Toward the Synthesis of Phomoidride D
Graham K. Murphy; Tatsuya Shirahata; Naoto Hama; Aaron Bedermann; Ping Dong; Travis C. McMahon; Barry M. Twenter; David A. Spiegel; Ivar M. McDonald; Nobuaki Taniguchi; Munenori Inoue; John L. Wood; Journal of Organic Chemistry 78 (2013) 477–489; doi:10.1021/jo302353g

data_4027856
_publ_section_title
;
 Toward the Synthesis of Phomoidride D
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              477
_journal_page_last               489
_journal_paper_doi               10.1021/jo302353g
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C33 H44 O10'
_chemical_formula_weight         600.68
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-10-25 # Formatted by publCIF
;
_cell_angle_alpha                95.50(3)
_cell_angle_beta                 94.23(3)
_cell_angle_gamma                100.07(3)
_cell_formula_units_Z            4
_cell_length_a                   7.7285(15)
_cell_length_b                   15.223(3)
_cell_length_c                   27.208(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3123.8(11)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1200
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26485
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9679
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       blade
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         15489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc 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_gt          0.1749
_refine_ls_wR_factor_ref         0.2127
_reflns_number_gt                7774
_reflns_number_total             15489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo302353g_si_002.cif
_cod_data_source_block           im02
_cod_database_code               4027856