Evidence for a Single Electron Shift in a Lewis Acid-Base Reaction.
Dong, Zhaowen; Cramer, Hanna H.; Schmidtmann, Marc; Paul, Lucas A.; Siewert, Inke; Müller, Thomas; Journal of the American Chemical Society 140 (2018) 15419–15424; doi:10.1021/jacs.8b09214

data_4133279
_publ_section_title
;
 Evidence for a Single Electron Shift in a Lewis Acid-Base Reaction.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15419
_journal_page_last               15424
_journal_paper_doi               10.1021/jacs.8b09214
_journal_volume                  140
_journal_year                    2018
_chemical_formula_structural     GeC4(CH3)2(Si(CH3)3)2Hf(C5H5)2B(C6F5)3
_chemical_formula_sum            'C40 H34 B F15 Ge Hf Si2'
_chemical_formula_weight         1117.74
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 93.9442(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1535(2)
_cell_length_b                   18.4694(5)
_cell_length_c                   21.3666(5)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.76
_cell_measurement_theta_min      2.29
_cell_volume                     3997.37(16)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            255001
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.249
_diffrn_reflns_theta_min         1.459
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.508
_exptl_absorpt_correction_T_max  0.7887
_exptl_absorpt_correction_T_min  0.5509
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.481
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         25184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20173
_reflns_number_total             25184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09214_si_001.cif
_cod_data_source_block           dzw156
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4133279
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.791
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              93832
_shelx_hkl_checksum              62024