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_4128931
_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         'C20 H31 Co'
_chemical_formula_sum            'C20 H31 Co'
_chemical_formula_weight         330.38
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.611(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0700(6)
_cell_length_b                   8.4605(6)
_cell_length_c                   12.8684(10)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.10
_cell_measurement_theta_min      2.88
_cell_volume                     876.86(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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  0.0838
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.836
_diffrn_reflns_theta_min         2.899
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  0.7480
_exptl_absorpt_correction_T_min  0.6950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0645 before and 0.0512 after correction. The Ratio of minimum to maximum transmission is 0.9291. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         5620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.1403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3938
_reflns_number_total             5620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00193_si_002.cif
_cod_data_source_block           p17300
_cod_database_code               4128931
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H6AB(0.5) H6AC(0.5) H6AA(0.5) H6BF(0.5) H6BE(0.5) H6BD(0.5)
 C1A(0.5) C1B(0.5) H1A(0.5)
3.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C6(H6AB,H6AC,H6AA), C6(H6BF,H6BE,H6BD)
;
_shelx_res_checksum              90106
_shelx_hkl_checksum              27579
_olex2_submission_special_instructions 'No special instructions were received'