Three new quinuclidine-based structures: second harmonic generation response for 1,2-bis(1-azoniabicyclo[2.2.2]octan-3-ylidene)hydrazine dichloride
Qiao, Liang; Chen, Xiao-Gang; Gao, Ji-Xing; Ai, Yong; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619005898

data_2021642
_publ_section_title
;
 Three new quinuclidine-based structures: second harmonic generation
 response for 1,2-bis(1-azoniabicyclo[2.2.2]octan-3-ylidene)hydrazine
 dichloride
;
_journal_coeditor_code           QS3081
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619005898
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C14 H24 N4 2+, 2Cl -'
_chemical_formula_moiety         'C14 H24 N4 2+, 2(Cl -)'
_chemical_formula_sum            'C14 H24 Cl2 N4'
_chemical_formula_weight         319.27
_chemical_name_systematic
;
1,2-Bis(1-azoniabicyclo[2.2.2]oct-3-ylidene)hydrazine dichloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.023(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1699(3)
_cell_length_b                   12.5258(7)
_cell_length_c                   10.6570(5)
_cell_measurement_reflns_used    2739
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8980
_cell_measurement_theta_min      3.2600
_cell_volume                     802.42(7)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2000)
;
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;
SHELXL2014 (Sheldrick, 2015b)
;
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;
SHELXL2014 (Sheldrick, 2015b)
;
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SHELXT (Sheldrick, 2015a)
;
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_diffrn_measured_fraction_theta_max 0.797
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_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5076
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.642
_diffrn_reflns_theta_min         2.548
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2005)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       bar
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.173
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 986 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   0.997
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4949
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0517P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                2820
_reflns_number_total             4949
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           PC
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_shelx_hkl_checksum              17512
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