Highly Selective Synthesis of Heterosubstituted Aromatic Sulfamides
Hof, Fraser; Iovine, Peter M.; Johnson, Darren W.; Rebek, Julius; Organic Letters 3 (2001) 4247–; doi:10.1021/ol0169731

data_1507545
_publ_contact_author
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Julius Rebek, Jr.
Skaggs Institute for Chemical Biology (MB26)
The Scripps Research Institute
10550 N. Torrey Pines Road
La Jolla, CA  92037
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_publ_section_title
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 Highly Selective Synthesis of Heterosubstituted Aromatic Sulfamides
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_journal_issue                   26
_journal_name_full               'Organic Letters'
_journal_page_first              4247
_journal_paper_doi               10.1021/ol0169731
_journal_volume                  3
_journal_year                    2001
_chemical_formula_sum            'C16 H22 N2 O6 S'
_chemical_formula_weight         370.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.343(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.100(6)
_cell_length_b                   11.223(5)
_cell_length_c                   11.773(5)
_cell_measurement_reflns_used    7169
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.32
_cell_volume                     1859.8(14)
_computing_cell_refinement
;
SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device_type  '3 circle diffractometer'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4833
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0594
_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^)+(0.1341P)^2^+0.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                1924
_reflns_number_total             2193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0169731_s2.cif
_cod_data_source_block           hofsulfs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1859.8(13)
_cod_original_sg_symbol_H-M      P2(1)/a
_cod_database_code               1507545