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_7714246
_publ_section_title
;
 Utilizing Bis(imino)dihydroacridanide Pincer Ligands in p-Block
 Chemistry: Synthesis and Catalysis of an Antimony Monocation Salt
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03310D
_journal_year                    2023
_chemical_formula_moiety         'C49 H48 Cl2 N3 Sb, C7 H8'
_chemical_formula_sum            'C56 H56 Cl2 N3 Sb'
_chemical_formula_weight         963.68
_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     iterative
_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                98.084(9)
_cell_angle_beta                 114.097(6)
_cell_angle_gamma                114.290(6)
_cell_formula_units_Z            2
_cell_length_a                   12.9492(14)
_cell_length_b                   15.3029(19)
_cell_length_c                   15.575(2)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.076
_cell_measurement_theta_min      3.785
_cell_volume                     2384.9(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55621
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.706
_diffrn_reflns_theta_min         3.347
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.918
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9260
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+1.8667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8808
_reflns_number_total             9260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03310d2.cif
_cod_data_source_block           LSbCl2
_cod_original_cell_volume        2384.9(5)
_cod_database_code               7714246
_shelx_shelxl_version_number     2018/3
_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
C34 \\sim C57 \\sim C58 \\sim C33 \\sim C59 \\sim C32: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Fixed Sof: C32(0.67) H32A(0.67) H32B(0.67) H32C(0.67) C33(0.67) H33A(0.67)
 H33B(0.67) H33C(0.67) C34(0.67) H34A(0.67) H34B(0.67) H34C(0.67) C57(0.33)
 H57A(0.33) H57B(0.33) H57C(0.33) C59(0.33) H59A(0.33) H59B(0.33) H59C(0.33)
 C58(0.33) H58A(0.33) H58B(0.33) H58C(0.33)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C50(H50A,H50B,H50C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C58(H58A,
 H58B,H58C)
;
_shelx_res_checksum              89775
_olex2_submission_special_instructions 'No special instructions were received'