Synthetic Studies on CP-225,917 and CP-263,114: Access to Advanced Tetracyclic Systems by Intramolecular Conjugate Displacement and [2,3]-Wittig Rearrangement
Farzad Malihi; Derrick L. J. Clive; Che-Chien Chang; Minaruzzaman; Journal of Organic Chemistry 78 (2013) 996–1013; doi:10.1021/jo302467w

data_4027914
_publ_section_title
;
 Synthetic Studies on CP-225,917 and CP-263,114: Access to Advanced
 Tetracyclic Systems by Intramolecular Conjugate Displacement and
 [2,3]-Wittig Rearrangement
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              996
_journal_page_last               1013
_journal_paper_doi               10.1021/jo302467w
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C39 H50 O9 Si'
_chemical_formula_sum            'C39 H50 O9 Si'
_chemical_formula_weight         690.88
_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                78.3311(3)
_cell_angle_beta                 83.2943(3)
_cell_angle_gamma                87.9616(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2074(2)
_cell_length_b                   15.3803(4)
_cell_length_c                   16.4727(5)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.54
_cell_volume                     1775.92(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Schneider & Sheldrick, 2002)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15716
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_correction_T_min  0.9447
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0494P)^2^+0.5156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                6657
_reflns_number_total             8061
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo302467w_si_001.cif
_cod_data_source_block           dlc0906
_cod_database_code               4027914