Exploiting the narrow gap of rearrangement between the substituents in the vicinal disubstitution reactions of diaryliodonium salts with pyridine N-sulfonamidates.
Wang, Yong; Li, Ming; Wen, Lirong; Jing, Peng; Su, Xiang; Chen, Chao; Organic & biomolecular chemistry 13 (2015) 751–763; doi:10.1039/c4ob01744g

data_7154176
_publ_section_title
;
 Exploiting the narrow gap of rearrangement between the substituents in
 the vicinal disubstitution reactions of diaryliodonium salts with
 pyridine N-sulfonamidates.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              751
_journal_page_last               763
_journal_paper_doi               10.1039/c4ob01744g
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C19 H19 F6 N2 O2 P S'
_chemical_formula_weight         484.40
_space_group_IT_number           14
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_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           SHELXL-97
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_cell_angle_beta                 94.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.338(3)
_cell_length_b                   10.040(2)
_cell_length_c                   14.189(3)
_cell_measurement_reflns_used    5992
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.33
_cell_volume                     2178.7(8)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  .9282
_exptl_absorpt_correction_T_min  .8729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .43
_exptl_crystal_size_min          .26
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_refine_ls_matrix_type           full
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+2.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                4725
_reflns_number_total             4971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob01744g2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7154174--7154176.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7154176
_refine_ls_r_factor_ref          0.0811