A folded conformation of an ascidiacyclamide derivative: 3-methoxysulfoxide-(2<i>R</i>,3<i>R</i>)-threoninyl desoxazoline-ascidiacyclamide
Mitsunobu Doi; Akiko Asano; Yoshihide Usami; Yoshio Katsuya; Masamichi Nakai; Masahiro Sasaki; Taizo Taniguchi; Hiroshi Hasegawa; Acta Crystallographica Section E 57 (2001) o1019–o1021; doi:10.1107/S1600536801016129

data_2200776
_publ_section_title
;
 A folded conformation of an ascidiacyclamide derivative:
 3-methoxysulfoxide-(2<i>R</i>,3<i>R</i>)-threoninyl
 desoxazoline-ascidiacyclamide
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1019
_journal_page_last               o1021
_journal_paper_doi               10.1107/S1600536801016129
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C38 H60 N8 O12 S4'
_chemical_formula_moiety         'C38 H60 N8 O12 S4'
_chemical_formula_sum            'C38 H60 N8 O12 S4'
_chemical_formula_weight         949.18
_chemical_name_common            asco8-m
_chemical_name_systematic
;
 Diastereomer 8 of desoxazolin-ascidiacyclamide derivatives
 cyclo(-Ile-D-allo-MsThr-D-Val-Thz-Ile-D-allo-MsThr-D-Val-Thz-)
 Ms=methoxysufonyl
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7820(3)
_cell_length_b                   19.6026(4)
_cell_length_c                   22.5181(7)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      1.19
_cell_volume                     4759.3(2)
_computing_cell_refinement       'MOSFLM (Leslie, 1999)'
_computing_data_collection       'PROCESS (Higashi, 1996)'
_computing_data_reduction        MOSFLM
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full .994
_diffrn_measured_fraction_theta_max .994
_diffrn_measurement_device_type  'Rigaku R-AXIS-IV'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  diamond
_diffrn_radiation_source         'double monochromated beam'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     .83600
_diffrn_reflns_av_R_equivalents  .0554
_diffrn_reflns_av_sigmaI/netI    .0503
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16269
_diffrn_reflns_theta_full        30.60
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    .265
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          .08
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.314
_refine_diff_density_min         -.665
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .38(15)
_refine_ls_extinction_coef       .0085(10)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          .0783
_refine_ls_R_factor_gt           .0750
_refine_ls_shift/su_max          .042
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1152P)^2^+7.3374P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .2014
_reflns_number_gt                4759
_reflns_number_total             4973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6056.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               2200776
_cod_database_fobs_code          2200776