Efforts to Total Synthesis of Philinopside E: Convergent Synthesis of the Sulfated Lanostane-Type Tetraglycoside
Bai, Shujin; Wu, Zhi-Yong; Huang, Qingyun; Zhang, Li; Chen, Pengwei; Wang, Cong; Zhang, Xiuli; Wang, Peng; Li, Ming; RSC Adv.  (2016) –; doi:10.1039/C5RA25845F

data_7223748
_publ_section_title
;
 Efforts to Total Synthesis of Philinopside E: Convergent Synthesis of the
 Sulfated Lanostane-Type Tetraglycoside
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA25845F
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C39 H74 O5 Si'
_chemical_formula_weight         651.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-08-21 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1715(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.2841(3)
_cell_length_b                   31.6830(16)
_cell_length_c                   10.0930(5)
_cell_measurement_temperature    296(2)
_cell_volume                     2006.43(17)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         3.247
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.502
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.254
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3268 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         9194
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.8857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                7632
_reflns_number_total             9194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra25845f2.cif
_cod_data_source_block           2sad
_cod_database_code               7223748
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-4
_shelx_res_checksum              21016