Oxidation of sulfides in aqueous media catalyzed by pyrazole-oxidoperoxido-molybdenum(VI) complexes
Bruno, Sofia M.; Amarante, Tatiana R.; Almeida Paz, Filipe A.; Pillinger, Martyn; Valente, Anabela A.; Gonçalves, Isabel S.; Inorganica Chimica Acta 511 (2020) 119814–; doi:10.1016/j.ica.2020.119814

data_1564173
_publ_section_title
;
 Oxidation of sulfides in aqueous media catalyzed by
 pyrazole-oxidoperoxido-molybdenum(VI) complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119814
_journal_paper_doi               10.1016/j.ica.2020.119814
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C10 H16 Mo8 N4 O26.20, 4(C5 H9 N2), 4(H2 O)'
_chemical_formula_sum            'C30 H60 Mo8 N12 O30.2'
_chemical_formula_weight         1839.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                115.385(2)
_cell_angle_beta                 91.606(2)
_cell_angle_gamma                108.6980(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6007(4)
_cell_length_b                   13.1512(7)
_cell_length_c                   14.6215(7)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.54
_cell_volume                     1388.58(12)
_computing_cell_refinement       'SAINT V8.37a   (Bruker, 2015)'
_computing_data_collection       'APEX3 2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37a   (Bruker, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST '
_diffrn_measurement_method       '\w / \f scans'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26732
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         3.574
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2016/2
  Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
  J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_description       Block
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.1044
_exptl_transmission_factor_min   0.0661
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7440
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+0.6616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0444
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7001
_reflns_number_total             7440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119814.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C30 H60 Mo8 N12 O30.20'
_cod_database_code               1564173
_shelx_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.733
_exptl_absorpt_special_details
;
?
;
_shelx_res_checksum              46346
_shelx_hkl_checksum              6829