Crystal structure of 3,14-dimethyl-2,6,13,17-tetraazoniatricyclo[16.4.0.07,12]docosane tetrachloride tetrahydrate from synchrotron X-ray data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E Crystallographic Communications 74 (2018) 1039–; doi:10.1107/S2056989018009337

data_2021177
_publ_section_title
;
 Crystal structure of
 3,14-dimethyl-2,6,13,17-tetraazoniatricyclo[16.4.0.07,12]docosane
 tetrachloride tetrahydrate from synchrotron X-ray data
;
_journal_coeditor_code           SJ5559
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1039
_journal_paper_doi               10.1107/S2056989018009337
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C20 H44 N4 4+, 4Cl -, 4H2 O'
_chemical_formula_moiety         'C20 H44 N4 4+, 4(Cl -), 4(H2 O)'
_chemical_formula_sum            'C20 H52 Cl4 N4 O4'
_chemical_formula_weight         554.45
_chemical_name_systematic
;
3,14-Dimethyl-2,6,13,17-tetraazoniatricyclo[16.4.0.0^7,12^]docosane
tetrachloride tetrahydrate
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 103.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5450(15)
_cell_length_b                   23.190(5)
_cell_length_c                   8.3370(17)
_cell_measurement_reflns_used    44298
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1419.5(5)
_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</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2015</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2015</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13816
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_min         1.557
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0863P)^2^+0.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                3504
_reflns_number_total             3797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5559sup1.cif
_cod_data_source_block           I
_cod_database_code               2021177
_cod_database_fobs_code          2021177
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              85779
_shelx_res_checksum              3839