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_4302218
_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         'C24 H22 I4 O11 S2'
_chemical_formula_sum            'C24 H22 I4 O11 S2'
_chemical_formula_weight         1058.18
_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
_audit_creation_date             05-05-26
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                114.221(4)
_cell_angle_beta                 111.995(4)
_cell_angle_gamma                91.960(4)
_cell_formula_units_Z            2
_cell_length_a                   10.707(3)
_cell_length_b                   12.529(4)
_cell_length_c                   13.899(4)
_cell_measurement_reflns_used    256
_cell_measurement_temperature    193
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1537.2(8)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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      193
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART'
_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  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18416
_diffrn_reflns_theta_full        26.661
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         1.776
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.245
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.16
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.286
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.33
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8633
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     140
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.000816
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 16.2 18.9 10.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0399
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0376
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5809
_reflns_number_total             6977
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.29410(8)
_oxford_structure_analysis_title 'XYZN file = SHELXL INS file, from DIRDIF out'
_cod_data_source_file            ic900282k_si_001.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4302218