Charge Distribution in Cationic Molybdenum Imido Alkylidene N-Heterocyclic Carbene Complexes: A Combined X-ray, XAS, XES, DFT, Mössbauer, and Catalysis Approach
Benedikter, Mathis; Musso, Janis; Kesharwani, Manoj K.; Sterz, K. Leonard; Elser, Iris; Ziegler, Felix; Fischer, Felix; Plietker, Bernd; Frey, Wolfgang; Kästner, Johannes; Winkler, Mario; van Slageren, Joris; Nowakowski, Michal; Bauer, Matthias; Buchmeiser, Michael R.; ACS Catalysis  (2020) 14810–14823; doi:10.1021/acscatal.0c03978

data_4518272
_publ_section_title
;
 Charge Distribution in Cationic Molybdenum Imido Alkylidene
 N-Heterocyclic Carbene Complexes: A Combined X-ray, XAS, XES, DFT,
 M\"ossbauer, and Catalysis Approach
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              14810
_journal_page_last               14823
_journal_paper_doi               10.1021/acscatal.0c03978
_journal_year                    2020
_chemical_formula_moiety         'C43 H47 F9 Mo N3 O, C32 H12 B F24'
_chemical_formula_sum            'C75 H59 B F33 Mo N3 O'
_chemical_formula_weight         1752.00
_chemical_name_common            4
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                104.613(3)
_cell_angle_beta                 96.591(3)
_cell_angle_gamma                92.480(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8175(6)
_cell_length_b                   15.5311(8)
_cell_length_c                   20.3008(10)
_cell_measurement_reflns_used    15826
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      28.448
_cell_measurement_theta_min      1.484
_cell_volume                     3873.7(3)
_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-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83141
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.448
_diffrn_reflns_theta_min         1.484
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_correction_T_min  0.8787
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.346
_refine_diff_density_max         1.806
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         19226
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+19.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15826
_reflns_number_total             19226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03978_si_004.cif
_cod_data_source_block           buch267_sq
_cod_database_code               4518272
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.905
_shelx_res_checksum              37828
_shelx_hkl_checksum              81414
_shelx_fab_checksum              48251