Non-classical polyinterhalides of chlorine monofluoride: experimental and theoretical characterization of [F(ClF)<sub>3</sub>]<sup/>.
Pröhm, Patrick; Schwarze, Nico; Müller, Carsten; Steinhauer, Simon; Beckers, Helmut; Rupf, Susanne M.; Riedel, Sebastian; Chemical communications (Cambridge, England) 57 (2021) 4843–4846; doi:10.1039/d1cc01088c

data_7128151
_publ_section_title
;
 Non-classical polyinterhalides of chlorine monofluoride: experimental and
 theoretical characterization of [F(ClF)<sub>3</sub>]<sup/>.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4843
_journal_page_last               4846
_journal_paper_doi               10.1039/d1cc01088c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '3(Cl F), F, C4 H12 N'
_chemical_formula_sum            'C4 H12 Cl3 F4 N'
_chemical_formula_weight         256.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8381(2)
_cell_length_b                   10.0385(2)
_cell_length_c                   9.3211(2)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      71.919
_cell_measurement_theta_min      4.404
_cell_volume                     1107.69(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17449
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.239
_diffrn_reflns_theta_min         5.779
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.675
_exptl_absorpt_correction_T_max  0.2261
_exptl_absorpt_correction_T_min  0.0832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1304 before and 0.0697 after correction. The Ratio of minimum to maximum transmission is 0.3680. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.296
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.495(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2178
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0296P)^2^+0.1596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2147
_reflns_number_total             2178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01088c2.cif
_cod_data_source_block           pp278_multabs_a
_cod_depositor_comments
'Adding full bibliography for 7128150--7128151.cif.'
_cod_database_code               7128151
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.210
_shelx_estimated_absorpt_t_min   0.102
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.505(15)
 0.495(15)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              51177
_olex2_submission_special_instructions 'No special instructions were received'