Lineariifolianoids I-L, four rare sesquiterpene lactone dimers inhibiting NO production from Inula lineariifolia
Chen, Li-Ping; Wu, Guo-Zhen; Dong, Hong-yuan; Yang, Niao; Zhang, Weidong; Li, Hui-Liang; RSC Adv.  (2016) –; doi:10.1039/C6RA23092J

data_7226938
_publ_section_title
;
 Lineariifolianoids I-L, four rare sesquiterpene lactone dimers inhibiting
 NO production from Inula lineariifolia
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23092J
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C32 H40 O8'
_chemical_formula_sum            'C32 H40 O8'
_chemical_formula_weight         552.64
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.76710(10)
_cell_length_b                   17.4066(3)
_cell_length_c                   18.8236(4)
_cell_measurement_reflns_used    5477
_cell_measurement_temperature    130
_cell_measurement_theta_max      68.594
_cell_measurement_theta_min      3.458
_cell_volume                     2872.58(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      130
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18070
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.469
_diffrn_reflns_theta_min         3.458
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.4500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1598 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.5975.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 1983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.15(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.6730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                4915
_reflns_number_total             5176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23092j2.cif
_cod_data_source_block           cu_dm16471_0m
_cod_database_code               7226938
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.866
_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:
 C1(H1A), C2(H2), C2'(H2'), C3'(H3'), C7(H7), C7'(H7'), C8(H8), C8'(H8'),
 C10(H10), C10'(H10')
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6'(H6'A,H6'B), C9(H9A,H9B), C9'(H9'A,H9'B),
 C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6A)
2.d Idealised Me refined as rotating group:
 C2"(H2"A,H2"B,H2"C), C14(H14A,H14B,H14C), C14'(H14D,H14E,H14F), C15(H15A,H15B,
 H15C), C15'(H15D,H15E,H15F)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O6(H6)
;
_shelx_res_checksum              4754
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'