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 79 (2016) 3134–3142; doi:10.1021/acs.jnatprod.6b00910

data_1545001
_publ_section_title
;
 Diterpenoids of the Cassane Type from Caesalpinia decapetala.
;
_journal_issue                   12
_journal_name_full               'Journal of natural products'
_journal_page_first              3134
_journal_page_last               3142
_journal_paper_doi               10.1021/acs.jnatprod.6b00910
_journal_volume                  79
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H30 O6'
_chemical_formula_sum            'C23 H30 O6'
_chemical_formula_weight         402.47
_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                 100.323(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4070(4)
_cell_length_b                   23.1784(13)
_cell_length_c                   11.0659(6)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.04
_cell_measurement_theta_min      5.68
_cell_volume                     2121.41(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 0.977
_diffrn_measured_fraction_theta_max 0.949
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21866
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.305
_diffrn_reflns_theta_min         4.487
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.7533
_exptl_transmission_factor_min   0.6363
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2293 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         6446
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0720P)^2^+1.1975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.631
_reflns_Friedel_fraction_full    0.662
_reflns_Friedel_fraction_max     0.632
_reflns_number_gt                6309
_reflns_number_total             6446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00910_si_003.cif
_cod_data_source_block           cu_zyh_1311_0m
_cod_database_code               1545001
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.867
_shelx_res_checksum              5625
_shelx_hkl_checksum              64661