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_4326789
_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 H4 B1 F4 I1 O4'
_chemical_formula_sum            'C8 H4 B F4 I O4'
_chemical_formula_weight         377.82
_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
_cell_angle_alpha                77.436(6)
_cell_angle_beta                 81.887(6)
_cell_angle_gamma                71.565(5)
_cell_formula_units_Z            4
_cell_length_a                   9.0868(4)
_cell_length_b                   10.3720(5)
_cell_length_c                   12.5120(8)
_cell_measurement_reflns_used    4988
_cell_measurement_temperature    123
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1088.59(11)
_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      123
_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
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28579
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.006
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  4
_diffrn_standards_number         4988
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.04
_refine_diff_density_min         -2.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9801
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4977
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.0003327
_refine_ls_shift/su_mean         0.0000098
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +14.33P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0941
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0941
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3816
_reflns_number_total             4988
_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   0.0578
_oxford_refine_ls_scale          0.3291(3)
_oxford_reflns_number_all        4977
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '_060210_VZ1'
_cod_data_source_file            ic201922n_si_001_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C8 H4 B1 F4 I1 O4'
_cod_database_code               4326789
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   2,X'S) H   (  21,X'S) 
RIDE O   (   6,X'S) H   (  62,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  12,X'S) H   ( 121,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                                                                             
;