Practical entry into the HIJKLM ring segment of ciguatoxin CTX3C
Oishi, Tohru; Uehara, Hisatoshi; Nagumo, Yoko; Shoji, Mitsuru; Le Brazidec, Jean-Yves; Kosaka, Masashi; Hirama, Masahiro; Chemical Communications  (2001) 381–; doi:10.1039/b009506k

data_7114758
_publ_section_title
;
 Practical entry into the HIJKLM ring segment of ciguatoxin CTX3C
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              381
_journal_paper_doi               10.1039/b009506k
_journal_year                    2001
_chemical_formula_moiety         'C39 H48 Br2 O10 '
_chemical_formula_sum            'C39 H48 Br2 O10'
_chemical_formula_weight         836.61
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5284(3)
_cell_length_b                   25.006(2)
_cell_length_c                   27.913(2)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.5
_cell_volume                     3858.8(5)
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    DirectMethod
_diffrn_measurement_device_type  'Quantum CCD/Rigaku AFC7'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27206
_diffrn_reflns_theta_max         26.00
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_Flack   -0.02(1)
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     460
_refine_ls_number_reflns         4740
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          -0.0040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                4740
_reflns_number_total             7494
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b009506k.txt
_cod_data_source_block           uehara-150k
_cod_original_cell_volume        3858.7(4)
_cod_original_sg_symbol_H-M      'P 21 21 21   '
_cod_original_formula_sum        'C39 H48 Br2 O10 '
_cod_database_code               7114758