Structurally Defined α-Tetralol-Based Chiral Hypervalent Iodine Reagents.
Hokamp, Tobias; Wirth, Thomas; The Journal of organic chemistry 84 (2019) 8674–8682; doi:10.1021/acs.joc.9b01315

data_4034110
_publ_section_title
;
 Structurally Defined \a-Tetralol-Based Chiral Hypervalent Iodine
 Reagents.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8674
_journal_page_last               8682
_journal_paper_doi               10.1021/acs.joc.9b01315
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C23.38 H26.75 Cl0.75 I N O7'
_chemical_formula_weight         587.19
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5783(5)
_cell_length_b                   23.5783(5)
_cell_length_c                   8.8815(4)
_cell_measurement_reflns_used    7889
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.2510
_cell_measurement_theta_min      3.5440
_cell_volume                     4937.5(3)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            46941
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.824
_diffrn_reflns_theta_min         3.352
_exptl_absorpt_coefficient_mu    1.421
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       needle
_exptl_crystal_F_000             2366
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6571
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+5.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3829
_reflns_number_total             6571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01315_si_005.cif
_cod_data_source_block           tw1825
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4034110
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.606
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              42359
_shelx_hkl_checksum              43597