Mechanism of Olefin Metathesis with Neutral and Cationic Molybdenum Imido Alkylidene N-Heterocyclic Carbene Complexes.
Herz, Katharina; Podewitz, Maren; Stöhr, Laura; Wang, Dongren; Frey, Wolfgang; Liedl, Klaus R.; Sen, Suman; Buchmeiser, Michael R.; Journal of the American Chemical Society 141 (2019) 8264–8276; doi:10.1021/jacs.9b02092

data_4127240
_publ_section_title
;
 Mechanism of Olefin Metathesis with Neutral and Cationic Molybdenum Imido
 Alkylidene N-Heterocyclic Carbene Complexes.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8264
_journal_page_last               8276
_journal_paper_doi               10.1021/jacs.9b02092
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C46 H43 F8 Mo N3 O5 S, C2 H4 Cl2'
_chemical_formula_sum            'C46 H47 Cl2 F8 Mo N3 O5 S'
_chemical_formula_weight         1072.76
_chemical_name_systematic        6a
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                85.916(3)
_cell_angle_beta                 73.747(2)
_cell_angle_gamma                75.819(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6134(7)
_cell_length_b                   13.4666(7)
_cell_length_c                   16.8383(10)
_cell_measurement_reflns_used    8938
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.446
_cell_measurement_theta_min      1.730
_cell_volume                     2662.2(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, 1991)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa AEXII 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     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42846
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.446
_diffrn_reflns_theta_min         1.730
_diffrn_source                   sealed-tube
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0497P)^2^+1.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8938
_reflns_number_total             10887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02092_si_003.cif
_cod_data_source_block           buch168
_cod_depositor_comments
'Adding full bibliography for 4127238--4127240.cif.'
_cod_database_code               4127240
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              16040
_shelx_hkl_checksum              71994
_shelx_fab_checksum              1224