Investigations of the polyiodides H3O·Ix (x = 3, 5 or 7) as dibenzo-18-crown-6 complexes
Kloo, Lars; Svensson, Per H.; Taylor, Michael J.; Journal of the Chemical Society, Dalton Transactions  (2000) 1061–; doi:10.1039/a908053h

data_7009011
_publ_contact_author
;
 Lars Kloo
 Inorganic Chemistry, Department of Chemistry, 
Royal Institute of Chemistry, S-1044 Stockholm, Sweden
;
_publ_section_title
;
 Investigations of the polyiodides H3O&#x00B7;Ix (x&#x2005;=&#x2005;3,
 5 or 7) as dibenzo-18-crown-6 complexes
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1061
_journal_paper_doi               10.1039/a908053h
_journal_year                    2000
_chemical_formula_sum            'C20 H27 I5 O7'
_chemical_formula_weight         1013.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Mon Apr 27 12:39:39 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 97.59(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2508(8)
_cell_length_b                   24.949(5)
_cell_length_c                   14.224(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     2902.3(14)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_orient_matrix_UB_11      -0.02572
_diffrn_orient_matrix_UB_12      -0.00902
_diffrn_orient_matrix_UB_13      -0.06884
_diffrn_orient_matrix_UB_21      -0.02748
_diffrn_orient_matrix_UB_22      0.03841
_diffrn_orient_matrix_UB_23      -0.01454
_diffrn_orient_matrix_UB_31      0.11631
_diffrn_orient_matrix_UB_32      0.00710
_diffrn_orient_matrix_UB_33      -0.00885
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6583
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        -7.95
_diffrn_standards_interval_count '120 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.394
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_description       rectangular
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_refine_diff_density_max         1.15
_refine_diff_density_min         -1.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.559
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2126
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.0007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0374
_reflns_number_observed          2126
_reflns_number_total             6158
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            a908053h.txt
_cod_data_source_block           '[H3O(dibenzo-18-crown-6)][I5]'
_cod_depositor_comments
;
Automatic conversion scripts had previously changed
'_atom_site_refinement_flags' tag values 'd' into 'D' as recommended by
'cif_core.dic' version 2.4.1. However, manual inspection revealed that the
underlying problem was actually related to a wrong tag names inside the 
atom site loop. '_atom_site_calc_flag' tag and '_atom_site_refinement_flags' 
tag were switched after consulting the original paper.

Antanas Vaitkus,
2015-03-28
;
_cod_original_cell_volume        2902(1)
_cod_original_sg_symbol_H-M      'P 21/a     '
_cod_database_code               7009011