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_7129270
_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            'C48 H34 O4 P2 Si'
_chemical_formula_weight         764.78
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_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                92.0040(10)
_cell_angle_beta                 96.5540(10)
_cell_angle_gamma                115.7740(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4128(3)
_cell_length_b                   9.5763(4)
_cell_length_c                   26.1896(10)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.906
_cell_measurement_theta_min      4.718
_cell_volume                     2102.51(14)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42323
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.442
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
;
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
; 
 Flack x determined using 4311 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.017(3)
_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   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         16270
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1152P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                11254
_reflns_number_total             16270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05576c2.cif
_cod_data_source_block           mo_d8v21604_0m
_cod_database_code               7129270
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2013-4
_shelx_res_checksum              15500