<i>cis</i>,<i>cis</i>-Ceratospongamide <i>N</i>,<i>N</i>-dimethylacetamide hemisolvate in the presence of twinning
Mitsunobu Doi; Akiko Asano; Kenji Yoza; Acta Crystallographica Section C 59 (2003) o323–o325; doi:10.1107/S010827010300369X

data_2013341
_publ_section_title
;
 <i>cis</i>,<i>cis</i>-Ceratospongamide
 <i>N</i>,<i>N</i>-dimethylacetamide hemisolvate in the presence of
 twinning
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o323
_journal_page_last               o325
_journal_paper_doi               10.1107/S010827010300369X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C41 H49 N7 O6 S, 0.5C4 H9 N O'
_chemical_formula_moiety         'C41 H49 N7 O6 S, 0.5C4 H9 N O'
_chemical_formula_sum            'C43 H53.5 N7.5 O6.5 S'
_chemical_formula_weight         811.51
_chemical_name_common            ccs1
_chemical_name_systematic
;
cis,cis-Ceratospongamide, N,N-dimethylacetamide hemisolvate
cyclo(-Ile-Oxz-Phe-Pro-Thz-Phe-Pro-)
;
_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'
_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                   12.6034(7)
_cell_length_b                   12.6075(7)
_cell_length_c                   53.536(3)
_cell_measurement_reflns_used    8337
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      2.3
_cell_volume                     8506.7(8)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (Seldrick & Gould, 1996)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker AXS SMART APEX area detector'
_diffrn_measurement_method       '\w scan'
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            102830
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.14
_diffrn_standards_decay_%        0.37
_diffrn_standards_interval_count 102830
_diffrn_standards_interval_time  '330 min'
_diffrn_standards_number         1242
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.8830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.274
_refine_ls_abs_structure_details '(Flack, 1983), 8904 Friedel pairs'
_refine_ls_abs_structure_Flack   0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         20493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0783P)^2^+1.9396P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                20401
_reflns_number_total             20493
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1101.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_original_formula_sum        'C43 H53.5 N7.5 O6.5 S1'
_cod_database_code               2013341
_cod_database_fobs_code          2013341