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_4518270
_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         'C42 H43 F6 Fe Mo N3 O6 S2, C H2 Cl2'
_chemical_formula_sum            'C43 H45 Cl2 F6 Fe Mo N3 O6 S2'
_chemical_formula_weight         1100.63
_chemical_name_common            6
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.676(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4984(6)
_cell_length_b                   18.3575(10)
_cell_length_c                   12.3063(7)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      1.84
_cell_volume                     2341.1(2)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40206
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.7052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(11)
_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     589
_refine_ls_number_reflns         11524
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                9606
_reflns_number_total             11524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs0c03978_si_006.cif
_cod_data_source_block           buch214
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4518270