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_7224041
_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(B F4), H2 O'
_chemical_formula_sum            'C6 H16 B2 F8 N2 O'
_chemical_formula_weight         305.83
_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                   13.231(10)
_cell_length_b                   7.883(7)
_cell_length_c                   11.786(10)
_cell_measurement_reflns_used    6680
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      6.54
_cell_volume                     1229.3(18)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7954
_diffrn_reflns_point_group_measured_fraction_full 0.828
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.188
_diffrn_reflns_theta_min         6.536
_exptl_absorpt_coefficient_mu    1.714
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 644 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_extinction_coef       0.016(4)
_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   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         1860
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0781P)^2^+0.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.595
_reflns_Friedel_fraction_full    0.654
_reflns_Friedel_fraction_max     0.650
_reflns_number_gt                1805
_reflns_number_total             2255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02066b2.cif
_cod_data_source_block           296
_cod_depositor_comments
'Adding full bibliography for 7224040--7224043.cif.'
_cod_original_cell_volume        1229.3(17)
_cod_database_code               7224041
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              10732