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_1564172
_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         'C6 H8 Mo N4 O5'
_chemical_formula_sum            'C6 H8 Mo N4 O5'
_chemical_formula_weight         312.10
_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   geom
_cell_angle_alpha                93.620(2)
_cell_angle_beta                 103.842(2)
_cell_angle_gamma                98.215(2)
_cell_formula_units_Z            4
_cell_length_a                   8.4202(6)
_cell_length_b                   9.3491(6)
_cell_length_c                   14.3933(9)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      2.53
_cell_volume                     1083.27(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      180(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.0217
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12968
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         3.568
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.224
_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    1.914
_exptl_crystal_description       Block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   0.0976
_exptl_transmission_factor_min   0.0650
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0196
_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^)+(0.0239P)^2^+0.3386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5455
_reflns_number_total             5798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119814.cif
_cod_data_source_block           1
_cod_database_code               1564172
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.919
_exptl_absorpt_special_details
;
?
;
_shelx_res_checksum              2552
_shelx_hkl_checksum              54562