Preparation, structure, and versatile reactivity of pseudocyclic benziodoxole triflate, new hypervalent iodine reagent
Akira Yoshimura; Khiem C. Nguyen; Scott C. Klasen; Akio Saito; Victor N. Nemykin; Viktor V. Zhdankin; Chem.Commun. 51 (2015) 7835–; doi:10.1039/C5cc02009C

data_7117069
_publ_section_title
;
 Preparation, structure, and versatile reactivity of pseudocyclic
 benziodoxole triflate, new hypervalent iodine reagent
;
_journal_name_full               Chem.Commun.
_journal_page_first              7835
_journal_paper_doi               10.1039/C5cc02009C
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration .
_chemical_formula_moiety         'C8 H6 F3 I1 O6 S1'
_chemical_formula_sum            'C8 H6 F3 I O6 S'
_chemical_formula_weight         414.10
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-01-26
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                98.200(7)
_cell_angle_beta                 93.463(7)
_cell_angle_gamma                91.657(7)
_cell_formula_units_Z            2
_cell_length_a                   5.4618(6)
_cell_length_b                   9.7781(11)
_cell_length_c                   11.8765(13)
_cell_measurement_reflns_used    4879
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     626.19(12)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4879
_diffrn_reflns_theta_full        25.333
_diffrn_reflns_theta_max         25.333
_diffrn_reflns_theta_min         3.474
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  2
_diffrn_standards_number         4879
_exptl_absorpt_coefficient_mu    2.781
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.77
_refine_diff_density_min         -4.04
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9851
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.0001059
_refine_ls_shift/su_mean         0.0000048
_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: 
 126. 155. 47.9 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2099
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.2099
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1414
_reflns_number_total             2283
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1351
_oxford_refine_ls_scale          0.839(6)
_oxford_reflns_number_all        2256
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '_09102013-1'
_cod_data_source_file            c5cc02009c3.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scan ' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C8 H6 F3 I1 O6 S1'
_cod_database_code               7117069
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   3,X'S) H   (  32,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE O   (   1,X'S) H   (  11,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;