1,4-Diazabicyclo[2.2.2]octane-based disalts showing non-centrosymmetric structures and phase transition behaviors
Han, Xiang-Bin; Hu, Pan; Shi, Chao; Zhang, Wen; CrystEngComm 18 (2016) 1563–; doi:10.1039/C5CE02066B

data_7224042
_publ_section_title
;
 1,4-Diazabicyclo[2.2.2]octane-based disalts showing non-centrosymmetric
 structures and phase transition behaviors
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1563
_journal_paper_doi               10.1039/C5CE02066B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C6 H14 N2, 2(Cl O4), H2 O'
_chemical_formula_sum            'C6 H16 Cl2 N2 O9'
_chemical_formula_weight         331.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-26 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.357(10)
_cell_length_b                   8.073(7)
_cell_length_c                   11.836(10)
_cell_measurement_reflns_used    8696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.445
_cell_measurement_theta_min      2.948
_cell_volume                     1276.3(18)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8696
_diffrn_reflns_point_group_measured_fraction_full 0.801
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.445
_diffrn_reflns_theta_min         2.948
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       sheet
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 645 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.021(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2917
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.503
_reflns_Friedel_fraction_full    0.591
_reflns_Friedel_fraction_max     0.546
_reflns_number_gt                2087
_reflns_number_total             2917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02066b2.cif
_cod_data_source_block           293
_cod_depositor_comments
'Adding full bibliography for 7224040--7224043.cif.'
_cod_database_code               7224042
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              97649