CO Reduction to CH3OSiMe3: Electrophile-Promoted Hydride Migration at a Single Fe Site.
Deegan, Meaghan M.; Peters, Jonas C.; Journal of the American Chemical Society 139 (2017) 2561–2564; doi:10.1021/jacs.6b12444

data_4125554
_publ_section_title
;
 CO Reduction to CH3OSiMe3: Electrophile-Promoted Hydride Migration at a
 Single Fe Site.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2561
_journal_page_last               2564
_journal_paper_doi               10.1021/jacs.6b12444
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C37 H55 B Fe O P3'
_chemical_formula_sum            'C37 H55 B Fe O P3'
_chemical_formula_weight         675.38
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.016(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9781(13)
_cell_length_b                   15.8664(18)
_cell_length_c                   20.543(2)
_cell_measurement_reflns_used    9470
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.585
_cell_measurement_theta_min      2.332
_cell_volume                     3486.3(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            229418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.332
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0742 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.9393. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'orange brown'
_exptl_crystal_colour_modifier   orange
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         13298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.6720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11887
_reflns_number_total             13298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12444_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 4125551--4125555.cif.'
_cod_database_code               4125554
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C20(H20), C29(H29), C23(H23), C35(H35), C32(H32)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C3(H3), C4(H4), C10(H10), C18(H18), C6(H6), C11(H11),
 C15(H15), C12(H12), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C24(H24A,H24B,H24C), C36(H36A,
 H36B,H36C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C),
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              56627
_shelx_hkl_checksum              78277
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'