β-Dihydroagarofuran-Type Sesquiterpenes from the Seeds of Celastrus monospermus and Their Lifespan-Extending Effects on the Nematode Caenorhabditis elegans.
Gao, Lei; Zhang, Rujun; Lan, Jianfeng; Ning, Ruonan; Wu, Di; Chen, Di; Zhao, Weimin; Journal of natural products 79 (2016) 3039–3046; doi:10.1021/acs.jnatprod.6b00648

data_1545002
_publ_section_title
;
 \b-Dihydroagarofuran-Type Sesquiterpenes from the Seeds of Celastrus
 monospermus and Their Lifespan-Extending Effects on the Nematode
 Caenorhabditis elegans.
;
_journal_issue                   12
_journal_name_full               'Journal of natural products'
_journal_page_first              3039
_journal_page_last               3046
_journal_paper_doi               10.1021/acs.jnatprod.6b00648
_journal_volume                  79
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H38 O11'
_chemical_formula_sum            'C30 H38 O11'
_chemical_formula_weight         574.60
_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
_audit_creation_date             2016-09-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4232(2)
_cell_length_b                   8.8867(2)
_cell_length_c                   18.0421(4)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.53
_cell_measurement_theta_min      4.84
_cell_volume                     1463.69(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18276
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         2.528
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.7979.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 2082 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4972
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0553P)^2^+0.1762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.876
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                4895
_reflns_number_total             4972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00648_si_001.cif
_cod_data_source_block           cu_2015087_0m
_cod_database_code               1545002
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C1(H1), C9(H9), C6(H6), C7(H7), C4(H4), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C30(H30), C29(H29)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C), C12(H12A,
 H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'