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_7714250
_publ_section_title
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 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         'C56 H58 Cl N5 Sb, C32 H12 B F24'
_chemical_formula_sum            'C88 H70 B Cl F24 N5 Sb'
_chemical_formula_weight         1821.50
_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             2022-11-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-21 deposited with the CCDC.	2023-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                84.139(2)
_cell_angle_beta                 74.036(2)
_cell_angle_gamma                66.218(2)
_cell_formula_units_Z            2
_cell_length_a                   16.8928(7)
_cell_length_b                   17.0063(8)
_cell_length_c                   19.8764(9)
_cell_measurement_reflns_used    9258
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      53.66
_cell_measurement_theta_min      2.47
_cell_volume                     5023.5(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            107781
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.155
_diffrn_reflns_theta_min         2.011
_diffrn_source_current           3.0
_diffrn_source_power             0.20958
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1028 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.9058.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         18455
_refine_ls_number_restraints     816
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1339P)^2^+19.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2432
_refine_ls_wR_factor_ref         0.2596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13739
_reflns_number_total             18455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03310d2.cif
_cod_data_source_block           LSbClB(ArF4)DMAP
_cod_database_code               7714250
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.568
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C032 \\sim C03D \\sim C03E \\sim C03F \\sim C030 \\sim C02D \\sim C02R \\sim
C034 \\sim C037 \\sim C02W \\sim C02L \\sim C028: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
3. Others
 Fixed Sof: F4(0.5) F5(0.5) F18(0.5) F7(0.5) F3(0.5) F1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00Y(H00Y), C012(H012), C013(H013), C015(H015), C017(H017),
 C018(H018), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01L(H01L),
 C01M(H01M), C01R(H01R), C01T(H01T), C01V(H01V), C01W(H01W), C01X(H01X),
 C01Y(H01Y), C021(H021), C022(H022), C023(H023), C024(H024), C027(H027),
 C02B(H02B), C02E(H02E), C02L(H02L), C02M(H02), C02N(H02N), C02Q(H02Q),
 C02R(H02R), C02W(H02Y), C02X(H1), C030(H030), C032(H032), C034(H034),
 C037(H037), C03D(H03J), C03E(H03K), C03F(H03L)
4.b Idealised Me refined as rotating group:
 C02F(H02A,H02C,H02D), C02I(H02F,H02G,H02H), C02P(H02I,H02J,H02K), C02S(H02M,
 H02O,H02P), C02T(H02S,H02T,H02U), C02U(H02V,H02W,H02X), C02Y(H02Z,H,HA),
 C035(H03A,H03B,H03C), C036(H03D,H03E,H03F), C03B(H03G,H03H,H03I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7462
_shelx_fab_checksum              46660
_olex2_submission_special_instructions 'No special instructions were received'