Turn-over of an oxazoline ring induced by chiral change of a folded ascidiacyclamide analogue: cyclo(Ile-<small>D</small>‒aThr‒<small>D</small>-Val‒Thz‒Ile‒<small>D</small>-Oxz‒<small>D</small>-Val‒Thz) <i>N,N</i>-dimethylformamide disolvate
Akiko Asano; Mitsunobu Doi; Acta Crystallographica Section E 60 (2004) o2449–o2451; doi:10.1107/S1600536804030247

data_2204729
_publ_section_title
;Turn-over of an oxazoline ring induced by chiral change of a folded
 ascidiacyclamide analogue:
 cyclo(Ile-<small>D</small>--aThr--<small>D</small>-Val--Thz--Ile--<small>D</small>-Oxz--<small>D</small>-Val--Thz)
 <i>N,N</i>-dimethylformamide disolvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2449
_journal_page_last               o2451
_journal_paper_doi               10.1107/S1600536804030247
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C36 H54 N8 O7 S2, 2C3 H7 N O'
_chemical_formula_moiety         'C36 H54 N8 O7 S2, 2C3 H7 N O'
_chemical_formula_sum            'C42 H68 N10 O9 S2'
_chemical_formula_weight         921.18
_chemical_name_common            asc9o
_chemical_name_systematic
;
 ascidiacyclamide analogue No.9
 cyclo(Ile-D-aThr(3R)-D-Val-Thz-Ile-D-Oxz(3S)-D-Val-Thz)
 isoleucyl-D-
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0310(10)
_cell_length_b                   11.0503(9)
_cell_length_c                   17.3580(10)
_cell_measurement_reflns_used    8060
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.45
_cell_volume                     2418.2(3)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'MacScience, M18XCE rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20955
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0.03
_diffrn_standards_interval_count 20955
_diffrn_standards_interval_time  660
_diffrn_standards_number         216
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_correction_T_min  0.8867
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.521
_refine_ls_abs_structure_details 'Flack (1983), 4576 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10109
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0967P)^2^+0.6439P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                8732
_reflns_number_total             10109
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp6018.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2204729
_cod_database_fobs_code          2204729