Stable Chloro- and Bromoxenate Cage Anions; [X3(XeO3)3](3-) and [X4(XeO3)4](4-) (X = Cl or Br).
Goettel, James T.; Haensch, Veit; Schrobilgen, Gary J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04067

data_4126230
_publ_section_title
;
 Stable Chloro- and Bromoxenate Cage Anions; [X3(XeO3)3](3-) and
 [X4(XeO3)4](4-) (X = Cl or Br).
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04067
_journal_year                    2017
_chemical_formula_sum            'C4 H12 Br N O3 Xe'
_chemical_formula_weight         444.45
_chemical_properties_physical
', Heat-sensitive,Shock sensitive energetic material.'
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-03-25 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.3724(6)
_cell_length_b                   11.6016(7)
_cell_length_c                   18.1066(11)
_cell_measurement_reflns_used    8841
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      39.24
_cell_measurement_theta_min      9.25
_cell_volume                     1938.3(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.944
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28875
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         39.265
_diffrn_reflns_theta_min         9.168
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.640
_exptl_absorpt_correction_T_max  0.5176
_exptl_absorpt_correction_T_min  0.1864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2.0-2 (Bruker, 2005)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         10837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8850
_reflns_number_total             10837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04067_si_002.cif
_cod_data_source_block           JG92_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

2021-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C16 H48 Br4 N4 O12 Xe4'
_cod_original_formula_weight         1333.42
_cod_original_formula_units_Z            2
_cod_database_code               4126230
_shelx_estimated_absorpt_t_min   0.183
_shelx_estimated_absorpt_t_max   0.487
_exptl_absorpt_special_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0428 before and 0.0343 after correction.
The Ratio of minimum to maximum transmission is 0.3601.
The \l/2 correction factor is 0.00150.
;
_shelxl_version_number           2014/6
_shelx_res_checksum              90886
_shelx_hkl_checksum              2846