Absolute stereostructures of cell-adhesion inhibitors, macrosphelides C, Eâ€“G and I, produced by a Periconia species separated from an Aplysia sea hare
Yamada, Takeshi; Iritani, Masashi; Doi, Mitsunobu; Minoura, Katsuhiko; Ito, Tadayoshi; Numata, Atsushi; Journal of the Chemical Society, Perkin Transactions 1  (2001) 3046–; doi:10.1039/b104337b

data_7216878
_publ_section_title
;
 Absolute stereostructures of cell-adhesion inhibitors, macrosphelides C,
 E\^a&#x20AC;&#x201C;G and I, produced by a Periconia species separated
 from an Aplysia sea hare
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3046
_journal_paper_doi               10.1039/b104337b
_journal_year                    2001
_chemical_formula_sum            'C16 H22 O7'
_chemical_formula_weight         326.34
_chemical_name_common            mpc
_chemical_name_systematic
; 
Macrosphelide C
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.514(2)
_cell_length_b                   28.460(2)
_cell_length_c                   5.860(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      21.07
_cell_measurement_theta_min      18.89
_cell_volume                     1753.5(7)
_computing_cell_refinement       'MSC/AFC Diffractmeter Control Software'
_computing_data_collection       'MSC/AFC Diffractmeter Control Software'
_computing_data_reduction        'MSC/AFC Diffractmeter Control Software'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson 1996)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      288(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       2\q-\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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2864
_diffrn_reflns_theta_full        67.63
_diffrn_reflns_theta_max         67.63
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   'North, Phillips & Mathews (1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.123
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_extinction_coef       0.0075(6)
_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   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                2185
_reflns_number_total             2473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104337b.txt
_cod_data_source_block           mpc
_cod_original_cell_volume        1753.4(7)
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               7216878