A β-sheet structure formed by C‒H···O hydrogen bonds between the thiazole rings and amide bonds of a dimeric desoxazoline ascidiacyclamide analogue
Asano, Akiko; Taniguchi, Taizo; Sasaki, Masahiro; Hasegawa, Hiroshi; Katsuya, Yoshio; Doi, Mitsunobu; Acta Crystallographica Section E 57 (2001) o834–o838; doi:10.1107/S160053680101279X

data_2200556
_publ_section_title
;
 A \b-sheet structure formed by C--H&#x00B7;&#x00B7;&#x00B7;O hydrogen
 bonds between the thiazole rings and amide bonds of a dimeric
 desoxazoline ascidiacyclamide analogue
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o834
_journal_page_last               o838
_journal_paper_doi               10.1107/S160053680101279X
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C72 H112 N16 O16 S4, 3C3 H7 N O, H2 O'
_chemical_formula_moiety         'C72 H112 N16 O16 S4, 3C3 H7 N O, H2 O'
_chemical_formula_sum            'C81 H135 N19 O20 S4'
_chemical_formula_weight         1823.32
_chemical_name_common            asco6d
_chemical_name_systematic
;
desoxazoline-ascidiacyclamide dimer (DMF & H2O solvated)
cyclo(-Ile-Thr-D-Val-Thz-Ile-D-alloIle-D-Val-Thz-)2
[Thz = thiazole, Thr = (2S,3R), D-alloThr = (2R,3R)]
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3492(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.55630(10)
_cell_length_b                   9.9957(2)
_cell_length_c                   42.9208(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4956.55(16)
_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  'PARST (Nardelli, 1995)'
_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 .931
_diffrn_measured_fraction_theta_max .931
_diffrn_measurement_device_type  'Rigaku RAXIS-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  .0378
_diffrn_reflns_av_sigmaI/netI    .0736
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15629
_diffrn_reflns_theta_full        30.25
_diffrn_reflns_theta_max         30.25
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    .168
_exptl_absorpt_correction_T_max  .66123
_exptl_absorpt_correction_T_min  .65673
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details   '(CYLABS; Nardelli, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          .01
_exptl_crystal_size_mid          .01
_exptl_crystal_size_min          .01
_refine_diff_density_max         1.515
_refine_diff_density_min         -1.214
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -.17(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         8977
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          .0973
_refine_ls_R_factor_gt           .0967
_refine_ls_shift/su_max          .017
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1312P)^2^+5.0564P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .2592
_reflns_number_gt                8890
_reflns_number_total             8977
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6037.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2200556
_cod_database_fobs_code          2200556