Crystallographic evidence for a continuum and reversal of roles in primary-secondary interactions in antimony Lewis acids: applications in carbonyl activation.
Sharma, Deepti; Benny, Annabel; Gupta, Radhika; Jemmis, Eluvathingal D.; Venugopal, Ajay; Chemical communications (Cambridge, England) 58 (2022) 11009–11012; doi:10.1039/d2cc04027a

data_7130679
_publ_section_title
;
 Crystallographic evidence for a continuum and reversal of roles in
 primary-secondary interactions in antimony Lewis acids: applications in
 carbonyl activation.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11009
_journal_page_last               11012
_journal_paper_doi               10.1039/d2cc04027a
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C24 H12 B Cl8, C24 H38 N O P Sb, C H2 Cl2'
_chemical_formula_sum            'C49 H52 B Cl10 N O P Sb'
_chemical_formula_weight         1188.94
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-23 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4940(18)
_cell_length_b                   12.5955(11)
_cell_length_c                   20.8355(18)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.63
_cell_measurement_theta_min      2.24
_cell_volume                     5284.1(8)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics    'ORTEP3- 2014.1(Farrugia, 1997) '
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker KAPPA 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  0.0537
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54028
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.995
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      1.495
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 6058 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         18591
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+3.0448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15329
_reflns_number_total             18591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04027a2.cif
_cod_data_source_block           2A
_cod_depositor_comments
'Adding full bibliography for 7130672--7130679.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7130679
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              30170
_shelx_hkl_checksum              75820