2-Iodylphenol Ethers: Preparation, X-ray Crystal Structure, and Reactivity of New Hypervalent Iodine(V) Oxidizing Reagents
Alexey Y. Koposov; Rashad R. Karimov; Ivan M. Geraskin; Victor N. Nemykin; Viktor V. Zhdankin; Journal of Organic Chemistry 71 (2006) 8452–8458; doi:10.1021/jo0614947

data_4022047
_publ_section_title
;
 2-Iodylphenol Ethers: Preparation, X-ray Crystal Structure,
 and Reactivity of New Hypervalent Iodine(V) Oxidizing Reagents
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8452
_journal_page_last               8458
_journal_paper_doi               10.1021/jo0614947
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C9 H11 I1 O3'
_chemical_formula_sum            'C9 H11 I O3'
_chemical_formula_weight         294.09
_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             05-02-04
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 102.746(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2665(15)
_cell_length_b                   13.0901(15)
_cell_length_c                   12.7349(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18
_cell_measurement_theta_min      15
_cell_volume                     1018.9(3)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Unknown
_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       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2444
_diffrn_reflns_theta_full        27.488
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         3.112
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.116
_exptl_absorpt_correction_T_max  0.39
_exptl_absorpt_correction_T_min  0.29
_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    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.73
_refine_diff_density_min         -1.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8219
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2121
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001338
_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: 
 259. 431. 276. 119. 33.5 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1051
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1031
_reflns_limit_h_max              7
_reflns_limit_h_min              -8
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2121
_reflns_number_total             2334
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            jo0614947si20060821_114101.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_H-M      'P 21/c'
_cod_original_formula_sum        'C9 H11 I1 O3'
_cod_database_code               4022047