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_4133091
_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            'C81 H57 B F24 Mo N3 P2'
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_space_group_name_H-M_alt        'P n a 21'
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_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      3.48
_cell_volume                     7277.8(3)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
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_diffrn_measured_fraction_theta_max 0.997
_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
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_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
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_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.660
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_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       plate
_exptl_crystal_F_000             3428
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_exptl_crystal_size_mid          0.344
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_refine_diff_density_max         1.096
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.052(8)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         13916
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+6.9175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0862
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_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13852
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08460_si_002.cif
_cod_data_source_block           mb47
_cod_database_code               4133091
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.478
_shelxl_version_number           2014-3
_shelx_res_checksum              37302
_shelx_hkl_checksum              51614