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_4518275
_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         'C26 H21 F18 Mo N O2'
_chemical_formula_sum            'C26 H21 F18 Mo N O2'
_chemical_formula_weight         817.38
_chemical_name_common            5
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 103.504(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4112(6)
_cell_length_b                   10.6334(6)
_cell_length_c                   23.3549(12)
_cell_measurement_reflns_used    7377
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      30.576
_cell_measurement_theta_min      1.716
_cell_volume                     2997.0(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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36888
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.576
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.344
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9156
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0383P)^2^+2.2316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7377
_reflns_number_total             9156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03978_si_005.cif
_cod_data_source_block           buch245
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518275
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.826
_shelx_res_checksum              30613
_shelx_hkl_checksum              38788