Comment on “1,4-Diazabicyclo[2.2.2]octane-based disalts showing non-centrosymmetric structures and phase transition behaviors” by X.-B. Han, P. Hu, C. Shi and W. Zhang, CrystEngComm, 2016, 18, 1563
Szafrański, Marek; CrystEngComm 19 (2017) 179–; doi:10.1039/C6CE01469K

data_7227250
_publ_section_title
;
 Comment on &#x201C;1,4-Diazabicyclo[2.2.2]octane-based disalts showing
 non-centrosymmetric structures and phase transition behaviors&#x201D; by
 X.-B. Han, P. Hu, C. Shi and W. Zhang, CrystEngComm, 2016, 18, 1563
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              179
_journal_paper_doi               10.1039/C6CE01469K
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         '2(Cl O4), C6 H14 N2, H2 O'
_chemical_formula_sum            'C6 H16 Cl2 N2 O9'
_chemical_formula_weight         331.11
_chemical_name_common            'dabco diperchlorate monohydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-09-01 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.9946(15)
_cell_angle_beta                 90.0068(15)
_cell_angle_gamma                89.9829(15)
_cell_formula_units_Z            4
_cell_length_a                   8.02169(15)
_cell_length_b                   11.7137(2)
_cell_length_c                   13.2529(2)
_cell_measurement_reflns_used    26839
_cell_measurement_temperature    200.0(1)
_cell_measurement_theta_max      30.1230
_cell_measurement_theta_min      2.3340
_cell_volume                     1245.29(4)
_computing_cell_refinement       CrysAlisRED
_computing_data_collection       CrysAlisCCD
_computing_data_reduction        CrysAlisRED
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.329
_diffrn_reflns_theta_min         2.320
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 6270 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.479(8)
_refine_ls_extinction_coef       0.0029(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         13523
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0344P)^2^+0.0476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                13218
_reflns_number_total             13523
_cod_data_source_file            c6ce01469k2.cif
_cod_data_source_block           D_2ClO4_H2O_200
_cod_depositor_comments
'Adding full bibliography for 7227245--7227250.cif.'
_cod_database_code               7227250
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4755(9) 0.5245(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
3. Restrained distances
 H3C-H3D
 1.35 with sigma of 0.005
 H1C-O1
 0.86 with sigma of 0.005
 O1-H1D
 0.86 with sigma of 0.005
 O2-H2C
 0.86 with sigma of 0.005
 O2-H2D
 0.86 with sigma of 0.005
 H2C-H2D
 1.35 with sigma of 0.005
 O4-H4C
 0.86 with sigma of 0.005
 O4-H4D
 0.86 with sigma of 0.005
 H4C-H4D
 1.35 with sigma of 0.005
 H3C-O3
 0.86 with sigma of 0.005
 O3-H3D
 0.86 with sigma of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
;
_shelx_res_checksum              37233
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'