Tris(<i>cis</i>-2-hydroxycyclohexane-1,3,5-triaminium) hydrogen sulfate octachloride dihydrate
Neis, Christian; Merten, Günter J.; Hegetschweiler, Kaspar; Acta Crystallographica Section E 68 (2012) o1899–o1900; doi:10.1107/S1600536812022374

data_2235182
_publ_section_title
;
 Tris(<i>cis</i>-2-hydroxycyclohexane-1,3,5-triaminium) hydrogen sulfate
 octachloride dihydrate
;
_journal_coeditor_code           NK2161
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1899
_journal_page_last               o1900
_journal_paper_doi               10.1107/S1600536812022374
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '3C6 H18 N3 O 3+, 8Cl -, H S O4 -, 2H2 O'
_chemical_formula_moiety
'3(C6 H18 N3 O 3+), 8(Cl -), H O4 S -, 2(H2 O)'
_chemical_formula_sum            'C18 H59 Cl8 N9 O9 S'
_chemical_formula_weight         861.40
_chemical_name_systematic
;
Tris(<i>cis</i>-2-hydroxycyclohexane-1,3,5-triaminium) hydrogen sulfate
octachloride dihydrate
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.6549(18)
_cell_length_b                   12.6549(18)
_cell_length_c                   43.616(9)
_cell_measurement_reflns_used    5824
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      38.04
_cell_measurement_theta_min      3.25
_cell_volume                     6049.1(17)
_computing_cell_refinement       'Stoe IPDS Software (Stoe & Cie, 1997)'
_computing_data_collection       'Stoe IPDS Software (Stoe & Cie, 1997)'
_computing_data_reduction        'Stoe IPDS Software (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS image plate'
_diffrn_measurement_method       'phi scans'
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            14259
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2724
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.319
_refine_ls_abs_structure_details 'Flack (1983), 1255 Friedel pairs'
_refine_ls_abs_structure_Flack   0.41(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2518
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          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^)+(0.0782P)^2^+1.7412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                2442
_reflns_number_total             2518
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nk2161.cif
_cod_data_source_block           I
_cod_original_cell_volume        6049.2(17)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               2235182
_cod_database_fobs_code          2235182