Drastic Enhancement of Activity in Iodane-Based α-Tosyloxylation of Ketones: Iodine(III) Does the Hypervalent Twist
Guilbault, Audrey-Anne; Legault, Claude Y.; ACS Catalysis 2 (2012) 219–; doi:10.1021/cs200612s

data_4505635
_publ_section_title
;
 Drastic Enhancement of Activity in Iodane-Based \a-Tosyloxylation of
 Ketones: Iodine(III) Does the Hypervalent Twist
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              219
_journal_paper_doi               10.1021/cs200612s
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C19 H22 I N O5 S'
_chemical_formula_weight         503.34
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_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_date             2011-05-06T09:26:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.67(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.172(3)
_cell_length_b                   7.921(3)
_cell_length_c                   33.699(8)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1910.5(12)
_computing_cell_refinement       Difrac
_computing_data_collection       Difrac
_computing_data_reduction        NRCVAX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
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_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3524
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  0.8392
_exptl_absorpt_correction_T_min  0.4636
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   Empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.75
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.059
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1635
_reflns_number_gt                2152
_reflns_number_total             3524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs200612s_si_003.cif
_cod_data_source_block           aag03153
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psi-Scan'
changed to 'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1910.4(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4505635