Self-Consistent Synthesis of the Squalene Synthase Inhibitor Zaragozic Acid C via Controlled Oligomerization
David A. Nicewicz; Andrew D. Satterfield; Daniel C. Schmitt; Jeffrey S. Johnson; Journal of the American Chemical Society 130 (2008) 17281–17283; doi:10.1021/ja808347q

data_4108911
_publ_section_title
;
 Self-Consistent Synthesis of the Squalene Synthase Inhibitor Zaragozic
 Acid C via Controlled Oligomerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17281
_journal_page_last               17283
_journal_paper_doi               10.1021/ja808347q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C43 H76 O12 Si3'
_chemical_formula_sum            'C43 H76 O12 Si3'
_chemical_formula_weight         869.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.349(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4540(3)
_cell_length_b                   37.1782(11)
_cell_length_c                   12.5431(4)
_cell_measurement_temperature    100(2)
_cell_volume                     5069.8(3)
_computing_cell_refinement       'Bruker-AXS APEX2'
_computing_data_collection       'Bruker-AXS APEX2'
_computing_data_reduction        'Bruker-AXS APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II'
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48052
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.9573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         12247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                9865
_reflns_number_total             12247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808347q_si_003.cif
_cod_data_source_block           c06080
_cod_database_code               4108911