3,14-Diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane dichloride tetrahydrate from synchrotron radiation
Moon, Dohyun; Subhan, Md Abdus; Choi, Jong-Ha; Acta Crystallographica Section E 69 (2013) o1620–; doi:10.1107/S1600536813027232

data_2238804
_publ_section_title
;
 3,14-Diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
 dichloride tetrahydrate from synchrotron radiation
;
_journal_coeditor_code           TK5261
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1620
_journal_paper_doi               10.1107/S1600536813027232
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C22 H46 N4 2+, 2Cl -, 4H2 O'
_chemical_formula_moiety         'C22 H46 N4 2+, 2(Cl -), 4(H2 O)'
_chemical_formula_sum            'C22 H54 Cl2 N4 O4'
_chemical_formula_weight         509.59
_chemical_name_systematic
;
3,14-Diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
dichloride tetrahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.122(4)
_cell_length_b                   13.616(3)
_cell_length_c                   10.565(2)
_cell_measurement_reflns_used    31113
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      66.38
_cell_measurement_theta_min      1.28
_cell_volume                     2878.7(12)
_computing_cell_refinement       '<i>HKL3000sm</i> (Otwinowski & Minor, 1997)'
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX</i> (Arvai & Nielsen, 1983)
;
_computing_data_reduction        '<i>HKL3000sm</i> (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72000
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13046
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.9224
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000 SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+2.1570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                3446
_reflns_number_total             3663
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5261.cif
_cod_data_source_block           I
_cod_original_cell_volume        2878.5(10)
_cod_database_code               2238804