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_7127290
_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         'C20 H16 N4 Sb, 3(C F3 O3 S), 0.5(C4 H10 O)'
_chemical_formula_sum            'C25 H21 F9 N4 O9.5 S3 Sb'
_chemical_formula_weight         918.39
_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             2020-03-17
_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                81.615(2)
_cell_angle_beta                 86.390(2)
_cell_angle_gamma                84.352(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1010(4)
_cell_length_b                   13.2750(6)
_cell_length_c                   13.8328(6)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.25
_cell_volume                     1643.32(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26237
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0488 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.9380.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.212
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0551P)^2^+2.4929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6611
_reflns_number_total             7241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02710c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7127289--7127291.cif.'
_cod_original_formula_sum        'C25 H21 F9 N4 O9.50 S3 Sb'
_cod_database_code               7127290
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1S-C2S \\sim O1S-C3S
 with sigma of 0.005
 C1S-C2S \\sim C3S-C4S
 with sigma of 0.005
 O1S-C4S \\sim O1S-C1S
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O1S \\sim C1S \\sim C2S \\sim C3S \\sim C4S: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
F1A \\sim F2A \\sim F3A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
F1B \\sim F2B \\sim F3B: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(O1S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C2S) \\sim Ueq, Uanis(C3S)
\\sim Ueq, Uanis(C4S) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
: with sigma of 0.005 and sigma for terminal atoms of 0.01
: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Fixed Sof: O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              12738
_shelx_hkl_checksum              37992
_olex2_submission_special_instructions 'No special instructions were received'