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_4518274
_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_sum            'C76 H58.5 B F33 Mo N3.5 O'
_chemical_formula_weight         1770.51
_chemical_name_common            1
_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-2016/4
_cell_angle_alpha                83.163(3)
_cell_angle_beta                 86.320(3)
_cell_angle_gamma                89.432(4)
_cell_formula_units_Z            4
_cell_length_a                   12.8710(8)
_cell_length_b                   15.3569(10)
_cell_length_c                   39.432(2)
_cell_measurement_reflns_used    20776
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      26.474
_cell_measurement_theta_min      1.490
_cell_volume                     7722.7(8)
_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, 1991)'
_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 1.000
_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  0.0566
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            118933
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.474
_diffrn_reflns_theta_min         1.490
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.9053
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             3564
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2308
_refine_ls_number_reflns         31698
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+6.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20776
_reflns_number_total             31698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03978_si_001.cif
_cod_data_source_block           buch243_sq
_cod_original_formula_sum        'C76 H58.50 B F33 Mo N3.50 O'
_cod_database_code               4518274
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              23315
_shelx_hkl_checksum              68387
_shelx_fab_checksum              22196