The <i>cis,cis</i>-proline isomer of ceratospongamide
Mitsunobu Doi; Aiko Yumiba; Akiko Asano; Acta Crystallographica Section E 58 (2002) o62–o64; doi:10.1107/S1600536801021079

data_2200823
_publ_section_title
;
 The <i>cis,cis</i>-proline isomer of ceratospongamide
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o62
_journal_page_last               o64
_journal_paper_doi               10.1107/S1600536801021079
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C41 H49 N7 O6 S'
_chemical_formula_moiety         'C41 H49 N7 O6 S'
_chemical_formula_sum            'C41 H49 N7 O6 S'
_chemical_formula_weight         767.93
_chemical_name_common            ccs
_chemical_name_systematic
;
 [cis,cis]-Ceratospongamide
 cyclo(-Ile-Oxz-Phe-Pro-Thz-Phe-Pro-)
 Oxz=oxazoline, Thz=thiazole
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.805(2)
_cell_length_b                   12.805(3)
_cell_length_c                   54.013(11)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      9.83
_cell_volume                     8856(3)
_computing_cell_refinement       'MSC/AFC Diffractmeter Control Software'
_computing_data_collection
;
MSC/AFC Diffractmeter Control Software
(Molecular Structure Corporation, 1991)
;
_computing_data_reduction        'MSC/AFC Diffractmeter Control Software'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .934
_diffrn_measured_fraction_theta_max .935
_diffrn_measurement_device_type  'Rigaku AFC-5R'
_diffrn_measurement_method       \2q-\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku RU200'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .1935
_diffrn_reflns_av_sigmaI/netI    .3798
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4364
_diffrn_reflns_theta_full        55.98
_diffrn_reflns_theta_max         55.98
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        98.18
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  .97
_exptl_absorpt_correction_T_min  .78
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .06
_refine_diff_density_max         .303
_refine_diff_density_min         -.219
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.688
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.688
_refine_ls_R_factor_all          .2172
_refine_ls_R_factor_gt           .0981
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.002P)^2^+5.200P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1264
_refine_ls_wR_factor_ref         .1554
_reflns_number_gt                2203
_reflns_number_total             4062
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6093.cif
_cod_data_source_block           I
_cod_original_cell_volume        8857(3)
_cod_database_code               2200823
_cod_database_fobs_code          2200823