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_7126961
_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         'Br6 C5, 0.5(C4 H6 N2)'
_chemical_formula_sum            'C7 H3 Br6 N'
_chemical_formula_weight         580.56
_chemical_name_systematic        Hexabromocyclopentadien
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-01
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5108(5)
_cell_length_b                   7.1691(4)
_cell_length_c                   21.9711(11)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    103.68
_cell_measurement_theta_max      25.648
_cell_measurement_theta_min      2.989
_cell_volume                     1340.56(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      103.68
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21875
_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         25.693
_diffrn_reflns_theta_min         2.566
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.933
_exptl_absorpt_correction_T_max  0.2483
_exptl_absorpt_correction_T_min  0.0140
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1687 before and 0.1116 after correction.
The Ratio of minimum to maximum transmission is 0.0564.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/acetonirtile'
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.360
_refine_ls_extinction_coef       0.0128(10)
_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   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0785P)^2^+20.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1317
_reflns_number_total             1385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04226a2.cif
_cod_data_source_block           pnma
_cod_depositor_comments
'Adding full bibliography for 7126959--7126962.cif.'
_cod_database_code               7126961
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.162
_shelx_estimated_absorpt_t_min   0.038
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5)
3.a Idealised Me refined as rotating group:
 C00D(H00A,H00B,H00C)
;
_shelx_res_checksum              52654
_olex2_submission_special_instructions 'No special instructions were received'