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_4028181
_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_formula_moiety         'C17.25 H21 I1 O3.75'
_chemical_formula_sum            'C17.25 H21 I O3.75'
_chemical_formula_weight         415.26
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_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             13-01-17
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                103.013(7)
_cell_angle_beta                 106.063(8)
_cell_angle_gamma                108.802(8)
_cell_formula_units_Z            8
_cell_length_a                   11.4401(4)
_cell_length_b                   17.2638(6)
_cell_length_c                   20.1815(14)
_cell_measurement_reflns_used    15576
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3402.5(5)
_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  0.053
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_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_full        27.483
_diffrn_reflns_theta_max         27.483
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_diffrn_standards_decay_%        0.00
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_exptl_absorpt_coefficient_mu    1.896
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_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
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_exptl_crystal_description       block
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         15541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.0009670
_refine_ls_shift/su_mean         0.0000202
_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: 
 10.5 13.8 3.87 
;
_refine_ls_weighting_scheme      calc
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_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              21
_reflns_limit_k_min              -22
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                12756
_reflns_number_total             15576
_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   0.0502
_oxford_refine_ls_scale          0.14521(3)
_oxford_reflns_number_all        15541
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            jo400212u_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C17.25 H21 I1 O3.75'
_cod_database_code               4028181