Preparation and X-ray Crystal Study of Benziodoxaborole Derivatives: New Hypervalent Iodine Heterocycles
Victor N. Nemykin; Andrey V. Maskaev; Margarita R. Geraskina; Mekhman S. Yusubov; Viktor V. Zhdankin; Inorganic Chemistry 50 (2011) 11263–11272; doi:10.1021/ic201922n

data_4326787
_publ_contact_author_address
; 
 Department of Chemistry & Biochemistry, 
 1039 University Drive,
 University of Minnesota Duluth, 
 Duluth, MN 55812, USA. 
;
_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
;
 Preparation and X-ray Crystal Study of Benziodoxaborole Derivatives: New
 Hypervalent Iodine Heterocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11263
_journal_page_last               11272
_journal_paper_doi               10.1021/ic201922n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C8 H5 B1 F3 I1 O4'
_chemical_formula_sum            'C8 H5 B F3 I O4'
_chemical_formula_weight         359.83
_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             10-06-07
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90.851(6)
_cell_angle_beta                 90.094(6)
_cell_angle_gamma                105.522(7)
_cell_formula_units_Z            2
_cell_length_a                   5.1165(3)
_cell_length_b                   7.9571(5)
_cell_length_c                   13.7918(9)
_cell_measurement_reflns_used    2482
_cell_measurement_temperature    298
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     540.95(6)
_computing_cell_refinement       'CrystalClear 2.0'
_computing_data_collection       'CrystalClear 2.0'
_computing_data_reduction        'CrystalStructure 4.0'
_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       'Rigaku RAPID II'
_diffrn_measurement_device_type  'Image Plate'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13990
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.020
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.209
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.95
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0211
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.0001383
_refine_ls_shift/su_mean         2.0542607
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.80P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0821
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0821
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2157
_reflns_number_total             2482
_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   0.0375
_oxford_refine_ls_scale          1.161(4)
_oxford_reflns_number_all        2478
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '_060510_VZ1'
_cod_data_source_file            ic201922n_si_001_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C8 H5 B1 F3 I1 O4'
_cod_database_code               4326787