Diterpenoids of the Cassane Type from Caesalpinia decapetala
Qiao, Yuben; Xu, Qianqian; Hu, Zhengxi; Li, Xiao-Nian; Xiang, Ming; Liu, Junjun; Huang, Jinfeng; Zhu, Hucheng; Wang, Jianping; Luo, Zengwei; Xue, Yongbo; Zhang, Yonghui; Journal of Natural Products  (2016) –; doi:10.1021/acs.jnatprod.6b00910

data_1544781
_publ_section_title
;
 Diterpenoids of the Cassane Type from Caesalpinia decapetala
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.6b00910
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H28 O5'
_chemical_formula_sum            'C21 H28 O5'
_chemical_formula_weight         360.43
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.247(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8585(10)
_cell_length_b                   13.8457(17)
_cell_length_c                   8.4093(10)
_cell_measurement_reflns_used    8551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.11
_cell_measurement_theta_min      3.19
_cell_volume                     878.45(19)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8276
_diffrn_reflns_point_group_measured_fraction_full 0.881
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.502
_diffrn_reflns_theta_min         5.479
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_exptl_transmission_factor_max   0.7532
_exptl_transmission_factor_min   0.4549
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 1064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_coef       0.025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2843
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0689P)^2^+0.1159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_full    0.773
_reflns_Friedel_fraction_max     0.746
_reflns_number_gt                2664
_reflns_number_total             2843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00910_si_002.cif
_cod_data_source_block           cu_zyh_1312_0m
_cod_database_code               1544781
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.853
_shelx_res_checksum              33561
_shelx_hkl_checksum              65510