cyclo(-Cha‒Oxz‒<small>D</small>-Val‒Thz‒Ile‒Oxz‒<small>D</small>-Val‒Thz-) <i>N,N</i>-dimethylacetamide dihydrate: a square form of cyclohexylalanine-incorporated ascidiacyclamide having the strongest cytotoxicity
Akiko Asano; Takeshi Yamada; Atsushi Numata; Mitsunobu Doi; Acta Crystallographica Section C 59 (2003) o488–o490; doi:10.1107/S0108270103014495

data_2013495
_publ_section_title
;cyclo(-Cha--Oxz--<small>D</small>-Val--Thz--Ile--Oxz--<small>D</small>-Val--Thz-)
 <i>N,N</i>-dimethylacetamide dihydrate: a square form of
 cyclohexylalanine-incorporated ascidiacyclamide having the strongest
 cytotoxicity
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o488
_journal_page_last               o490
_journal_paper_doi               10.1107/S0108270103014495
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C39 H56 N8 O6 S2, C4 H9 N O, 2H2 O'
_chemical_formula_moiety         'C39 H56 N8 O6 S2, C4 H9 N O, 2H2 O'
_chemical_formula_sum            'C43 H69 N9 O9 S2'
_chemical_formula_weight         920.19
_chemical_name_common            ChaASC
_chemical_name_systematic
;
Ascidiacyclamide analogue (Ile1 was replaced with Cha)
cyclo(-Cha-Oxz-D-Val-Thz-Ile-Oxz-D-Val-Thz-) Cha=cyclohexylalanine
from dimethylacetamide solution
;
_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                 105.252(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.283(2)
_cell_length_b                   14.153(2)
_cell_length_c                   13.452(2)
_cell_measurement_reflns_used    9020
_cell_measurement_temperature    90.0(10)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.14
_cell_volume                     2439.8(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (Sheldrick & Gould, 1996)'
_diffrn_ambient_temperature      90.0(10)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD'
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22268
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.52
_diffrn_standards_interval_count 22302
_diffrn_standards_interval_time  405
_diffrn_standards_number         342
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.348
_refine_ls_abs_structure_details '(Flack, 1983), 5087 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         11112
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0937P)^2^+0.2367P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                9973
_reflns_number_total             11112
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1130.cif
_cod_data_source_block           I
_cod_original_cell_volume        2439.8(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2013495
_cod_database_fobs_code          2013495