Cp* Noninnocence Leads to a Remarkably Weak C-H Bond via Metallocene Protonation.
Chalkley, Matthew J.; Oyala, Paul H.; Peters, Jonas C.; Journal of the American Chemical Society 141 (2019) 4721–4729; doi:10.1021/jacs.9b00193

data_4128932
_publ_section_title
;
 Cp* Noninnocence Leads to a Remarkably Weak C-H Bond via Metallocene
 Protonation.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4721
_journal_page_last               4729
_journal_paper_doi               10.1021/jacs.9b00193
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C21 H33 Co'
_chemical_formula_sum            'C21 H33 Co'
_chemical_formula_weight         344.40
_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   geom
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.956(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8973(5)
_cell_length_b                   9.6767(4)
_cell_length_c                   15.1146(6)
_cell_measurement_reflns_used    9426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.68
_cell_measurement_theta_min      2.50
_cell_volume                     1883.84(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0897
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            114061
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.726
_diffrn_reflns_theta_min         2.500
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8896.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         8739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+1.5515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6765
_reflns_number_total             8739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00193_si_002.cif
_cod_data_source_block           mjc
_cod_database_code               4128932
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C00A(H00A,H00B,H00C), C00D(H00D,H00E,H00F), C00E(H00G,H00H,H00I), C00F(H00J,
 H00K,H00L), C00G(H00M,H00N,H00O), C00H(H00P,H00Q,H00R), C00I(H00S,H00T,H00U),
 C00J(H00V,H00W,H00X), C00K(H00Y,H,HA), C00L(H00Z,HB,HC), C00M(H00,HD,HE)
;
_shelx_res_checksum              72823
_shelx_hkl_checksum              76701
_olex2_submission_special_instructions 'No special instructions were received'