#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/35/7003560.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_7003560
loop_
_publ_author_name
'Chaves, Sílvia'
'Gil, Marco'
'Canário, Sónia'
'Jelic, Ratomir'
'Romão, Maria João'
'Trincão, José'
'Herdtweck, Eberhardt'
'Sousa, Joana'
'Diniz, Carmen'
'Fresco, Paula'
'Santos, M. Amélia'
_publ_section_title
;
 Biologically relevant O,S-donor compounds. Synthesis, molybdenum
 complexation and xanthine oxidase inhibition
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              1773
_journal_page_last               1782
_journal_paper_doi               10.1039/b717172b
_journal_year                    2008
_chemical_formula_moiety         'C12 H11 Mo O6.50 S2'
_chemical_formula_sum            'C12 H11 Mo O6.5 S2'
_chemical_formula_weight         419.27
_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                103.8730(10)
_cell_angle_beta                 106.2010(10)
_cell_angle_gamma                90.0260(10)
_cell_formula_units_Z            4
_cell_length_a                   9.8133(2)
_cell_length_b                   10.9684(2)
_cell_length_c                   14.5117(3)
_cell_measurement_reflns_used    9209
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      2.72
_cell_volume                     1452.40(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows/Platon'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            81371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.9761
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-Bruker Nonius area detector scaling and absorption correction - V2.10'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.376
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5108
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0539P)²+4.2233P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                4450
_reflns_number_total             5108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717172b.txt
_cod_data_source_block           a
_cod_original_sg_symbol_Hall     'P -1'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C12 H11 Mo O6.50 S2'
_cod_database_code               7003560
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 0.11473(3) 0.42933(3) 0.28806(2) 0.01634(10) Uani 1 1 d . . .
S1 S -0.03116(10) 0.60071(9) 0.23897(7) 0.0199(2) Uani 1 1 d . . .
S2 S 0.31955(10) 0.29525(9) 0.32241(7) 0.0194(2) Uani 1 1 d . . .
O11 O 0.0253(3) 0.2886(3) 0.2166(2) 0.0253(6) Uani 1 1 d . . .
O12 O 0.0452(3) 0.4603(3) 0.3866(2) 0.0252(6) Uani 1 1 d . . .
O18 O 0.1813(3) 0.4576(2) 0.16679(18) 0.0177(5) Uani 1 1 d . . .
O28 O 0.2870(3) 0.5619(2) 0.36562(18) 0.0171(5) Uani 1 1 d . . .
O24 O 0.6666(3) 0.6016(2) 0.42758(18) 0.0175(5) Uani 1 1 d . . .
014 O 0.1657(3) 0.6699(2) 0.01284(18) 0.0187(6) Uani 1 1 d . . .
C11 C 0.0408(4) 0.6311(3) 0.1520(3) 0.0167(7) Uani 1 1 d . . .
C12 C 0.0054(4) 0.7314(4) 0.1062(3) 0.0207(8) Uani 1 1 d . . .
H12 H -0.0604 0.7866 0.1234 0.025 Uiso 1 1 calc R . .
C13 C 0.0673(4) 0.7464(4) 0.0374(3) 0.0213(8) Uani 1 1 d . . .
H13 H 0.0417 0.8112 0.0062 0.026 Uiso 1 1 calc R . .
C16 C 0.1467(4) 0.5518(3) 0.1264(3) 0.0152(7) Uani 1 1 d . . .
C15 C 0.2106(4) 0.5781(3) 0.0588(3) 0.0162(7) Uani 1 1 d . . .
C17 C 0.3310(4) 0.5141(4) 0.0305(3) 0.0241(9) Uani 1 1 d . . .
H17A H 0.2969 0.4588 -0.0346 0.036 Uiso 1 1 calc R . .
H17B H 0.3736 0.4661 0.0771 0.036 Uiso 1 1 calc R . .
H17C H 0.4005 0.5758 0.0307 0.036 Uiso 1 1 calc R . .
C21 C 0.4565(4) 0.4086(3) 0.3615(3) 0.0170(8) Uani 1 1 d . . .
C22 C 0.6017(4) 0.3842(4) 0.3795(3) 0.0190(8) Uani 1 1 d . . .
H22 H 0.6284 0.3018 0.3697 0.023 Uiso 1 1 calc R . .
C23 C 0.7008(4) 0.4812(4) 0.4108(3) 0.0197(8) Uani 1 1 d . . .
H23 H 0.7961 0.4646 0.4213 0.024 Uiso 1 1 calc R . .
C25 C 0.5286(4) 0.6304(3) 0.4118(3) 0.0168(8) Uani 1 1 d . . .
C26 C 0.4207(4) 0.5352(3) 0.3785(3) 0.0152(7) Uani 1 1 d . . .
C27 C 0.5058(4) 0.7659(3) 0.4365(3) 0.0203(8) Uani 1 1 d . . .
H27A H 0.4702 0.7858 0.4932 0.030 Uiso 1 1 calc R . .
H27B H 0.4380 0.7860 0.3812 0.030 Uiso 1 1 calc R . .
H27C H 0.5943 0.8141 0.4512 0.030 Uiso 1 1 calc R . .
Mo2 Mo 0.67047(3) -0.15010(3) 0.21585(2) 0.01580(10) Uani 1 1 d . . .
S4 S 0.65863(10) 0.03042(8) 0.37987(7) 0.0195(2) Uani 1 1 d . . .
S3 S 0.41237(10) -0.12763(9) 0.16455(8) 0.0230(2) Uani 1 1 d . . .
O22 O 0.6285(3) -0.2655(2) 0.2668(2) 0.0227(6) Uani 1 1 d . . .
O21 O 0.6991(3) -0.2317(2) 0.10771(19) 0.0228(6) Uani 1 1 d . . .
O44 O 1.1182(3) 0.1560(2) 0.45876(19) 0.0223(6) Uani 1 1 d . . .
O34 O 0.4218(3) 0.2524(3) 0.10705(19) 0.0246(6) Uani 1 1 d . . .
O48 O 0.8706(3) -0.0893(2) 0.28659(18) 0.0167(5) Uani 1 1 d . . .
O38 O 0.6600(3) 0.0194(2) 0.16770(19) 0.0195(6) Uani 1 1 d . . .
C31 C 0.4098(4) 0.0140(4) 0.1337(3) 0.0203(8) Uani 1 1 d . . .
C32 C 0.2850(4) 0.0738(4) 0.1019(3) 0.0244(9) Uani 1 1 d . . .
H32 H 0.1961 0.0330 0.0891 0.029 Uiso 1 1 calc R . .
C33 C 0.2962(5) 0.1912(4) 0.0902(3) 0.0285(10) Uani 1 1 d . . .
H33 H 0.2136 0.2309 0.0696 0.034 Uiso 1 1 calc R . .
C35 C 0.5448(4) 0.1968(4) 0.1337(3) 0.0220(8) Uani 1 1 d . . .
C36 C 0.5421(4) 0.0755(4) 0.1445(3) 0.0198(8) Uani 1 1 d . . .
C37 C 0.6738(5) 0.2763(4) 0.1496(3) 0.0287(10) Uani 1 1 d . . .
H37A H 0.7045 0.2567 0.0908 0.043 Uiso 1 1 calc R . .
H37B H 0.7475 0.2608 0.2040 0.043 Uiso 1 1 calc R . .
H37C H 0.6536 0.3633 0.1645 0.043 Uiso 1 1 calc R . .
C41 C 0.8304(4) 0.0830(3) 0.4112(3) 0.0169(8) Uani 1 1 d . . .
C42 C 0.8947(4) 0.1919(3) 0.4877(3) 0.0197(8) Uani 1 1 d . . .
H42 H 0.8404 0.2410 0.5236 0.024 Uiso 1 1 calc R . .
C43 C 1.0337(5) 0.2230(4) 0.5076(3) 0.0251(9) Uani 1 1 d . . .
H43 H 1.0738 0.2944 0.5577 0.030 Uiso 1 1 calc R . .
C45 C 1.0630(4) 0.0517(3) 0.3847(3) 0.0186(8) Uani 1 1 d . . .
C46 C 0.9220(4) 0.0142(3) 0.3595(2) 0.0145(7) Uani 1 1 d . . .
C47 C 1.1692(4) -0.0133(4) 0.3387(3) 0.0239(9) Uani 1 1 d . . .
H47A H 1.1639 0.0112 0.2787 0.036 Uiso 1 1 calc R . .
H47B H 1.1495 -0.1027 0.3239 0.036 Uiso 1 1 calc R . .
H47C H 1.2628 0.0096 0.3838 0.036 Uiso 1 1 calc R . .
O5 O 0.9300(3) 0.0405(3) 0.1105(2) 0.0278(6) Uani 1 1 d D . .
H51 H 0.964(5) 0.121(3) 0.153(3) 0.043(14) Uiso 1 1 d D . .
H52 H 0.840(4) 0.021(6) 0.117(5) 0.08(2) Uiso 1 1 d D . .
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'
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
O12 Mo1 O11 102.62(14) . . ?
O12 Mo1 O28 91.60(12) . . ?
O11 Mo1 O28 158.55(12) . . ?
O12 Mo1 O18 159.57(12) . . ?
O11 Mo1 O18 90.65(12) . . ?
O28 Mo1 O18 80.58(10) . . ?
O12 Mo1 S1 84.00(10) . . ?
O11 Mo1 S1 107.61(9) . . ?
O28 Mo1 S1 89.59(7) . . ?
O18 Mo1 S1 77.14(7) . . ?
O12 Mo1 S2 109.08(9) . . ?
O11 Mo1 S2 83.15(9) . . ?
O28 Mo1 S2 77.01(7) . . ?
O18 Mo1 S2 87.66(7) . . ?
S1 Mo1 S2 161.26(3) . . ?
C11 S1 Mo1 100.58(13) . . ?
C21 S2 Mo1 99.46(13) . . ?
C16 O18 Mo1 123.9(2) . . ?
C26 O28 Mo1 123.3(2) . . ?
C23 O24 C25 121.0(3) . . ?
C13 014 C15 121.4(3) . . ?
C12 C11 C16 118.3(3) . . ?
C12 C11 S1 124.3(3) . . ?
C16 C11 S1 117.4(3) . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
014 C13 C12 121.5(3) . . ?
014 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
O18 C16 C15 121.8(3) . . ?
O18 C16 C11 119.9(3) . . ?
C15 C16 C11 118.3(3) . . ?
014 C15 C16 120.6(3) . . ?
014 C15 C17 113.6(3) . . ?
C16 C15 C17 125.8(3) . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C26 118.5(3) . . ?
C22 C21 S2 124.5(3) . . ?
C26 C21 S2 117.0(3) . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 O24 122.0(3) . . ?
C22 C23 H23 119.0 . . ?
O24 C23 H23 119.0 . . ?
O24 C25 C26 120.1(3) . . ?
O24 C25 C27 115.6(3) . . ?
C26 C25 C27 124.3(3) . . ?
O28 C26 C25 120.6(3) . . ?
O28 C26 C21 120.3(3) . . ?
C25 C26 C21 119.0(3) . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O21 Mo2 O22 103.82(12) . . ?
O21 Mo2 O48 96.88(12) . . ?
O22 Mo2 O48 106.95(12) . . ?
O21 Mo2 O38 90.59(11) . . ?
O22 Mo2 O38 159.87(12) . . ?
O48 Mo2 O38 84.75(10) . . ?
O21 Mo2 S3 102.12(9) . . ?
O22 Mo2 S3 85.28(10) . . ?
O48 Mo2 S3 154.26(7) . . ?
O38 Mo2 S3 77.90(7) . . ?
O21 Mo2 S4 165.34(9) . . ?
O22 Mo2 S4 90.36(9) . . ?
O48 Mo2 S4 75.05(7) . . ?
O38 Mo2 S4 76.65(7) . . ?
S3 Mo2 S4 82.47(3) . . ?
C41 S4 Mo2 94.71(13) . . ?
C31 S3 Mo2 100.42(14) . . ?
C43 O44 C45 120.0(3) . . ?
C33 O34 C35 121.0(3) . . ?
C46 O48 Mo2 128.9(2) . . ?
C36 O38 Mo2 123.0(2) . . ?
C32 C31 C36 118.6(4) . . ?
C32 C31 S3 123.9(3) . . ?
C36 C31 S3 117.5(3) . . ?
C33 C32 C31 118.9(4) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
O34 C33 C32 122.3(4) . . ?
O34 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
O34 C35 C36 120.2(4) . . ?
O34 C35 C37 114.5(3) . . ?
C36 C35 C37 125.3(4) . . ?
O38 C36 C35 120.8(4) . . ?
O38 C36 C31 120.4(3) . . ?
C35 C36 C31 118.7(4) . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 C46 116.2(3) . . ?
C42 C41 S4 124.9(3) . . ?
C46 C41 S4 118.9(3) . . ?
C43 C42 C41 119.5(4) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 O44 123.3(3) . . ?
C42 C43 H43 118.4 . . ?
O44 C43 H43 118.4 . . ?
O44 C45 C46 120.3(3) . . ?
O44 C45 C47 113.8(3) . . ?
C46 C45 C47 125.8(3) . . ?
O48 C46 C45 119.1(3) . . ?
O48 C46 C41 120.2(3) . . ?
C45 C46 C41 120.7(3) . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H51 O5 H52 108(5) . . ?
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 O12 1.714(3) . ?
Mo1 O11 1.718(3) . ?
Mo1 O28 2.095(3) . ?
Mo1 O18 2.127(2) . ?
Mo1 S1 2.4832(10) . ?
Mo1 S2 2.4993(10) . ?
S1 C11 1.703(4) . ?
S2 C21 1.705(4) . ?
O18 C16 1.306(4) . ?
O28 C26 1.316(4) . ?
O24 C23 1.344(4) . ?
O24 C25 1.359(4) . ?
014 C13 1.346(5) . ?
014 C15 1.346(4) . ?
C11 C12 1.412(5) . ?
C11 C16 1.427(5) . ?
C12 C13 1.346(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C16 C15 1.384(5) . ?
C15 C17 1.480(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C22 1.413(5) . ?
C21 C26 1.413(5) . ?
C22 C23 1.344(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C25 C26 1.385(5) . ?
C25 C27 1.476(5) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Mo2 O21 1.708(3) . ?
Mo2 O22 1.714(3) . ?
Mo2 O48 1.975(3) . ?
Mo2 O38 2.130(2) . ?
Mo2 S3 2.4630(10) . ?
Mo2 S4 2.7376(9) . ?
S4 C41 1.682(4) . ?
S3 C31 1.716(4) . ?
O44 C43 1.345(5) . ?
O44 C45 1.357(4) . ?
O34 C33 1.335(5) . ?
O34 C35 1.353(5) . ?
O48 C46 1.337(4) . ?
O38 C36 1.308(5) . ?
C31 C32 1.404(5) . ?
C31 C36 1.414(6) . ?
C32 C33 1.347(6) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C35 C36 1.379(5) . ?
C35 C37 1.467(6) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.424(5) . ?
C41 C46 1.430(5) . ?
C42 C43 1.339(6) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C45 C46 1.365(5) . ?
C45 C47 1.483(5) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
O5 H51 0.95(2) . ?
O5 H52 0.94(2) . ?
