Crystal structure of 3,14-diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane dinitrate dihydrate from synchrotron X-ray data
Moon, Dohyun; Jeon, Sunghwan; Ryoo, Keon Sang; Choi, Jong-Ha; Acta Crystallographica Section E 75 (2019) 921–924; doi:10.1107/S2056989019007655

data_2242964
_publ_section_title
;
 Crystal structure of
 3,14-diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
 dinitrate dihydrate from synchrotron X-ray data
;
_journal_coeditor_code           SJ5572
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              921
_journal_page_last               924
_journal_paper_doi               10.1107/S2056989019007655
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C22 H46 N4 2+, 2N O3 -, 2H2 O'
_chemical_formula_moiety         'C22 H46 N4 2+, 2(N O3 -), 2H2 O'
_chemical_formula_sum            'C22 H50 N6 O8'
_chemical_formula_weight         526.68
_chemical_name_systematic
;
3,14-Diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
dinitrate dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 96.46(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6420(17)
_cell_length_b                   16.687(3)
_cell_length_c                   9.7340(19)
_cell_measurement_reflns_used    46866
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     1394.8(5)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC Program</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 0.976
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14284
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.035
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.069
_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            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.555
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1295P)^2^+0.2454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                2968
_reflns_number_total             3736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5572sup1.cif
_cod_data_source_block           I
_cod_database_code               2242964
_cod_database_fobs_code          2242964
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              62235
_shelx_res_checksum              14716