Xylopsides A-D, four rare guaiane dimers with two unique bridged pentacyclic skeletons from Xylopia vielana.
Xie, Yang-Guo; Guo, Yi-Gong; Wu, Guo-Jing; Zhu, Sheng-Lan; Cheng, Tao-Fang; Zhang, Yu; Yan, Shi-Kai; Jin, Hui-Zi; Zhang, Wei-Dong; Organic & biomolecular chemistry 16 (2018) 8408–8412; doi:10.1039/c8ob01689e

data_7156411
_publ_section_title
;
 Xylopsides A-D, four rare guaiane dimers with two unique bridged
 pentacyclic skeletons from Xylopia vielana.
;
_journal_issue                   37
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8408
_journal_page_last               8412
_journal_paper_doi               10.1039/c8ob01689e
_journal_volume                  16
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H40 O2'
_chemical_formula_sum            'C30 H40 O2'
_chemical_formula_weight         432.62
_chemical_name_systematic        X-90
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                97.812(2)
_cell_angle_beta                 92.511(2)
_cell_angle_gamma                94.499(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6619(3)
_cell_length_b                   7.6737(3)
_cell_length_c                   21.9350(9)
_cell_measurement_reflns_used    7978
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      65.07
_cell_measurement_theta_min      5.80
_cell_volume                     1271.83(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12847
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        65.098
_diffrn_reflns_theta_max         65.098
_diffrn_reflns_theta_min         5.801
_exptl_absorpt_coefficient_mu    0.524
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       blcok
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.7526
_exptl_transmission_factor_min   0.6687
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.3(9)
_refine_ls_extinction_coef       0.037(6)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7691
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0931
_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^)+(0.1764P)^2^+1.3661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2768
_refine_ls_wR_factor_ref         0.2842
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                6937
_reflns_number_total             7691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob01689e2.cif
_cod_data_source_block           ta_a
_cod_depositor_comments
'Adding full bibliography for 7156410--7156411.cif.'
_cod_database_code               7156411
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              15640