A perchlorate salt of an octaprotonated cryptand
McKee, Vickie; Morgan, Grace G.; Acta Crystallographica Section C 59 (2003) o150–o152; doi:10.1107/S0108270103002580

data_2013116
_publ_section_title
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 A perchlorate salt of an octaprotonated cryptand
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_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o150
_journal_page_last               o152
_journal_paper_doi               10.1107/S0108270103002580
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C33 H59 N11 8+, 8Cl O4 1-, 5H2 O'
_chemical_formula_moiety         'C33 H59 N11 8+, 8Cl O4 1-, 5H2 O'
_chemical_formula_sum            'C33 H69 Cl8 N11 O37'
_chemical_formula_weight         1495.59
_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           SHELXL97
_cell_angle_alpha                84.258(9)
_cell_angle_beta                 76.394(8)
_cell_angle_gamma                65.092(8)
_cell_formula_units_Z            2
_cell_length_a                   12.9265(13)
_cell_length_b                   13.6798(14)
_cell_length_c                   18.5310(19)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4.5
_cell_volume                     2888.7(6)
_computing_cell_refinement       'XSCANS (Siemens, 1990a)'
_computing_data_collection       'XSCANS (Siemens, 1990a)'
_computing_data_reduction        'XSCANS (Siemens, 1990a)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      128(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w 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  0.105
_diffrn_reflns_av_sigmaI/netI    0.036
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9513
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(SHELXTL/PC; Siemens, 1990b)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         9055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0435
_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^)+(0.058P)^2^+4.792P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                7315
_reflns_number_total             9055
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1519.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               2013116
_cod_database_fobs_code          2013116