The [2+2] cycloaddition product of perhalogenated cyclopentadienyl cations: structural characterization of salts of the [C<sub>10</sub>Cl<sub>10</sub>]<sup>2+</sup> and [C<sub>10</sub>Br<sub>10</sub>]<sup>2+</sup> dications.
Rupf, Susanne Margot; Pröhm, Patrick; Malischewski, Moritz; Chemical communications (Cambridge, England) 56 (2020) 9834–9837; doi:10.1039/d0cc04226a

data_7126962
_publ_section_title
;
 The [2+2] cycloaddition product of perhalogenated cyclopentadienyl
 cations: structural characterization of salts of the
 [C<sub>10</sub>Cl<sub>10</sub>]<sup>2+</sup> and
 [C<sub>10</sub>Br<sub>10</sub>]<sup>2+</sup> dications.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9834
_journal_page_last               9837
_journal_paper_doi               10.1039/d0cc04226a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(F16 Sb3), C10 Cl10, 2(Cl F O2 S)'
_chemical_formula_sum            'C10 Cl12 F34 O4 S2 Sb6'
_chemical_formula_weight         2050.12
_chemical_name_systematic        '[C10Cl10][Sb3F16]2'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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_primary     dual
_audit_creation_date             2020-06-15
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8021(4)
_cell_length_b                   19.9917(8)
_cell_length_c                   12.0793(5)
_cell_measurement_reflns_used    9428
_cell_measurement_temperature    102.37
_cell_measurement_theta_max      28.318
_cell_measurement_theta_min      2.654
_cell_volume                     2347.32(17)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      102.37
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            93745
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.338
_exptl_absorpt_correction_T_max  0.4951
_exptl_absorpt_correction_T_min  0.3835
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0909 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.7746.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.901
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: SO2ClF'
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.222
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+3.8218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5673
_reflns_number_total             5828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04226a2.cif
_cod_data_source_block           p21_n
_cod_depositor_comments
'Adding full bibliography for 7126959--7126962.cif.'
_cod_database_code               7126962
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.446
_shelx_estimated_absorpt_t_min   0.314
_olex2_refinement_description
;
1. Others
 Fixed Sof: O00X(0.6) O1(0.6) O1A(0.4) O2(0.4)
;
_shelx_res_checksum              22614
_olex2_submission_special_instructions 'No special instructions were received'