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_7714248
_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 H49 N3'
_chemical_formula_sum            'C49 H49 N3'
_chemical_formula_weight         679.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 104.596(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6632(6)
_cell_length_b                   18.3235(8)
_cell_length_c                   15.7420(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.37
_cell_measurement_theta_min      3.77
_cell_volume                     3813.9(3)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.962
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39746
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.376
_diffrn_reflns_theta_min         3.773
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         6734
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0414P)^2^+1.8108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6017
_reflns_number_total             6734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03310d2.cif
_cod_data_source_block           LH
_cod_database_code               7714248
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim C01G \\sim C1 \\sim C01F \\sim C2 \\sim C01E \\sim C016: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Fixed Sof: C01E(0.75) H01l(0.75) H01m(0.75) H01n(0.75) C01F(0.75) H01o(0.75)
 H01p(0.75) H01q(0.75) C01G(0.75) H01r(0.75) H01s(0.75) H01t(0.75) C1(0.25)
 H1a(0.25) H1b(0.25) H1c(0.25) C2(0.25) H2a(0.25) H2b(0.25) H2c(0.25) C4(0.25)
 H4a(0.25) H4b(0.25) H4c(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 N001(H001), C00A(H00A), C00C(H00C), C00E(H00E), C00H(H00H), C00M(H00M),
 C00P(H00P), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014), C015(H015), C017(H017), C018(H018), C01A(H01d),
 C01B(H01e)
4.b Idealised Me refined as rotating group:
 C00O(H00b,H00d,H00f), C00Q(H00g,H00i,H00j), C019(H01a,H01b,H01c), C01C(H01f,
 H01g,H01h), C01D(H01i,H01j,H01k), C01E(H01l,H01m,H01n), C01F(H01o,H01p,H01q),
 C01G(H01r,H01s,H01t), C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C4(H4a,H4b,H4c)
;
_shelx_res_checksum              36064
_olex2_submission_special_instructions 'No special instructions were received'