Intramolecular Iron-Mediated C-H Bond Heterolysis with an Assist of Pendant Base in a [FeFe]-Hydrogenase Model.
Zheng, Dehua; Wang, Ning; Wang, Mei; Ding, Shengda; Ma, Chengbing; Darensbourg, Marcetta Y.; Hall, Michael B.; Sun, Licheng; Journal of the American Chemical Society  (2014) 141007112505006–; doi:10.1021/ja5078014

data_4122749
_publ_section_title
;
 Intramolecular Iron-Mediated C-H Bond Heterolysis with an Assist of
 Pendant Base in a [FeFe]-Hydrogenase Model.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141007112505006
_journal_paper_doi               10.1021/ja5078014
_journal_year                    2014
_chemical_formula_moiety         'C72 H55 B Cl2 F24 Fe2 N2 O4 P2 S2'
_chemical_formula_sum            'C72 H55 B Cl2 F24 Fe2 N2 O4 P2 S2'
_chemical_formula_weight         1787.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                96.816(2)
_cell_angle_beta                 106.050(2)
_cell_angle_gamma                117.220(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7976(13)
_cell_length_b                   13.3807(13)
_cell_length_c                   13.8252(14)
_cell_measurement_reflns_used    4309
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.58
_cell_measurement_theta_min      2.57
_cell_volume                     1938.2(3)
_computing_cell_refinement       'APEXII (Bruker, 2012a)'
_computing_data_collection       'APEXII (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_molecular_graphics    'shelXLe (H\"ubschle 2011)'
_computing_publication_material  'Ciftab (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12326
_diffrn_reflns_point_group_measured_fraction_full 0.708
_diffrn_reflns_point_group_measured_fraction_max 0.728
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.837
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2009) was employed for absorption correction.
wR2(int) was XXXXX before and  XXXXX after correction.
The ratio of minimum to maximum transmission factors was XXXXXX
Additional spherical absorption correction applied with mu*r =  XXXXXX
The \l/2 correction was not applied
;
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2521 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         9954
_refine_ls_number_restraints     993
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.465
_reflns_Friedel_fraction_full    0.449
_reflns_Friedel_fraction_max     0.462
_reflns_number_gt                8754
_reflns_number_total             9954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5078014_si_005.cif
_cod_data_source_block           ok
_cod_database_code               4122749
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.938
_shelxl_version_number           2014-1
_shelx_res_checksum              20168
_shelx_hkl_checksum              43377