Synthesis and characterization of a Sb(v)-containing polyoxomolybdate serving as a catalyst for sulfoxidation.
Lu, Jingkun; Wang, Yaping; Ma, Xinyi; Niu, Yanjun; Singh, Vikram; Ma, Pengtao; Zhang, Chao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8070–8077; doi:10.1039/c8dt01273c

data_7046375
_publ_section_title
;
 Synthesis and characterization of a Sb(v)-containing polyoxomolybdate
 serving as a catalyst for sulfoxidation.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8070
_journal_page_last               8077
_journal_paper_doi               10.1039/c8dt01273c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(Mo24 Na10 O136 Sb10), 4(C4 H12 N), 6(O)'
_chemical_formula_sum            'C16 H48 Mo12 N4 Na5 O74 Sb5'
_chemical_formula_weight         3355.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2579(7)
_cell_length_b                   23.8635(14)
_cell_length_c                   13.8297(8)
_cell_measurement_reflns_used    4646
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.25
_cell_volume                     4045.4(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9858
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.707
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.578
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1298 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.6014. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.755
_exptl_crystal_description       block
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.801
_refine_diff_density_min         -1.828
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+122.7571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1674
_reflns_number_total             1955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01273c2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7046375.cif.'
_cod_database_code               7046375
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Sb2, Na2}
{Sb3, Na3}
3. Uiso/Uaniso restraints and constraints
Uanis(Sb2) = Uanis(Na2)
Uanis(Sb3) = Uanis(Na3)
4. Others
 Fixed Sof: Sb2(0.125) Na2(0.125) Sb3(0.25) Na3(0.25) Na1(0.25) H1A(0.5)
 H1B(0.5) H1C(0.5) H2A(0.5) H2B(0.5) H2C(0.5) O6W(0.25)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_shelxl_version_number     2018/1
_olex2_submission_special_instructions 'No special instructions were received'