Dicyclohexano-18-crown-6 hydroxonium tribromide
Muhammad Idiris Saleh; Eny Kusrini; Hoong-Kun Fun; Jeannie Bee-Jan Teh; Acta Crystallographica Section E 63 (2007) o3790–o3791; doi:10.1107/S1600536807039244

data_2215058
_publ_section_title
;
 Dicyclohexano-18-crown-6 hydroxonium tribromide
;
_journal_coeditor_code           CI2434
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3790
_journal_page_last               o3791
_journal_paper_doi               10.1107/S1600536807039244
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H36 O6 , H3 O + , Br3 -'
_chemical_formula_moiety         'C20 H36 O6 , H3 O + , Br3 -'
_chemical_formula_sum            'C20 H39 Br3 O7'
_chemical_formula_weight         631.24
_chemical_name_systematic
;
Dicyclohexano-18-crown-6 hydroxonium tribromide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2703(9)
_cell_length_b                   13.1939(14)
_cell_length_c                   23.363(3)
_cell_measurement_reflns_used    5411
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      1.74
_cell_volume                     2549.3(5)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PLATON (Spek, 2003)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0892
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31119
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.783
_exptl_absorpt_correction_T_max  0.6286
_exptl_absorpt_correction_T_min  0.2475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.812
_refine_ls_abs_structure_details 'Flack (1983), with 2535 Friedel pairs'
_refine_ls_abs_structure_Flack   0.638(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5850
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0578P)^2^+1.0999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                4248
_reflns_number_total             5850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2434.cif
_cod_data_source_block           I
_cod_database_code               2215058
_cod_database_fobs_code          2215058