An arene-stabilized η<sup>5</sup>-pentamethylcyclopentadienyl antimony dication acts as a source of Sb<sup>+</sup> or Sb<sup>3+</sup> cations.
Zhou, Jiliang; Kim, Hyehwang; Liu, Liu Leo; Cao, Levy L.; Stephan, Douglas W.; Chemical communications (Cambridge, England) 56 (2020) 12953–12956; doi:10.1039/d0cc02710c

data_7127291
_publ_section_title
;
 An arene-stabilized \h<sup>5</sup>-pentamethylcyclopentadienyl antimony
 dication acts as a source of Sb<sup>+</sup> or Sb<sup>3+</sup> cations.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12953
_journal_page_last               12956
_journal_paper_doi               10.1039/d0cc02710c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H56 N4 Sb, B C24 F20, C7 H8'
_chemical_formula_sum            'C61 H64 B F20 N4 Sb'
_chemical_formula_weight         1365.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-29 deposited with the CCDC.	2020-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.897(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.218(3)
_cell_length_b                   8.3161(12)
_cell_length_c                   20.922(3)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.44
_cell_measurement_theta_min      2.45
_cell_volume                     3102.5(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    ortep3
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73380
_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         26.371
_diffrn_reflns_theta_min         1.816
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1032 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.9324.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6332
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+3.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5339
_reflns_number_total             6332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02710c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7127289--7127291.cif.'
_cod_original_cell_volume        3102.5(7)
_cod_database_code               7127291
_shelxl_version_number           2014-3
_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. Restrained distances
 C2S-C7S \\sim C6S-C7S
 with sigma of 0.002
3. Rigid bond restraints
 C6S, C5S, C4S, C3S, C2S, C1S, C7S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C6S \\sim C5S \\sim C4S \\sim C3S \\sim C2S \\sim C1S \\sim C7S: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C6S(0.5) H6S(0.5) C5S(0.5) H5S(0.5) C4S(0.5) H4S(0.5) C3S(0.5)
 H3S(0.5) C2S(0.5) H2S(0.5) C1S(0.5) C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C7(H7), C10(H10), C4(H4)
6.b Aromatic/amide H refined with riding coordinates:
 C6S(H6S), C5S(H5S), C4S(H4S), C3S(H3S), C2S(H2S)
6.c Fitted hexagon refined as free rotating group:
 C6S(C5S,C4S,C3S,C2S,C1S)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C11(H11A,H11B,
 H11C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C),
 C7S(H7SA,H7SB,H7SC)
;
_shelx_res_checksum              69162
_shelx_hkl_checksum              59986
_olex2_submission_special_instructions 'No special instructions were received'