Crystal structure of 3,14-dimethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane bis(perchlorate) from synchrotron X-ray data
Moon, Dohyun; Jeon, Sunghwan; Choi, Jong-Ha; Acta Crystallographica Section E 77 (2021) 551–554; doi:10.1107/S2056989021004278

data_2243812
_publ_section_title
;
 Crystal structure of
 3,14-dimethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
 bis(perchlorate) from synchrotron X-ray data
;
_journal_coeditor_code           VM2247
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              551
_journal_page_last               554
_journal_paper_doi               10.1107/S2056989021004278
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C20 H42 N4 2+, 2Cl O4 -'
_chemical_formula_moiety         'C20 H42 N4 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C20 H42 Cl2 N4 O8'
_chemical_formula_weight         537.47
_chemical_name_systematic
;
3,14-Dimethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
bis(perchlorate)
;
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.689(2)
_cell_length_b                   8.4450(17)
_cell_length_c                   14.020(3)
_cell_measurement_reflns_used    41946
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1263.9(4)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i> (Shin <i>et al.</i>,  2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND 4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12842
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm</i> Scalepack; Otwinowski <i>et al.</i>,  2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.443
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0553
_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^)+(0.1016P)^2^+0.4023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1719
_reflns_number_gt                3164
_reflns_number_total             3549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2247sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243812
_cod_database_fobs_code          2243812
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              3195
_shelx_res_checksum              57002