Cationic molybdenum oxo alkylidenes stabilized by N-heterocyclic carbenes: from molecular systems to efficient supported metathesis catalysts
Musso, Janis V.; De Jesus Silva, Jordan; Benedikter, Mathis J.; Groos, Jonas; Frey, Wolfgang; Copéret, Christophe; Buchmeiser, Michael R.; Chemical Science 13 (2022) 8649–8656; doi:10.1039/D2SC03321F

data_1567403
_publ_section_title
;
 Cationic molybdenum oxo alkylidenes stabilized by N-heterocyclic
 carbenes: from molecular systems to efficient supported metathesis
 catalysts
;
_journal_issue                   29
_journal_name_full               'Chemical Science'
_journal_page_first              8649
_journal_page_last               8656
_journal_paper_doi               10.1039/D2SC03321F
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety
'C16 Al F36 O4, C36 H42 F5 Mo N2 O3, 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C53 H44 Al Cl F41 Mo N2 O7'
_chemical_formula_weight         1758.27
_chemical_name_common            Mo-8
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-02-09 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                79.898(2)
_cell_angle_beta                 78.994(2)
_cell_angle_gamma                86.057(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9654(8)
_cell_length_b                   13.8876(9)
_cell_length_c                   19.3009(12)
_cell_measurement_reflns_used    13437
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.403
_cell_measurement_theta_min      1.490
_cell_volume                     3356.2(4)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71115
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.403
_diffrn_reflns_theta_min         1.490
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       prism
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.421
_exptl_crystal_size_min          0.343
_refine_diff_density_max         1.794
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         16752
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+12.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13437
_reflns_number_total             16752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03321f2.cif
_cod_data_source_block           buch346
_cod_database_code               1567403
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              69595