Highly Oxygenated Triterpenoids and Rare Tetraterpenoids from <i>Abies chensiensis</i> and Their Antibacterial Activity.
Wei, Wen-Jun; Song, Qiu-Yan; Ying, Jin-Chuan; Li, Hang-Ying; Ma, Kai-Liang; Li, Yida; Li, Ya; Gao, Kun; Journal of natural products 82 (2019) 2859–2869; doi:10.1021/acs.jnatprod.9b00616

data_1552568
_publ_section_title
;
 Highly Oxygenated Triterpenoids and Rare Tetraterpenoids from <i>Abies
 chensiensis</i> and Their Antibacterial Activity.
;
_journal_issue                   10
_journal_name_full               'Journal of natural products'
_journal_page_first              2859
_journal_page_last               2869
_journal_paper_doi               10.1021/acs.jnatprod.9b00616
_journal_volume                  82
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H48 O4'
_chemical_formula_sum            'C30 H48 O4'
_chemical_formula_weight         472.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3328(3)
_cell_length_b                   16.9299(8)
_cell_length_c                   21.8307(9)
_cell_measurement_reflns_used    4785
_cell_measurement_temperature    295.72(11)
_cell_measurement_theta_max      68.7640
_cell_measurement_theta_min      6.8480
_cell_volume                     2710.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.72(11)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   19.0000  -90.0000 28

  2 omega  -57.00   15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   19.0000  -90.0000 72

  3 omega    2.00   41.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 39

  4 omega   79.00  119.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 40

  5 omega   65.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 27

  6 omega   21.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   79.0000 -121.3684 26

  7 omega   34.00   69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   59.0000 -170.3608 35

  8 omega   46.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 45

  9 omega   44.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   90.0000 44

 10 omega   64.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000 -120.0000 26

 11 omega   37.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000    0.0000 26

 12 omega   53.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   30.0000 26

 13 omega   42.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -103.0000 -173.0000 26

 14 omega   83.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -103.0000 -173.0000 29

 15 omega   79.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 35

 16 omega   50.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 26

 17 omega   78.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000 -120.0000 99

 18 omega   40.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  150.0000 62

 19 omega   40.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 25

 20 omega   35.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 58

 21 omega   48.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -60.0000 26

 22 omega   51.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -60.0000 26

 23 omega  141.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   30.0000 34

 24 omega   47.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   30.0000 35

 25 omega  -79.00   15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  -50.0000   60.0000 94

 26 omega  -17.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  150.0000 103

 27 omega   27.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  -60.0000 100

 28 omega  -20.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  150.0000 148

 29 omega   20.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   81.0000  -50.0758 26

 30 omega  -15.00   76.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -30.0000 91

 31 omega   68.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000    0.0000 80
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0153702000
_diffrn_orient_matrix_UB_12      -0.0459412000
_diffrn_orient_matrix_UB_13      -0.0607006000
_diffrn_orient_matrix_UB_21      0.0777364000
_diffrn_orient_matrix_UB_22      -0.0741170000
_diffrn_orient_matrix_UB_23      0.0315233000
_diffrn_orient_matrix_UB_31      -0.1945594000
_diffrn_orient_matrix_UB_32      -0.0259793000
_diffrn_orient_matrix_UB_33      0.0174125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17156
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         4.05
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.113
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.1733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                3880
_reflns_number_total             4782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np9b00616_si_004.cif
_cod_data_source_block           ac_1_30
_cod_original_cell_volume        2710.2(2)
_cod_database_code               1552568
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C15(H15), C17(H17), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,
 H12B), C16(H16A,H16B), C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_date_sample_data_collection 2018-09-17
_olex2_submission_special_instructions 'No special instructions were received'