Minor Nortriterpenoids from the Twigs and Leaves of Rhododendron latoucheae.
Liu, Fei; Wang, Ya-Nan; Li, Yong; Ma, Shuang-Gang; Qu, Jing; Liu, Yun-Bao; Niu, Chang-Shan; Tang, Zhong-Hai; Li, Yu-Huan; Li, Li; Yu, Shi-Shan; Journal of natural products 81 (2018) 1721–1733; doi:10.1021/acs.jnatprod.7b01074

data_1553355
_publ_section_title
;
 Minor Nortriterpenoids from the Twigs and Leaves of Rhododendron
 latoucheae.
;
_journal_issue                   8
_journal_name_full               'Journal of natural products'
_journal_page_first              1721
_journal_page_last               1733
_journal_paper_doi               10.1021/acs.jnatprod.7b01074
_journal_volume                  81
_journal_year                    2018
_chemical_formula_moiety         'C29 H42 O3, 0.25(C H4 O)'
_chemical_formula_sum            'C29.25 H43 O3.25'
_chemical_formula_weight         446.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-12
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.902(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.884(3)
_cell_length_b                   7.0425(7)
_cell_length_c                   15.7032(17)
_cell_measurement_reflns_used    6304
_cell_measurement_temperature    106.3
_cell_measurement_theta_max      71.0140
_cell_measurement_theta_min      4.3149
_cell_volume                     4925.7(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      106.3
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -56.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  116.0000   -3.0000 39

  2 omega  -67.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  -37.0000   30.0000 59

  3 omega   40.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919 -116.0000   87.0000 44

  4 omega   42.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   37.0000 -120.0000 53

  5 omega  -31.00   56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000    0.0000 87

  6 omega   15.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   77.0000  -30.0000 68

  7 omega   63.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   37.0000 -180.0000 43

  8 omega   23.00   85.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919 -116.0000  -92.0000 62

  9 omega  -27.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000  -90.0000 81

 10 omega  -20.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000  120.0000 73

 11 omega   84.00  117.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -116.0000   87.0000 33

 12 omega   82.00  172.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 90

 13 omega   66.00   97.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 31

 14 omega  121.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 56

 15 omega   40.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 29

 16 omega   82.00  176.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 94

 17 omega   52.00  134.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -120.0000 82

 18 omega  106.00  175.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 69

 19 omega  106.00  175.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 69

 20 omega   43.00  142.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -163.0000  119.0000 99

 21 omega   64.00  131.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  120.0000 67

 22 omega   46.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 31

 23 omega   82.00  174.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 92

 24 omega   83.00  139.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 56

 25 omega   86.00  114.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -106.0000 -151.0000 28
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0182325000
_diffrn_orient_matrix_UB_12      0.1429115000
_diffrn_orient_matrix_UB_13      -0.0402297000
_diffrn_orient_matrix_UB_21      0.0204485000
_diffrn_orient_matrix_UB_22      -0.1626940000
_diffrn_orient_matrix_UB_23      -0.0169362000
_diffrn_orient_matrix_UB_31      -0.0211364000
_diffrn_orient_matrix_UB_32      -0.0333801000
_diffrn_orient_matrix_UB_33      -0.0911221000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17142
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.098
_diffrn_reflns_theta_min         4.318
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 3344 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9288
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.1140
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+63.3665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2516
_refine_ls_wR_factor_ref         0.2528
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                8930
_reflns_number_total             9288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np7b01074_si_001.cif
_cod_data_source_block           exp_4703
_cod_database_code               1553355
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.756
_shelx_hkl_checksum              39548
_shelx_res_checksum              76137
_shelx_shelxl_version_number     2014/7