A dicationic distibine stabilized by intramolecular π–π interaction and second-sphere coordination
Zhang, Lingjie; Huang, Minghao; Zhou, Jiliang; Chemical Communications 61 (2025) 8592–8595; doi:10.1039/D5CC01730K

data_7134521
_publ_section_title
;
 A dicationic distibine stabilized by intramolecular \p--\p interaction
 and second-sphere coordination
;
_journal_issue                   47
_journal_name_full               'Chemical Communications'
_journal_page_first              8592
_journal_page_last               8595
_journal_paper_doi               10.1039/D5CC01730K
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C24 H25 N4 Sb, 1.5(C7 H8), F6 P'
_chemical_formula_sum            'C34.5 H37 F6 N4 P Sb'
_chemical_formula_weight         774.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-12-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-03-07 deposited with the CCDC.	2025-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.8847(5)
_cell_length_b                   14.7666(4)
_cell_length_c                   23.3770(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.54
_cell_volume                     6820.2(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      153.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103272
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.878
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0840 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.8948.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6990
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+13.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6666
_reflns_number_total             6990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01730k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7134519--7134521.cif.'
_cod_original_formula_sum        'C34.50 H37 F6 N4 P Sb'
_cod_database_code               7134521
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.608
_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. Restrained distances
 P1-F3 \\sim P1-F6
 with sigma of 0.005
 P2-F14 \\sim P2-F15
 with sigma of 0.005
 P2-F16 \\sim P2-F15
 with sigma of 0.005
 F13-F14 \\sim F13-F11
 with sigma of 0.005
3. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F5(0.5) F6(0.5) F4(0.5) P2(0.5) F11(0.5)
 F12(0.5) F13(0.5) F15(0.5) F16(0.5) F14(0.5) C1S(0.5) H1S(0.5) C6S(0.5)
 C5S(0.5) H5S(0.5) C3S(0.5) H3S(0.5) C4S(0.5) H4S(0.5) C2S(0.5) H2S(0.5)
 C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C16(H16), C3(H3), C22(H22), C5(H5), C9(H9), C19(H19), C10(H10),
 C11(H11), C20(H20), C4(H4), C12(H12), C21(H21), C29(H29), C25(H25), C26(H26),
 C30(H30), C28(H28), C1S(H1S), C5S(H5S), C3S(H3S), C4S(H4S), C2S(H2S)
4.b Fitted hexagon refined as free rotating group:
 C1S(C6S,C5S,C3S,C4S,C2S)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C15(H15A,H15B,
 H15C), C31(H31A,H31B,H31C), C7S(H7SA,H7SB,H7SC)
;
_shelx_res_checksum              87145
_shelx_hkl_checksum              52106
_olex2_submission_special_instructions 'No special instructions were received'