Organocalcium Complex-Catalyzed Selective Redistribution of ArSiH3 or Ar(alkyl)SiH2 to Ar3SiH or Ar2(alkyl)SiH
Li, Tao; McCabe, Karl N.; Maron, Laurent; Leng, Xuebing; Chen, Yaofeng; ACS Catalysis  (2021) 6348–6356; doi:10.1021/acscatal.1c00463

data_4518770
_publ_section_title
;
 Organocalcium Complex-Catalyzed Selective Redistribution of ArSiH3 or
 Ar(alkyl)SiH2 to Ar3SiH or Ar2(alkyl)SiH
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              6348
_journal_page_last               6356
_journal_paper_doi               10.1021/acscatal.1c00463
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C48 H84 Ca2 N8'
_chemical_formula_sum            'C48 H84 Ca2 N8'
_chemical_formula_weight         853.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5031(5)
_cell_length_b                   49.3831(15)
_cell_length_c                   13.0859(3)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.774
_cell_measurement_theta_min      3.624
_cell_volume                     12603.3(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.04
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28810
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.948
_diffrn_reflns_theta_min         3.623
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1571 before and 0.0810 after correction. The Ratio of minimum to maximum transmission is 0.8503. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.899
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.123(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5646
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+6.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4561
_reflns_number_total             5646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00463_si_004.cif
_cod_data_source_block           mj19400
_cod_database_code               4518770
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.877(18)
 0.123(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C4(H4), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              55274
_shelx_hkl_checksum              96271
_shelx_fab_checksum              10303
_olex2_submission_special_instructions 'No special instructions were received'