Oxidoperoxidomolybdenum(vi) complexes with acylpyrazolonate ligands: synthesis, structure and catalytic properties.
Begines, Emilio; Carrasco, Carlos J.; Montilla, Francisco; Álvarez, Eleuterio; Marchetti, Fabio; Pettinari, Riccardo; Pettinari, Claudio; Galindo, Agustín; Dalton transactions (Cambridge, England : 2003) 47 (2017) 197–208; doi:10.1039/c7dt03939e

data_7702166
_publ_section_title
;
 Oxidoperoxidomolybdenum(vi) complexes with acylpyrazolonate ligands:
 synthesis, structure and catalytic properties.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              197
_journal_page_last               208
_journal_paper_doi               10.1039/c7dt03939e
_journal_volume                  47
_journal_year                    2017
_chemical_formula_moiety         'C13 H8 F5 Mo N2 O7, C24 H20 P'
_chemical_formula_sum            'C37 H28 F5 Mo N2 O7 P'
_chemical_formula_weight         834.52
_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
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-10-19 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                88.5380(10)
_cell_angle_beta                 84.4170(10)
_cell_angle_gamma                71.8310(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1318(4)
_cell_length_b                   13.3189(6)
_cell_length_c                   13.8696(6)
_cell_measurement_reflns_used    7516
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.57
_cell_volume                     1769.85(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29875
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.609
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.9075
_exptl_absorpt_correction_T_min  0.7900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       plate
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6358
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0471P)^2^+1.1365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6026
_reflns_number_total             6358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03939e2.cif
_cod_data_source_block           2
_cod_database_code               7702166
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.908
_shelx_res_checksum              31919