Utilizing Bis(imino)dihydroacridanide Pincer Ligands in p-Block Chemistry: Synthesis and Catalysis of an Antimony Monocation Salt
Lan, Xiaofang; Zhang, Xin; Mei, Yanbo; Hu, Chaopeng; Liu, Liu Leo; Dalton Transactions  (2023) –; doi:10.1039/D3DT03310D

data_7714249
_publ_section_title
;
 Utilizing Bis(imino)dihydroacridanide Pincer Ligands in p-Block
 Chemistry: Synthesis and Catalysis of an Antimony Monocation Salt
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03310D
_journal_year                    2023
_chemical_formula_moiety         'C49 H48 Cl N3 Sb, C32 H12 B F24, C5 H12'
_chemical_formula_sum            'C86 H72 B Cl F24 N3 Sb'
_chemical_formula_weight         1771.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-21 deposited with the CCDC.	2023-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                91.171(5)
_cell_angle_beta                 101.962(4)
_cell_angle_gamma                112.763(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0357(8)
_cell_length_b                   15.0197(11)
_cell_length_c                   24.7036(17)
_cell_measurement_reflns_used    3487
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      49.48
_cell_measurement_theta_min      3.52
_cell_volume                     4003.3(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker PHOTON II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.1307
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37201
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         3.211
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.948
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1010 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.8503.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.970
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         14260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.1107
_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^)+(0.0682P)^2^+59.5631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2576
_refine_ls_wR_factor_ref         0.2729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10175
_reflns_number_total             14260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03310d2.cif
_cod_data_source_block           LSbCl-BArF4
_cod_database_code               7714249
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.506
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(F01J) = Uanis(F00J)
3.a Secondary CH2 refined with riding coordinates:
 C02X(H02P,H02Q), C033(H03J,H03K), C037(H03L,H03M)
3.b Aromatic/amide H refined with riding coordinates:
 C00Y(H00Y), C013(H013), C015(H015), C016(H016), C018(H018), C019(H019),
 C01A(H01I), C01B(H01D), C01D(H01J), C01E(H01L), C01G(H01H), C01K(H01K),
 C01M(H01M), C01P(H01P), C01S(H01S), C01V(H01V), C01W(H01W), C01Z(H01Z),
 C020(H020), C024(H024), C026(H026), C027(H027), C02A(H02M), C02B(H02B),
 C02I(H02I), C02J(H02J), C02N(H02N), C02O(H02O), C02R(H02R), C02S(H02S),
 C02T(H02T), C02U(H02U), C02W(H02W), C030(H030), C034(H034), C035(H035)
3.c Idealised Me refined as rotating group:
 C014(H01A,H01B,H01C), C01C(H01E,H01F,H01G), C02Q(H02A,H02C,H02D), C02V(H02E,
 H02F,H02G), C02Y(H02H,H02K,H02L), C02Z(H02V,H02X,H02Y), C031(H03A,H03B,H03C),
 C032(H03D,H03E,H03F), C036(H03G,H03H,H03I), C038(H03N,H03O,H03P)
;
_shelx_res_checksum              10273
_olex2_submission_special_instructions 'No special instructions were received'