7(2) 2_655 . . . ?
Mo Mo S3 S4 78.64(15) 2_655 . . . ?
N2 Mo S3 Mo 98.2(2) . . . 2_655 ?
S3 Mo S3 Mo -8.34(11) 2_655 . . 2_655 ?
S1 Mo S3 Mo -160.35(8) . . . 2_655 ?
S2 Mo S3 Mo -120.47(12) . . . 2_655 ?
S4 Mo S3 Mo -78.64(15) . . . 2_655 ?
S4 Mo S3 Mo -48.95(10) 2_655 . . 2_655 ?
Mo S3 S4 S4 -43.2(3) . . . 2_655 ?
Mo S3 S4 S4 32.4(3) 2_655 . . 2_655 ?
Mo S3 S4 Mo 75.65(7) 2_655 . . . ?
Mo S3 S4 Mo -75.65(7) . . . 2_655 ?
N2 Mo S4 S3 -5.7(5) . . . . ?
S3 Mo S4 S3 -116.30(13) 2_655 . . . ?
S1 Mo S4 S3 91.79(13) . . . . ?
S2 Mo S4 S3 157.68(11) . . . . ?
S4 Mo S4 S3 -138.6(3) 2_655 . . . ?
Mo Mo S4 S3 -68.76(11) 2_655 . . . ?
N2 Mo S4 S4 132.9(4) . . . 2_655 ?
S3 Mo S4 S4 138.6(3) . . . 2_655 ?
S3 Mo S4 S4 22.34(18) 2_655 . . 2_655 ?
S1 Mo S4 S4 -129.57(19) . . . 2_655 ?
S2 Mo S4 S4 -63.7(2) . . . 2_655 ?
Mo Mo S4 S4 69.88(19) 2_655 . . 2_655 ?
N2 Mo S4 Mo 63.0(4) . . . 2_655 ?
S3 Mo S4 Mo 68.76(11) . . . 2_655 ?
S3 Mo S4 Mo -47.55(8) 2_655 . . 2_655 ?
S1 Mo S4 Mo 160.55(9) . . . 2_655 ?
S2 Mo S4 Mo -133.57(7) . . . 2_655 ?
S4 Mo S4 Mo -69.88(19) 2_655 . . 2_655 ?
S3 Mo N2 C10 -31(3) . . . . ?
S3 Mo N2 C10 80(3) 2_655 . . . ?
S1 Mo N2 C10 -118(3) . . . . ?
S2 Mo N2 C10 170(3) . . . . ?
S4 Mo N2 C10 -27(3) . . . . ?
S4 Mo N2 C10 71(3) 2_655 . . . ?
Mo Mo N2 C10 25(3) 2_655 . . . ?
C4 N1 C1 S1 -178.5(7) . . . . ?
C2 N1 C1 S1 1.8(10) . . . . ?
C4 N1 C1 S2 3.8(11) . . . . ?
C2 N1 C1 S2 -175.9(6) . . . . ?
Mo S1 C1 N1 176.4(6) . . . . ?
Mo S1 C1 S2 -5.6(4) . . . . ?
Mo S2 C1 N1 -176.5(6) . . . . ?
Mo S2 C1 S1 5.6(4) . . . . ?
C1 N1 C2 C3 -86.9(9) . . . . ?
C4 N1 C2 C3 93.3(9) . . . . ?
C1 N1 C4 C5 -99.9(10) . . . . ?
C2 N1 C4 C5 79.8(10) . . . . ?
Mo N2 C10 C11 -135(3) . . . . ?
Mo N2 C10 C15 46(4) . . . . ?
C15 C10 C11 C12 -0.6(13) . . . . ?
N2 C10 C11 C12 -179.3(8) . . . . ?
C10 C11 C12 C13 1.3(14) . . . . ?
C11 C12 C13 C14 -1.6(15) . . . . ?
C11 C12 C13 C16 179.0(10) . . . . ?
C12 C13 C14 C15 1.1(18) . . . . ?
C16 C13 C14 C15 -179.4(11) . . . . ?
C13 C14 C15 C10 -0.4(18) . . . . ?
C11 C10 C15 C14 0.2(14) . . . . ?
N2 C10 C15 C14 178.9(9) . . . . ?
