Secondary Hypervalent I(III)...O Interactions: Synthesis and Structure of Hypervalent Complexes of Diphenyl-λ3-iodanes with 18-Crown-6
Masahito Ochiai; Takashi Suefuji; Kazunori Miyamoto; Norihiro Tada; Satoru Goto; Motoo Shiro; Shigeru Sakamoto; Kentaro Yamaguchi; Journal of the American Chemical Society 125 (2003) 769–773; doi:10.1021/ja0211205

data_4113391
_publ_section_title
;
 Secondary Hypervalent I(III)...O Interactions: Synthesis and Structure of
 Hypervalent Complexes of Diphenyl-\l3-iodanes with 18-Crown-6
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              769
_journal_page_last               773
_journal_paper_doi               10.1021/ja0211205
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety
'C10 H10 I 1+, C12 H24 O6, B F4 1-, 1.5(H2 O)'
_chemical_formula_sum            'C24 H37 B F4 I O7.5'
_chemical_formula_weight         659.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Tue Aug 27 16:24:06 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 101.446(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.544(1)
_cell_length_b                   21.210(2)
_cell_length_c                   14.297(2)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    113.2
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      2.4
_cell_volume                     2836.6(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXsan (MSC & Rigaku, 1999)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_refinement  'teXsan (MSC & Rigaku, 1999)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9821
_diffrn_measured_fraction_theta_max 0.9821
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25918
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1340.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.06
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     353
_refine_ls_number_reflns         8137
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.0014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                5561
_reflns_number_total             8141
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja0211205_s2.cif
_cod_data_source_block           RGK629raplt_Tokushima_Univ
_cod_original_cell_volume        2836.7(6)
_cod_original_formula_sum        'C24 H37 B F4 I O7.50 '
_cod_database_code               4113391