Mechanistic Studies on Rhodium-Catalyzed Enantioselective Silylation of Aryl C-H Bonds.
Lee, Taegyo; Hartwig, John F.; Journal of the American Chemical Society 139 (2017) 4879–4886; doi:10.1021/jacs.7b00737

data_4126153
_publ_section_title
;
 Mechanistic Studies on Rhodium-Catalyzed Enantioselective Silylation of
 Aryl C-H Bonds.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4879
_journal_page_last               4886
_journal_paper_doi               10.1021/jacs.7b00737
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C57 H63 O P2 Rh S Si'
_chemical_formula_weight         989.07
_chemical_name_common            compound4
_chemical_name_systematic        compound4
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   22.1200(17)
_cell_length_b                   22.8814(16)
_cell_length_c                   9.7523(7)
_cell_measurement_reflns_used    9416
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.27
_cell_volume                     4936.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
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_diffrn_ambient_temperature      100(2)
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_diffrn_measurement_device_type  'Bruker APEX-II CCD'
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0243
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_diffrn_reflns_theta_max         25.392
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_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.517
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       rod
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
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_refine_diff_density_min         -0.274
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_refine_ls_abs_structure_details
; 
 Flack x determined using 3772 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.022(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0183P)^2^+2.1472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0466
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                8754
_reflns_number_total             9051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00737_si_002.cif
_cod_data_source_block           compound4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_database_code               4126153
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
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_shelx_res_checksum              43512
_shelx_hkl_checksum              12371