Total Synthesis of (\±)-Phomactin A. Lessons Learned from Respecting a Challenging Structural Topology
Grant S. Buchanan; Kevin P. Cole; Yu Tang; Richard P. Hsung; Journal of Organic Chemistry 76 (2011) 7027–7039; doi:10.1021/jo200936r

data_4026545
_publ_section_title
;
 Total Synthesis of (\+-)-Phomactin A. Lessons Learned from Respecting a
 Challenging Structural Topology
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7027
_journal_page_last               7039
_journal_paper_doi               10.1021/jo200936r
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C25 H44 O4 Si'
_chemical_formula_sum            'C25 H44 O4 Si'
_chemical_formula_weight         436.69
_chemical_name_common            04320
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                101.813(1)
_cell_angle_beta                 93.644(1)
_cell_angle_gamma                94.256(1)
_cell_formula_units_Z            2
_cell_length_a                   9.4004(7)
_cell_length_b                   10.2614(8)
_cell_length_c                   13.271(1)
_cell_measurement_reflns_used    2890
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.30
_cell_volume                     1245.50(16)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15061
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0612P)^2^+0.3984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                4766
_reflns_number_total             5696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200936r_si_003.cif
_cod_data_source_block           04320
_cod_original_cell_volume        1245.5(2)
_cod_database_code               4026545