5,5,7,12,14,14-Hexamethyl-1,8-diaza-4,11-diazoniacyclotetradeca-4,11-diene dichloride trihydrate
Ismail, Wafiuddin; Yamin, Bohari M.; Daran, Jean-Claude; Acta Crystallographica Section E 68 (2012) o1476–o1477; doi:10.1107/S1600536812016649

data_2234660
_publ_section_title
;
 5,5,7,12,14,14-Hexamethyl-1,8-diaza-4,11-diazoniacyclotetradeca-4,11-diene
 dichloride trihydrate
;
_journal_coeditor_code           HG5196
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1476
_journal_page_last               o1477
_journal_paper_doi               10.1107/S1600536812016649
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C16 H34 N4 2+, 2Cl -, 3H2 O'
_chemical_formula_moiety         'C16 H34 N4 2+, 2(Cl -), 3(H2 O)'
_chemical_formula_sum            'C16 H40 Cl2 N4 O3'
_chemical_formula_weight         407.42
_chemical_melting_point_gt       372.1
_chemical_melting_point_lt       372.8
_chemical_name_systematic
;
5,5,7,12,14,14-Hexamethyl-1,8-diaza-4,11-diazoniacyclotetradeca-4,11-diene
dichloride trihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.752(9)
_cell_angle_beta                 86.085(9)
_cell_angle_gamma                71.886(8)
_cell_formula_units_Z            2
_cell_length_a                   8.576(4)
_cell_length_b                   10.735(4)
_cell_length_c                   13.438(6)
_cell_measurement_reflns_used    2072
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.58
_cell_volume                     1128.6(8)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), PARST (Nardelli, 1995) and PLATON
(Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 83.66
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD area-detector
;
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11977
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_correction_T_min  0.8971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                2878
_reflns_number_total             3987
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg5196.cif
_cod_data_source_block           I
_cod_original_cell_volume        1128.7(8)
_cod_database_code               2234660
_cod_database_fobs_code          2234660