Preparation and x-ray Structural Study of 1-Arylbenziodoxolones
Mekhman S. Yusubov; Roza Y. Yusubova; Victor N. Nemykin; Viktor V. Zhdankin; Journal of Organic Chemistry 78 (2013) 3767–3773; doi:10.1021/jo400212u

data_4028183
_publ_contact_author_address
; 
 Department of Chemistry of Chemistry & Biochemistry, 
 University of Minnesota Duluth,
 1039 University Drive 
 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 Structural Study of 1-Arylbenziodoxolones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3767
_journal_page_last               3773
_journal_paper_doi               10.1021/jo400212u
_journal_volume                  78
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H15 I1 O2'
_chemical_formula_sum            'C16 H15 I O2'
_chemical_formula_weight         366.20
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-01-16
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.6678(14)
_cell_length_b                   11.6678(14)
_cell_length_c                   9.4235(6)
_cell_measurement_reflns_used    1694
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     1111.0(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.049
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6159
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.492
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  1
_diffrn_standards_number         1694
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.370
_refine_diff_density_max         1.74
_refine_diff_density_min         -2.41
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3346
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.0001802
_refine_ls_shift/su_mean         0.0000087
_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: 
 104. 129. 38.4 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0921
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0921
_reflns_limit_h_max              7
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_gt                2416
_reflns_number_total             3374
_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   0.0876
_oxford_refine_ls_scale          1.257(4)
_oxford_reflns_number_all        3346
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            jo400212u_si_002_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 31 '
_cod_original_formula_sum        'C16 H15 I1 O2'
_cod_database_code               4028183