Bioactive Sesquiterpenoids from the Peeled Stems of Syringa pinnatifolia.
Zhang, Ruifei; Feng, Xiao; Su, Guozhu; Mu, Zejing; Zhang, Hexinge; Zhao, Yanan; Jiao, Shungang; Cao, Lan; Chen, Suyile; Tu, Pengfei; Chai, Xingyun; Journal of natural products 81 (2018) 1711–1720; doi:10.1021/acs.jnatprod.7b01071

data_1553351
_publ_section_title
;
 Bioactive Sesquiterpenoids from the Peeled Stems of Syringa pinnatifolia.
;
_journal_issue                   8
_journal_name_full               'Journal of natural products'
_journal_page_first              1711
_journal_page_last               1720
_journal_paper_doi               10.1021/acs.jnatprod.7b01071
_journal_volume                  81
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H24 O2'
_chemical_formula_sum            'C15 H24 O2'
_chemical_formula_weight         236.34
_chemical_melting_point          432.8(4)
_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
_audit_creation_date             2017-09-07
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.02825(15)
_cell_length_b                   12.9002(4)
_cell_length_c                   17.5524(6)
_cell_measurement_reflns_used    1983
_cell_measurement_temperature    107.3
_cell_measurement_theta_max      70.7551
_cell_measurement_theta_min      3.4223
_cell_volume                     1364.97(7)
_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)/Bruker'
_diffrn_ambient_temperature      107.3
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -15.00   15.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  111.0000  -30.0000 30

  2 omega   21.00   48.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   45.0000  -90.0000 27

  3 omega  -26.00   53.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000 -180.0000 79

  4 omega   37.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.7919 -127.0000 -112.0000 49

  5 omega  -13.00  104.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.7919    0.0000   30.0000 117

  6 omega   47.00  111.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 64

  7 omega   45.00   98.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 53

  8 omega  105.00  130.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 25

  9 omega   42.00   96.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 54

 10 omega   44.00   89.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 45

 11 omega   91.00  176.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85

 12 omega   41.00   73.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 32

 13 omega   64.00  114.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -60.0000 50

 14 omega   73.00   98.00   1.0000    2.2000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0983315000
_diffrn_orient_matrix_UB_12      0.1054442000
_diffrn_orient_matrix_UB_13      -0.0235083000
_diffrn_orient_matrix_UB_21      -0.0132982000
_diffrn_orient_matrix_UB_22      -0.0320938000
_diffrn_orient_matrix_UB_23      -0.0843895000
_diffrn_orient_matrix_UB_31      -0.2351478000
_diffrn_orient_matrix_UB_32      0.0460174000
_diffrn_orient_matrix_UB_33      -0.0050123000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4476
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.017
_diffrn_reflns_theta_min         4.253
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96075
_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_colour            colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 932 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0468P)^2^+0.4002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                2429
_reflns_number_total             2586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np7b01071_si_003.cif
_cod_data_source_block           exp_5108
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '432.35-433.25 K' was
changed to '432.8(4)' -- the average value was taken and precision
was estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1553351
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.869
_shelx_hkl_checksum              6985
_shelx_res_checksum              42496
_shelx_shelxl_version_number     2014/7