Calcium-Catalyzed Dehydrogenative Silylation of Aromatic Ethers with Hydrosilane
Zhao, Lanxiao; Shi, Xianghui; Cheng, Jianhua; ACS Catalysis 11 (2021) 2041–2046; doi:10.1021/acscatal.0c05440

data_4518526
_publ_section_title
;
 Calcium-Catalyzed Dehydrogenative Silylation of Aromatic Ethers with
 Hydrosilane
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              2041
_journal_page_last               2046
_journal_paper_doi               10.1021/acscatal.0c05440
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C55 H76 B1 Br1 Ca1 N6 O1'
_chemical_formula_sum            'C55 H76 B Br Ca N6 O'
_chemical_formula_weight         968.01
_chemical_name_common            '[(TpAd,iPr)Ca(o-MeO-C6H3-Br-p)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.288(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9092(8)
_cell_length_b                   22.3669(12)
_cell_length_c                   18.0189(11)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      2.16
_cell_volume                     5102.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            91021
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.155
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.558
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         8925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+10.5597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7353
_reflns_number_total             8925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05440_si_001.cif
_cod_data_source_block           Zhao04-2020
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518526
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              19402
_shelx_hkl_checksum              16834