Systemic Study on the Biogenic Pathways of Yezo'otogirins: Total Synthesis and Antitumor Activities of (±)-Yezo'otogirin C and Its Structural Analogues.
Yang, Wei; Cao, Jingming; Zhang, Mengxun; Lan, Rongfeng; Zhu, Lizhi; Du, Guangyan; He, Shuzhong; Lee, Chi-Sing; The Journal of organic chemistry 80 (2014) 836–; doi:10.1021/jo502267g

data_4030536
_publ_section_title
;
 Systemic Study on the Biogenic Pathways of Yezo'otogirins: Total
 Synthesis and Antitumor Activities of (+-)-Yezo'otogirin C and Its
 Structural Analogues.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              836
_journal_paper_doi               10.1021/jo502267g
_journal_volume                  80
_journal_year                    2014
_chemical_formula_sum            'C23 H38 O4'
_chemical_formula_weight         378.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.794(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.0238(5)
_cell_length_b                   16.1168(2)
_cell_length_c                   8.6240(6)
_cell_measurement_reflns_used    35420
_cell_measurement_temperature    293(2)
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_cell_measurement_theta_min      6.60
_cell_volume                     4357.1(3)
_computing_cell_refinement       'CrystalClear-SM Auto 2.0 r4'
_computing_data_collection       'CrystalClear-SM 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Auto 2.0 r4'
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_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            40404
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.291
_diffrn_reflns_theta_min         6.627
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.870
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
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_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3917
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+1.8097P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3471
_reflns_number_total             3917
_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_res_checksum              94828
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