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_7714247
_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         'C53 H58 Li N3 O'
_chemical_formula_sum            'C53 H58 Li N3 O'
_chemical_formula_weight         759.96
_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
_audit_creation_date             2022-11-18
_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                87.949(2)
_cell_angle_beta                 69.745(2)
_cell_angle_gamma                81.798(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0383(5)
_cell_length_b                   13.7852(6)
_cell_length_c                   14.1852(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.52
_cell_measurement_theta_min      3.24
_cell_volume                     2185.64(16)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.964
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29440
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.511
_diffrn_reflns_theta_min         3.239
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5641
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1309 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.7485.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.5530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7587
_reflns_number_total             8351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03310d2.cif
_cod_data_source_block           LLi
_cod_database_code               7714247
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B)
1.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C9(H9), C10(H10), C13(H13), C17(H17), C23(H23), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
1.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              18385
_olex2_submission_special_instructions 'No special instructions were received'