Concise Synthesis and Application of Enantiopure Spirobiphenoxasilin-Diol and Its Related Chiral Ligands
Yang, Lei; Xu, Wen-Qiang; Liu, Tao; Wu, Yichen; Wang, Bi-Qin; Wang, Peng; Chemical Communications  (2021) –; doi:10.1039/D1CC05576C

data_7129269
_publ_section_title
;
 Concise Synthesis and Application of Enantiopure Spirobiphenoxasilin-Diol
 and Its Related Chiral Ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05576C
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C24 H20 O6 Si'
_chemical_formula_weight         432.49
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2021-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.569(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1800(5)
_cell_length_b                   27.5745(18)
_cell_length_c                   9.1884(6)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.952
_cell_measurement_theta_min      4.772
_cell_volume                     2163.0(2)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26188
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
; 
 Flack x determined using 2546 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_coef       0.0055(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8019
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.1044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6455
_reflns_number_total             8019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05576c2.cif
_cod_data_source_block           mo_d8v21603_0m
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7129269
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              1112