The Stereochemical Assignment and Conformational Analysis of the V/W-Ring Juncture of Maitotoxin
Laura R. Cook; Hitoshi Oinuma; Marcus A. Semones; Yoshito Kishi; Journal of the American Chemical Society 119 (1997) 7928–7937; doi:10.1021/ja971259t

data_4117012
_publ_section_title
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 The Stereochemical Assignment and Conformational Analysis of the V/W-Ring
 Juncture of Maitotoxin
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7928
_journal_page_last               7937
_journal_paper_doi               10.1021/ja971259t
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C33 H36 N4 O16'
_chemical_formula_weight         744.66
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6105(13)
_cell_length_b                   6.0850(6)
_cell_length_c                   20.975(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      999.00
_cell_volume                     1725.7(3)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3181
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       plates
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.58(332)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.622
_refine_ls_goodness_of_fit_obs   1.673
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2970
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.668
_refine_ls_restrained_S_obs      1.673
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_obs          0.0896
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.8596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1661
_refine_ls_wR_factor_obs         0.1418
_reflns_number_observed          2279
_reflns_number_total             2971
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971259t_3.cif
_cod_data_source_block           Compound_13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.8596P] 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^)+(0.0249P)^2^+0.8596P] 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               4117012