Total Syntheses of Multiple Cladiellin Natural Products by Use of a Completely General Strategy
J. Stephen Clark; Raphaëlle Berger; Stewart T. Hayes; Hans Martin Senn; Louis J. Farrugia; Lynne H. Thomas; Angus J. Morrison; Luca Gobbi; Journal of Organic Chemistry 78 (2013) 673–696; doi:10.1021/jo302542h

data_4027870
_publ_section_title
;
 Total Syntheses of Multiple Cladiellin Natural Products by Use of a
 Completely General Strategy
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              673
_journal_page_last               696
_journal_paper_doi               10.1021/jo302542h
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C24 H40 O3 Si'
_chemical_formula_sum            'C24 H40 O3 Si'
_chemical_formula_weight         404.65
_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                73.623(8)
_cell_angle_beta                 87.036(7)
_cell_angle_gamma                63.785(7)
_cell_formula_units_Z            2
_cell_length_a                   8.8106(11)
_cell_length_b                   9.7886(14)
_cell_length_c                   16.251(2)
_cell_measurement_reflns_used    4805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.40
_cell_volume                     1202.0(3)
_computing_cell_refinement       'Bruker AXS X8 Apex2'
_computing_data_collection       'Bruker AXS X8 Apex2'
_computing_data_reduction        'Bruker AXS SAINT V7.60A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18131
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.4625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                3974
_reflns_number_total             5478
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo302542h_si_001_1.cif
_cod_data_source_block           comp_40
_cod_database_code               4027870