Iron-catalyzed asymmetric hydrosilylation of ketones
Ziqing Zuo; Lei Zhang; Xuebing Leng; Zheng Huang; Chem.Commun. 51 (2015) 5073–; doi:10.1039/C5cc00612K

data_7116739
_publ_section_title
;
 Iron-catalyzed asymmetric hydrosilylation of ketones
;
_journal_name_full               Chem.Commun.
_journal_page_first              5073
_journal_paper_doi               10.1039/C5cc00612K
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C26.5 H36.5 Br2 Fe N3.5 O1.5'
_chemical_formula_weight         643.76
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-01-20 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.090(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.777(4)
_cell_length_b                   10.030(3)
_cell_length_c                   17.685(5)
_cell_measurement_reflns_used    3003
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.34
_cell_volume                     2755.3(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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  0.1132
_diffrn_reflns_av_unetI/netI     0.2432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26394
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.324
_diffrn_reflns_theta_min         1.169
_exptl_absorpt_coefficient_mu    3.475
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
; 
 Flack x determined using 2290 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.019(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         15709
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1556
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                7485
_reflns_number_total             15709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc00612k2_a.cif
_cod_data_source_block           mo_dm14439_0m
_cod_depositor_comments
;
2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C53 H73 Br4 Fe2 N7 O3'
_cod_original_formula_weight         1287.52
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2755.3(12)
_cod_database_code               7116739
_shelx_estimated_absorpt_t_min   0.681
_shelx_estimated_absorpt_t_max   0.966
_shelxl_version_number           2014-3
_shelx_res_checksum              15605
_shelx_hkl_checksum              46293