Episulfonium ion-mediated cyclic peptide and triazine synthesis
Fox, David J.; Morley, Thomas J.; Warren, Stuart; Organic & Biomolecular Chemistry 4 (2006) 3120–; doi:10.1039/b606882k

data_7151268
_publ_section_title
;
 Episulfonium ion-mediated cyclic peptide and triazine synthesis
;
_journal_issue                   16
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              3120
_journal_paper_doi               10.1039/b606882k
_journal_volume                  4
_journal_year                    2006
_chemical_formula_moiety         'C36 H45 N3 O3 S3,0.5(H2 O)'
_chemical_formula_sum            'C36 H46 N3 O3.5 S3'
_chemical_formula_weight         672.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.977(1)
_cell_angle_beta                 80.763(1)
_cell_angle_gamma                75.344(1)
_cell_formula_units_Z            4
_cell_length_a                   12.2457(2)
_cell_length_b                   13.6867(3)
_cell_length_c                   22.7701(5)
_cell_measurement_reflns_used    78940
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     3636.02(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_sigmaI/netI    0.1283
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39905
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         16301
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.0705
_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^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.2067
_reflns_number_gt                8840
_reflns_number_total             16301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606882k.txt
_cod_data_source_block           sw0601
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C36 H46 N3 O3.50 S3'
_cod_database_code               7151268