Stereoselective synthesis of a highly oxygenated decahydrocyclopenta[g]chromene derivative: the common tricyclic framework of leucosceptrine and leucosesterterpenone
Hideki Abe; Yuri Horii; Megumi Hagiwara; Toyoharu Kobayashi; Hisanaka Ito; Chem.Commun. 51 (2015) 6108–; doi:10.1039/C5cc00879D

data_7116885
_publ_section_title
;
 Stereoselective synthesis of a highly oxygenated
 decahydrocyclopenta[g]chromene derivative: the common tricyclic framework
 of leucosceptrine and leucosesterterpenone
;
_journal_name_full               Chem.Commun.
_journal_page_first              6108
_journal_paper_doi               10.1039/C5cc00879D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C29 H46 O5 Si'
_chemical_formula_sum            'C29 H46 O5 Si'
_chemical_formula_weight         502.75
_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_date             'December 19 2013'
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-20 deposited with the CCDC.
2015-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.7770(6)
_cell_angle_beta                 91.5850(6)
_cell_angle_gamma                102.5500(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3975(6)
_cell_length_b                   11.1440(6)
_cell_length_c                   13.6268(8)
_cell_measurement_reflns_used    7066
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.44
_cell_volume                     1398.60(14)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0219
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13770
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_correction_T_min  0.9765
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Crystal Faces plugin in Bruker APEX2 software
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0371P)^2^+0.7570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                4480
_reflns_number_total             4936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00879d2.cif
_cod_data_source_block           p-1_a
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1  '
_cod_database_code               7116885