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_7131418
_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         'C10 H14 Cl2 Mo O4'
_chemical_formula_sum            'C10 H14 Cl2 Mo O4'
_chemical_formula_weight         365.05
_chemical_name_systematic        'Molybdenum bis(acetylacetonate) dichloride'
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-02
_audit_creation_method
;
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                92.355(3)
_cell_angle_beta                 112.501(3)
_cell_angle_gamma                118.207(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2362(5)
_cell_length_b                   7.3583(5)
_cell_length_c                   7.9687(6)
_cell_measurement_reflns_used    5512
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      3.26
_cell_volume                     332.36(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7118
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.462
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0605 before and 0.0470 after correction.
 The Ratio of minimum to maximum transmission is 0.89.

Final HKLF 4 output contains 21648 reflections, Rint = 0.1455
 (6569 with I > 3sig(I), Rint = 0.0793)
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             182
_exptl_crystal_recrystallization_method
'from acetonitrile at -35 degree Celsius'
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0220
_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^)+0.6511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1473
_reflns_number_total             1496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00572k2.cif
_cod_data_source_block           fma_377_4_0m
_cod_depositor_comments
'Adding full bibliography for 7131417--7131422.cif.'
_cod_database_code               7131418
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.773
_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:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              21274
_shelx_hkl_checksum              3895
_olex2_date_sample_data_collection 2021-03-03
_olex2_date_sample_submission    2021-03-03
_olex2_submission_original_sample_id FMA_377
_olex2_submission_special_instructions 'No special instructions were received'