Molybdenum(IV) β-diketonate complexes as highly active catalysts for allylic substitution reactions.
Masero, Fabio; Mougel, Victor; Chemical communications (Cambridge, England) 59 (2023) 4636–4639; doi:10.1039/d3cc00572k

data_7131421
_publ_section_title
;
 Molybdenum(IV) &#x3b2;-diketonate complexes as highly active catalysts
 for allylic substitution reactions.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4636
_journal_page_last               4639
_journal_paper_doi               10.1039/d3cc00572k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C24 H38 F6 Mo O10 S2'
_chemical_formula_sum            'C24 H38 F6 Mo O10 S2'
_chemical_formula_weight         760.60
_chemical_name_systematic
'Molybdenum bis(pivaloylmethanate) bis(triflate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_length_c                   18.382(5)
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_cell_measurement_theta_max      52.388
_cell_measurement_theta_min      4.842
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_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
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_diffrn_measurement_device       'three-circle diffractometer'
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_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
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_diffrn_source                   'microfocus sealed X-ray tube'
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_diffrn_source_type              'Incoatec I\ms'
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'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
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_exptl_crystal_recrystallization_method
'from acetonitrile at -35 degree Celsius'
_exptl_crystal_size_max          0.615
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.194
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3253
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_refine_ls_R_factor_all          0.0605
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+18.6454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2770
_reflns_number_total             3253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00572k2.cif
_cod_data_source_block           fma_479-firsttry
_cod_depositor_comments
'Adding full bibliography for 7131417--7131422.cif.'
_cod_original_cell_volume        3280.5(14)
_cod_database_code               7131421
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.891
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              49668
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_olex2_date_sample_data_collection 2021-06-01
_olex2_date_sample_submission    2021-06-01
_olex2_submission_original_sample_id FMA_479
_olex2_submission_special_instructions 'No special instructions were received'