ProDOT-Assisted Isomerically Pure Indophenines.
Pappenfus, Ted M.; Helmin, Andrew J.; Wilcox, Wyatt D.; Severson, Sarah M.; Janzen, Daron E.; The Journal of organic chemistry 84 (2019) 11253–11257; doi:10.1021/acs.joc.9b01525

data_4033887
_publ_section_title
;
 ProDOT-Assisted Isomerically Pure Indophenines.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11253
_journal_page_last               11257
_journal_paper_doi               10.1021/acs.joc.9b01525
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C62 H84 Br2 N2 O6 S2'
_chemical_formula_sum            'C62 H84 Br2 N2 O6 S2'
_chemical_formula_weight         1177.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                78.429(6)
_cell_angle_beta                 89.290(6)
_cell_angle_gamma                88.540(6)
_cell_formula_units_Z            1
_cell_length_a                   6.2227(12)
_cell_length_b                   13.638(3)
_cell_length_c                   17.947(4)
_cell_measurement_reflns_used    10580
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      3.02
_cell_volume                     1491.6(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14270
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.019
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             620.00
_exptl_crystal_size_max          0.610
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6087
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.7495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                3451
_reflns_number_total             6087
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo9b01525_si_002.cif
_cod_data_source_block           User-defined
_cod_database_code               4033887
_shelxl_version_number           2013-3
_shelx_res_checksum              93886
_shelx_hkl_checksum              1013