Proton-Coupled Electron Transfer to a Molybdenum Ethylene Complex Yields a β-Agostic Ethyl: Structure, Dynamics and Mechanism.
Bezdek, Máté J; Chirik, Paul J.; Journal of the American Chemical Society 140 (2018) 13817–13826; doi:10.1021/jacs.8b08460

data_4133093
_publ_section_title
;
 Proton-Coupled Electron Transfer to a Molybdenum Ethylene Complex Yields
 a \b-Agostic Ethyl: Structure, Dynamics and Mechanism.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13817
_journal_page_last               13826
_journal_paper_doi               10.1021/jacs.8b08460
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C49 H45 Mo N3 P2'
_chemical_formula_weight         833.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 96.8570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3714(2)
_cell_length_b                   16.5866(3)
_cell_length_c                   22.7054(4)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.14
_cell_measurement_theta_min      3.31
_cell_volume                     3877.99(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'I\mS microfocus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29124
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.157
_diffrn_reflns_theta_min         3.308
_exptl_absorpt_coefficient_mu    3.849
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         7344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0225P)^2^+3.9974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6859
_reflns_number_total             7344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08460_si_002.cif
_cod_data_source_block           mb51
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133093
_shelx_estimated_absorpt_t_min   0.541
_shelx_estimated_absorpt_t_max   0.726
_shelxl_version_number           2014-3
_shelx_res_checksum              40387
_shelx_hkl_checksum              5597