Hydronium perchlorate–dibenzo-18-crown-6 (1/1): monoclinic polymorph
Pojarová, Michaela; Fejfarová, Karla; Makrlík, Emanuel; Acta Crystallographica Section E 66 (2010) o3341–o3342; doi:10.1107/S1600536810048622

data_2228359
_publ_section_title
;
 Hydronium perchlorate--dibenzo-18-crown-6 (1/1): monoclinic polymorph
;
_journal_coeditor_code           HB5736
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3341
_journal_page_last               o3342
_journal_paper_doi               10.1107/S1600536810048622
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'H3 O +, Cl O4 -, C20 H24 O6'
_chemical_formula_moiety         'H3 O +, Cl O4 -, C20 H24 O6'
_chemical_formula_sum            'C20 H27 Cl O11'
_chemical_formula_weight         478.9
_chemical_name_systematic
;
Hydronium perchlorate--dibenzo-18-crown-6 (1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 100.0011(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.65860(10)
_cell_length_b                   26.7718(3)
_cell_length_c                   19.1518(2)
_cell_measurement_reflns_used    20984
_cell_measurement_temperature    123.9
_cell_measurement_theta_max      62.4718
_cell_measurement_theta_min      3.2989
_cell_volume                     4372.05(8)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'Crysalis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      123.9
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method       'rotation method data acquisition using \w'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36184
_diffrn_reflns_theta_full        62.56
_diffrn_reflns_theta_max         62.56
_diffrn_reflns_theta_min         3.3
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.4546
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.07
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    198
_refine_ls_number_parameters     595
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0221
_refine_ls_shift/su_mean         0.0012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(I)+0.0016I^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                5283
_reflns_number_total             6865
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hb5736.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228359
_cod_database_fobs_code          2228359