Preparation, Structure, and Unexpected Chemistry of Phosphoranyl-Derived Benziodoxoles
Viktor V. Zhdankin; Olena Maydanovych; Jon Herschbach; Robert McDonald; Rik R. Tykwinski; Journal of the American Chemical Society 124 (2002) 11614–11615; doi:10.1021/ja0277780

data_4115183
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       rik.tykwinski@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr Rik R. Tykwinski'
_publ_contact_author_phone       1(780)4925307
_publ_section_title
;
 Preparation, Structure, and Unexpected Chemistry of Phosphoranyl-Derived
 Benziodoxoles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11614
_journal_page_last               11615
_journal_paper_doi               10.1021/ja0277780
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C58 H48 Cl I2 N O6 P2'
_chemical_formula_weight         1206.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.895(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2285(9)
_cell_length_b                   29.139(3)
_cell_length_c                   17.8515(17)
_cell_measurement_reflns_used    3764
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.608
_cell_measurement_theta_min      2.239
_cell_volume                     5206.4(9)
_computing_cell_refinement       'Bruker SHELXTL (Sheldrick, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SHELXTL (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1931
_diffrn_reflns_av_sigmaI/netI    0.2651
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25391
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.9345
_exptl_absorpt_correction_T_min  0.7430
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10670
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.2138
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                4600
_reflns_number_total             10670
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0277780_s1_2.cif
_cod_data_source_block           compound(3b)
_cod_original_cell_volume        5206.4(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4115183