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_7126959
_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         'Br10 C10, 2(As2 F11), 4(Cl F O2 S)'
_chemical_formula_sum            'C10 As4 Br10 Cl4 F26 O8 S4'
_chemical_formula_weight         2110.92
_chemical_name_systematic        '[C10Br10][As2F11]2'
_chemical_properties_physical    Moisture-sensitive,Heat-sensitive
_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_primary     dual
_audit_creation_date             2020-04-30
_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                68.761(2)
_cell_angle_beta                 74.151(2)
_cell_angle_gamma                75.960(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8126(5)
_cell_length_b                   11.9355(8)
_cell_length_c                   12.5355(8)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    100.09
_cell_measurement_theta_max      26.444
_cell_measurement_theta_min      2.687
_cell_volume                     1166.97(13)
_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      100.09
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0568
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            80540
_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         26.443
_diffrn_reflns_theta_min         2.434
_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    11.948
_exptl_absorpt_correction_T_max  0.5612
_exptl_absorpt_correction_T_min  0.3527
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0892 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.6285.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.004
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: SO2ClF'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00184(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0157P)^2^+8.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4445
_reflns_number_total             4806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04226a2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7126959--7126962.cif.'
_cod_database_code               7126959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.387
_shelx_estimated_absorpt_t_min   0.264
_olex2_refinement_description
;
1. Others
 Fixed Sof: S2(0.6) Cl3(0.6) F2(0.6) S1(0.4) Cl1(0.4) F3(0.4)
;
_shelx_res_checksum              76218
_olex2_submission_special_instructions 'No special instructions were received'