Self-Assembly of Hydroxy(phenyl)iodonium Ions in Acidic Aqueous Solution: Preparation, and X-ray Crystal Structures of Oligomeric Phenyliodine(III) Sulfates
Victor N. Nemykin; Alexey Y. Koposov; Brian C. Netzel; Mekhman S. Yusubov; Viktor V. Zhdankin; Inorganic Chemistry 48 (2009) 4908–4917; doi:10.1021/ic900282k

data_4302219
_publ_contact_author_address
; 
 Department of Chemistry, 
 University of Minnesota Duluth, 
 1039 University Drive, 
 Duluth, MN, 55812. 
;
_publ_contact_author_email       vnemykin@d.umn.edu
_publ_contact_author_fax         '+1 218 7267394'
_publ_contact_author_name        'Victor N. Nemykin'
_publ_contact_author_phone       '+1 218 7266729'
_publ_section_title
;
Self-Assembly of Hydroxy(phenyl)iodonium Ions in Acidic Aqueous Solution:
Preparation, and X-ray Crystal Structures of Oligomeric Phenyliodine(III)
Sulfates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4908
_journal_page_last               4917
_journal_paper_doi               10.1021/ic900282k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C16 H16 I2 O5'
_chemical_formula_sum            'C16 H16 I2 O5'
_chemical_formula_weight         542.11
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-06-01
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 107.36(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.946(4)
_cell_length_b                   9.383(3)
_cell_length_c                   17.097(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     1829.1(10)
_computing_cell_refinement       'Win AFC'
_computing_data_collection       'Win AFC'
_computing_data_reduction        'TeXsan 10.3.b'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4458
_diffrn_reflns_theta_full        27.521
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         2.504
_diffrn_standards_decay_%        92.70
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.459
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al, 1968) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         5.04
_refine_diff_density_min         -2.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3556
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1738
_refine_ls_R_factor_gt           0.1249
_refine_ls_shift/su_max          0.000039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ 
 Method = SHELXL 97 (Sheldrick, 1997) 
 W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] 
 P(i) are: 
 0.200 0.00 0.00 0.00 0.00 0.333 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         2.5011
_refine_ls_wR_factor_gt          0.3041
_refine_ls_wR_factor_ref         0.3041
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2532
_reflns_number_total             4196
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2644(11)
_oxford_structure_analysis_title 'XYZN file = SHELXL INS file, from DIRDIF out'
_cod_data_source_file            ic900282k_si_002.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4302219