The highly solvated structure of theonellapeptolide Id, a tridecapeptide lactone from the Okinawa marine sponge <i>Theonella swinhoei</i>
Mitsunobu Doi; Toshimasa Ishida; Motomasa Kobayashi; Jeffrey R. Deschamps; Judith L. Flippen-Anderson; Acta Crystallographica Section C 55 (1999) 796–798; doi:10.1107/S0108270198014383

data_2008521
_publ_section_title
;
 The highly solvated structure of theonellapeptolide Id, a
 tridecapeptide lactone from the Okinawa marine sponge <i>Theonella
 swinhoei</i>
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              796
_journal_page_last               798
_journal_paper_doi               10.1107/S0108270198014383
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C70 H125 N13 O16,12(H2 O)'
_chemical_formula_sum            'C70 H149 N13 O28'
_chemical_formula_weight         1621.0
_chemical_name_common            TNLP
_chemical_name_systematic        Theonellapeptolide-Id
_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'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.205(4)
_cell_length_b                   37.941(8)
_cell_length_c                   12.227(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.09
_cell_measurement_theta_min      9.92
_cell_volume                     9837(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1991
;
_computing_data_reduction        'MSC/AFC Diffractometer Control Software'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution
'SnB (Miller et al., 1994; Chang et al., 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku AFC-5R/RU-200'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8571
_diffrn_reflns_theta_full        62.89
_diffrn_reflns_theta_max         62.89
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        3.64
_diffrn_standards_interval_count 100
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.594
_refine_ls_abs_structure_details
'determined by chemical methods (see Kobayashi, Kanzaki et al., 1994)'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    'H-atom treatment: mixed'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         8571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.136
_refine_ls_R_factor_gt           0.113
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.14P)^2^+18.50P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.287
_reflns_number_gt                7490
_reflns_number_total             8571
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sx1064.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.14P)^2^+18.50P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.14P)^2^+18.50P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2008521