Total Synthesis of the G2/M DNA Damage Checkpoint Inhibitor Psilostachyin C
Chao Li; Shanghui Tu; Shuguang Wen; Shan Li; Junbiao Chang; Feng Shao; Xiaoguang Lei; Journal of Organic Chemistry 76 (2011) 3566–3570; doi:10.1021/jo2001275

data_4026242
_publ_section_title
;
 Total Synthesis of the G2/M DNA Damage Checkpoint Inhibitor Psilostachyin
 C
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3566
_journal_page_last               3570
_journal_paper_doi               10.1021/jo2001275
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C38 H58 O10'
_chemical_formula_weight         674.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.357(5)
_cell_length_b                   10.230(2)
_cell_length_c                   18.278(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3729.4(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18182
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_correction_T_min  0.9831
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+3.0882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                3082
_reflns_number_total             3283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2001275_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        3729.4(13)
_cod_database_code               4026242