Synthesis, characterization and oxygen atom transfer reactivity of a pair of Mo(IV)O- and Mo(VI)O2-enedithiolate complexes ‒ a look at both ends of the catalytic transformation
Ghosh, Ashta Chandra; Samuel, Prinson P.; Schulzke, Carola; Dalton Trans.  (2017) –; doi:10.1039/C7DT01470H

data_7043059
_publ_section_title
;
 Synthesis, characterization and oxygen atom transfer reactivity of a pair
 of Mo(IV)O- and Mo(VI)O2-enedithiolate complexes -- a look at both ends
 of the catalytic transformation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01470H
_journal_year                    2017
_chemical_formula_sum            'C56 H88 Mo N2 O S4'
_chemical_formula_weight         1029.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-04-03 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.281(3)
_cell_length_b                   14.491(3)
_cell_length_c                   27.124(5)
_cell_measurement_reflns_used    49982
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.7
_cell_measurement_theta_min      2.8
_cell_volume                     5613(2)
_computing_cell_refinement       'X-Area by STOE & Cie GmbH'
_computing_data_collection       'X-Area by STOE & Cie GmbH'
_computing_data_reduction        'X-Area by STOE & Cie GmbH'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  IPDSII
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.864
_diffrn_reflns_theta_min         1.501
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.9502
_exptl_absorpt_correction_T_min  0.7937
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       stick
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 3992 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9861
_reflns_number_total             10862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01470h2.cif
_cod_data_source_block           ad266b
_cod_database_code               7043059
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              50107