#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/38/4323817.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_4323817
loop_
_publ_author_name
'Runtong Wang'
'Mark S. Mashuta'
'John F. Richardson'
'Mark E. Noble'
_publ_contact_author
;
Mark E. Noble
Department of Chemistry and Center for Chemical Catalysis
University of Louisville
Louisville
KY 40292
USA
;
_publ_contact_author_email
;
MENOBL01@ulkyvm.louisville.edu
JFRICH01@ulkyvm.louisville.edu
msmash01@homer.louisville.edu
;
_publ_contact_author_fax         (502)852-8149
_publ_contact_author_phone       (502)852-7296
_publ_section_title
;
 Oxidation at a Dimolybdenum(V) Sulfur Bridge. Formation of SO and SO2
 Bridges. Facile Extrusion of SO from the SO2 Bridge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3022
_journal_page_last               3030
_journal_paper_doi               10.1021/ic951518k
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         'C31 H42 N2 Mo2 O8 P2 S6 '
_chemical_formula_sum            'C31 H42 Mo2 N2 O8 P2 S6'
_chemical_formula_weight         1018.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Fri Nov 10 07:00:44 1995'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 100.79(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.591(9)
_cell_length_b                   25.34(1)
_cell_length_c                   14.048(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      30.0
_cell_volume                     4403(4)
_computing_cell_refinement       'Enraf Nonius Diffractometer Control 1988'
_computing_data_collection       'Enraf Nonius Diffractometer Control 1988'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_orient_matrix_UB_11      -0.07592
_diffrn_orient_matrix_UB_12      0.01342
_diffrn_orient_matrix_UB_13      -0.01354
_diffrn_orient_matrix_UB_21      -0.02327
_diffrn_orient_matrix_UB_22      -0.03053
_diffrn_orient_matrix_UB_23      0.03611
_diffrn_orient_matrix_UB_31      0.01474
_diffrn_orient_matrix_UB_32      0.02104
_diffrn_orient_matrix_UB_33      0.06134
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10407
_diffrn_reflns_theta_max         27.51
_diffrn_standards_decay_%        -0.39
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             2072.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.83
_refine_ls_extinction_coef       9.8E-8
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.28
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6411
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.043
_refine_ls_shift/esd_max         0.051
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/σ²(F)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.043
_reflns_number_observed          6411
_reflns_number_total             10090
_reflns_observed_criterion       3.00
_cod_data_source_file            ic951518k_2.cif
_cod_data_source_block           COMPOUND#4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/\s^2^(F)' 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^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4403(3)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C31 H42 N2 Mo2 O8 P2 S6 '
_cod_database_code               4323817
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
Mo(1) 0.22585(3) 0.14170(2) -0.13581(3) 0.0498(1) Uij ? ?
Mo(2) 0.19482(3) 0.03015(2) -0.19299(3) 0.0492(1) Uij ? ?
S(1) 0.21053(9) 0.10539(5) -0.29965(9) 0.0504(4) Uij ? ?
S(2) 0.2058(1) 0.06706(6) -0.03253(9) 0.0573(4) Uij ? ?
S(3) 0.2786(1) 0.18871(7) 0.0227(1) 0.0843(6) Uij ? ?
S(4) 0.2985(1) 0.22628(6) -0.1902(1) 0.0686(5) Uij ? ?
S(5) 0.2140(1) -0.05472(6) -0.1005(1) 0.0706(5) Uij ? ?
S(6) 0.2267(1) -0.03346(7) -0.3214(1) 0.0827(6) Uij ? ?
P(1) 0.3218(1) 0.24903(7) -0.0519(1) 0.0737(5) Uij ? ?
P(2) 0.2376(1) -0.08988(6) -0.2218(1) 0.0794(6) Uij ? ?
O(1) 0.3941(2) 0.1156(1) -0.1104(2) 0.055(1) Uij ? ?
O(2) 0.3704(2) 0.0325(1) -0.1567(2) 0.056(1) Uij ? ?
O(3) 0.2617(3) 0.3020(2) -0.0368(3) 0.082(1) Uij ? ?
O(4) 0.4389(3) 0.2694(2) -0.0112(3) 0.103(2) Uij ? ?
O(5) 0.1599(4) -0.1375(2) -0.2532(4) 0.108(2) Uij ? ?
O(6) 0.3467(3) -0.1219(2) -0.2105(3) 0.099(2) Uij ? ?
O(7) 0.3033(3) 0.0526(1) 0.0372(2) 0.070(1) Uij ? ?
O(8) 0.1054(3) 0.0662(2) 0.0065(3) 0.078(1) Uij ? ?
N(1) 0.0888(3) 0.1558(2) -0.1567(3) 0.053(1) Uij ? ?
N(2) 0.0557(3) 0.0312(2) -0.2248(3) 0.053(1) Uij ? ?
C(1) -0.0223(4) 0.1624(2) -0.1745(3) 0.050(2) Uij ? ?
C(2) -0.0713(4) 0.1896(2) -0.2547(4) 0.073(2) Uij ? ?
C(3) -0.1815(5) 0.1958(3) -0.2749(4) 0.080(2) Uij ? ?
C(4) -0.2452(4) 0.1756(2) -0.2145(4) 0.065(2) Uij ? ?
C(5) -0.1954(4) 0.1486(2) -0.1347(4) 0.072(2) Uij ? ?
C(6) -0.0854(4) 0.1415(2) -0.1131(4) 0.064(2) Uij ? ?
C(7) -0.3662(5) 0.1822(3) -0.2400(5) 0.105(3) Uij ? ?
C(8) -0.0549(4) 0.0291(2) -0.2581(3) 0.047(1) Uij ? ?
C(9) -0.0969(4) 0.0450(2) -0.3504(4) 0.069(2) Uij ? ?
C(10) -0.2072(5) 0.0410(3) -0.3846(4) 0.077(2) Uij ? ?
C(11) -0.2751(4) 0.0208(2) -0.3270(4) 0.068(2) Uij ? ?
C(12) -0.2318(4) 0.0045(2) -0.2354(4) 0.070(2) Uij ? ?
C(13) -0.1218(4) 0.0082(2) -0.1992(4) 0.060(2) Uij ? ?
C(14) -0.3958(5) 0.0167(3) -0.3670(5) 0.109(3) Uij ? ?
C(15) 0.4292(4) 0.0698(2) -0.1210(4) 0.052(2) Uij ? ?
C(16) 0.5471(4) 0.0597(2) -0.0911(4) 0.078(2) Uij ? ?
C(17) 0.1453(5) 0.3064(3) -0.0639(5) 0.097(3) Uij ? ?
C(18) 0.1128(5) 0.3579(3) -0.0281(5) 0.098(3) Uij ? ?
C(19) 0.5307(7) 0.2360(4) -0.0104(7) 0.168(5) Uij ? ?
C(20) 0.6129(7) 0.2435(4) 0.0636(8) 0.179(5) Uij ? ?
C(21) 0.0433(7) -0.1314(3) -0.2690(8) 0.144(4) Uij ? ?
C(22) -0.0007(8) -0.1661(5) -0.1942(9) 0.186(5) Uij ? ?
C(23) 0.4500(6) -0.0964(3) -0.1745(6) 0.115(3) Uij ? ?
C(24) 0.5310(6) -0.1167(4) -0.2224(6) 0.136(4) Uij ? ?
C(25) 0.3408(4) 0.1057(2) -0.3411(4) 0.063(2) Uij ? ?
C(26) 0.3281(4) 0.1320(2) -0.4382(4) 0.056(2) Uij ? ?
C(27) 0.3581(5) 0.1829(3) -0.4467(5) 0.081(2) Uij ? ?
C(28) 0.3444(6) 0.2064(3) -0.5395(7) 0.108(3) Uij ? ?
C(29) 0.3011(7) 0.1777(4) -0.6190(6) 0.114(4) Uij ? ?
C(30) 0.2716(6) 0.1280(4) -0.6098(5) 0.106(3) Uij ? ?
C(31) 0.2848(5) 0.1051(3) -0.5202(5) 0.081(2) Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo 0 8 -1.683 0.686 'International Tables'
S 0 24 0.125 0.123 'International Tables'
P 0 8 0.102 0.094 'International Tables'
O 0 32 0.011 0.006 'International Tables'
N 0 8 0.006 0.003 'International Tables'
C 0 124 0.003 0.002 'International Tables'
H 0 176 0.000 0.000 'International Tables'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mo(2) Mo(1) S(1) 53.23(3) ? ? ? yes
Mo(2) Mo(1) S(2) 52.48(4) ? ? ? yes
Mo(2) Mo(1) S(3) 134.30(4) ? ? ? yes
Mo(2) Mo(1) S(4) 140.85(4) ? ? ? yes
Mo(2) Mo(1) O(1) 80.10(9) ? ? ? yes
Mo(2) Mo(1) N(1) 94.3(1) ? ? ? yes
S(1) Mo(1) S(2) 105.70(5) ? ? ? yes
S(1) Mo(1) S(3) 167.08(5) ? ? ? yes
S(1) Mo(1) S(4) 90.17(5) ? ? ? yes
S(1) Mo(1) O(1) 86.75(9) ? ? ? yes
S(1) Mo(1) N(1) 91.0(1) ? ? ? yes
S(2) Mo(1) S(3) 83.01(5) ? ? ? yes
S(2) Mo(1) S(4) 159.16(5) ? ? ? yes
S(2) Mo(1) O(1) 82.63(9) ? ? ? yes
S(2) Mo(1) N(1) 92.9(1) ? ? ? yes
S(3) Mo(1) S(4) 79.28(5) ? ? ? yes
S(3) Mo(1) O(1) 84.91(10) ? ? ? yes
S(3) Mo(1) N(1) 98.2(1) ? ? ? yes
S(4) Mo(1) O(1) 84.93(9) ? ? ? yes
S(4) Mo(1) N(1) 100.4(1) ? ? ? yes
O(1) Mo(1) N(1) 174.2(2) ? ? ? yes
Mo(1) Mo(2) S(1) 53.07(3) ? ? ? yes
Mo(1) Mo(2) S(2) 52.71(3) ? ? ? yes
Mo(1) Mo(2) S(5) 133.57(4) ? ? ? yes
Mo(1) Mo(2) S(6) 141.48(4) ? ? ? yes
Mo(1) Mo(2) O(2) 80.42(9) ? ? ? yes
Mo(1) Mo(2) N(2) 97.5(1) ? ? ? yes
S(1) Mo(2) S(2) 105.76(5) ? ? ? yes
S(1) Mo(2) S(5) 166.85(5) ? ? ? yes
S(1) Mo(2) S(6) 91.04(5) ? ? ? yes
S(1) Mo(2) O(2) 85.89(9) ? ? ? yes
S(1) Mo(2) N(2) 91.3(1) ? ? ? yes
S(2) Mo(2) S(5) 82.24(5) ? ? ? yes
S(2) Mo(2) S(6) 158.37(5) ? ? ? yes
S(2) Mo(2) O(2) 83.87(10) ? ? ? yes
S(2) Mo(2) N(2) 96.5(1) ? ? ? yes
S(5) Mo(2) S(6) 78.93(6) ? ? ? yes
S(5) Mo(2) O(2) 84.60(10) ? ? ? yes
S(5) Mo(2) N(2) 98.2(1) ? ? ? yes
S(6) Mo(2) O(2) 83.86(10) ? ? ? yes
S(6) Mo(2) N(2) 96.7(1) ? ? ? yes
O(2) Mo(2) N(2) 177.2(2) ? ? ? yes
Mo(1) S(1) Mo(2) 73.70(4) ? ? ? yes
Mo(1) S(1) C(25) 112.2(2) ? ? ? yes
Mo(2) S(1) C(25) 111.9(2) ? ? ? yes
Mo(1) S(2) Mo(2) 74.80(4) ? ? ? yes
Mo(1) S(2) O(7) 115.3(2) ? ? ? yes
Mo(1) S(2) O(8) 115.3(2) ? ? ? yes
Mo(2) S(2) O(7) 114.8(2) ? ? ? yes
Mo(2) S(2) O(8) 116.1(2) ? ? ? yes
O(7) S(2) O(8) 114.8(2) ? ? ? yes
Mo(1) S(3) P(1) 87.09(7) ? ? ? yes
Mo(1) S(4) P(1) 86.83(7) ? ? ? yes
Mo(2) S(5) P(2) 87.46(7) ? ? ? yes
Mo(2) S(6) P(2) 87.42(8) ? ? ? yes
S(3) P(1) S(4) 106.70(9) ? ? ? yes
S(3) P(1) O(3) 113.6(2) ? ? ? yes
S(3) P(1) O(4) 113.1(2) ? ? ? yes
S(4) P(1) O(3) 112.9(2) ? ? ? yes
S(4) P(1) O(4) 114.0(2) ? ? ? yes
O(3) P(1) O(4) 96.5(2) ? ? ? yes
S(5) P(2) S(6) 106.18(10) ? ? ? yes
S(5) P(2) O(5) 113.6(2) ? ? ? yes
S(5) P(2) O(6) 114.2(2) ? ? ? yes
S(6) P(2) O(5) 113.5(2) ? ? ? yes
S(6) P(2) O(6) 112.7(2) ? ? ? yes
O(5) P(2) O(6) 96.8(2) ? ? ? yes
Mo(1) O(1) C(15) 127.6(3) ? ? ? yes
Mo(2) O(2) C(15) 128.0(3) ? ? ? yes
P(1) O(3) C(17) 121.3(4) ? ? ? yes
P(1) O(4) C(19) 120.8(5) ? ? ? yes
P(2) O(5) C(21) 121.4(4) ? ? ? yes
P(2) O(6) C(23) 120.8(4) ? ? ? yes
Mo(1) N(1) C(1) 175.1(4) ? ? ? yes
Mo(2) N(2) C(8) 174.4(4) ? ? ? yes
N(1) C(1) C(2) 119.8(4) ? ? ? yes
N(1) C(1) C(6) 121.3(4) ? ? ? yes
C(2) C(1) C(6) 118.9(5) ? ? ? yes
C(1) C(2) C(3) 120.9(5) ? ? ? yes
C(2) C(3) C(4) 120.9(5) ? ? ? yes
C(3) C(4) C(5) 117.7(5) ? ? ? yes
C(3) C(4) C(7) 119.5(5) ? ? ? yes
C(5) C(4) C(7) 122.7(5) ? ? ? yes
C(4) C(5) C(6) 122.5(5) ? ? ? yes
C(1) C(6) C(5) 119.0(5) ? ? ? yes
N(2) C(8) C(9) 119.7(4) ? ? ? yes
N(2) C(8) C(13) 119.8(4) ? ? ? yes
C(9) C(8) C(13) 120.5(4) ? ? ? yes
C(8) C(9) C(10) 119.5(5) ? ? ? yes
C(9) C(10) C(11) 120.9(5) ? ? ? yes
C(10) C(11) C(12) 118.9(5) ? ? ? yes
C(10) C(11) C(14) 119.6(6) ? ? ? yes
C(12) C(11) C(14) 121.5(5) ? ? ? yes
C(11) C(12) C(13) 121.4(5) ? ? ? yes
C(8) C(13) C(12) 118.8(5) ? ? ? yes
O(1) C(15) O(2) 123.4(4) ? ? ? yes
O(1) C(15) C(16) 118.6(5) ? ? ? yes
O(2) C(15) C(16) 117.9(5) ? ? ? yes
O(3) C(17) C(18) 108.0(5) ? ? ? yes
O(4) C(19) C(20) 115.5(9) ? ? ? yes
O(5) C(21) C(22) 108.3(8) ? ? ? yes
O(6) C(23) C(24) 110.5(6) ? ? ? yes
S(1) C(25) C(26) 109.8(3) ? ? ? yes
C(25) C(26) C(27) 121.4(6) ? ? ? yes
C(25) C(26) C(31) 120.3(5) ? ? ? yes
C(27) C(26) C(31) 118.3(6) ? ? ? yes
C(26) C(27) C(28) 119.6(7) ? ? ? yes
C(27) C(28) C(29) 119.6(7) ? ? ? yes
C(28) C(29) C(30) 120.3(8) ? ? ? yes
C(29) C(30) C(31) 120.3(8) ? ? ? yes
C(26) C(31) C(30) 121.8(7) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo(1) Mo(2) 2.9440(6) ? ? yes
Mo(1) S(1) 2.452(1) ? ? yes
Mo(1) S(2) 2.427(1) ? ? yes
Mo(1) S(3) 2.502(2) ? ? yes
Mo(1) S(4) 2.505(2) ? ? yes
Mo(1) O(1) 2.184(3) ? ? yes
Mo(1) N(1) 1.733(4) ? ? yes
Mo(2) S(1) 2.457(1) ? ? yes
Mo(2) S(2) 2.420(1) ? ? yes
Mo(2) S(5) 2.502(2) ? ? yes
Mo(2) S(6) 2.507(2) ? ? yes
Mo(2) O(2) 2.175(3) ? ? yes
Mo(2) N(2) 1.725(4) ? ? yes
S(1) C(25) 1.840(5) ? ? yes
S(2) O(7) 1.467(3) ? ? yes
S(2) O(8) 1.469(4) ? ? yes
S(3) P(1) 1.987(2) ? ? yes
S(4) P(1) 1.995(2) ? ? yes
S(5) P(2) 1.993(2) ? ? yes
S(6) P(2) 1.989(2) ? ? yes
P(1) O(3) 1.576(4) ? ? yes
P(1) O(4) 1.565(4) ? ? yes
P(2) O(5) 1.564(4) ? ? yes
P(2) O(6) 1.578(4) ? ? yes
O(1) C(15) 1.262(6) ? ? yes
O(2) C(15) 1.245(6) ? ? yes
O(3) C(17) 1.448(6) ? ? yes
O(4) C(19) 1.432(9) ? ? yes
O(5) C(21) 1.451(8) ? ? yes
O(6) C(23) 1.455(7) ? ? yes
N(1) C(1) 1.384(5) ? ? yes
N(2) C(8) 1.385(5) ? ? yes
C(1) C(2) 1.367(6) ? ? yes
C(1) C(6) 1.383(6) ? ? yes
C(2) C(3) 1.372(7) ? ? yes
C(3) C(4) 1.371(7) ? ? yes
C(4) C(5) 1.363(7) ? ? yes
C(4) C(7) 1.508(7) ? ? yes
C(5) C(6) 1.374(7) ? ? yes
C(8) C(9) 1.366(6) ? ? yes
C(8) C(13) 1.390(6) ? ? yes
C(9) C(10) 1.386(7) ? ? yes
C(10) C(11) 1.380(7) ? ? yes
C(11) C(12) 1.365(7) ? ? yes
C(11) C(14) 1.522(7) ? ? yes
C(12) C(13) 1.386(7) ? ? yes
C(15) C(16) 1.488(6) ? ? yes
C(17) C(18) 1.482(9) ? ? yes
C(19) C(20) 1.34(1) ? ? yes
C(21) C(22) 1.55(1) ? ? yes
C(23) C(24) 1.419(9) ? ? yes
C(25) C(26) 1.501(7) ? ? yes
C(26) C(27) 1.357(7) ? ? yes
C(26) C(31) 1.360(7) ? ? yes
C(27) C(28) 1.414(9) ? ? yes
C(28) C(29) 1.36(1) ? ? yes
C(29) C(30) 1.33(1) ? ? yes
C(30) C(31) 1.368(9) ? ? yes
