Anti-neuroinflammatory asarone derivatives from the rhizomes of Acorus tatarinowii
Qin, Da-Peng; Feng, Xiao-Lin; Zhang, Wei-Yang; Gao, Hao; Cheng, Xiao-Rui; Zhou, Wen-Xia; Yu, Yang; Yao, Xin-Sheng; RSC Adv. 7 (2017) 8512–; doi:10.1039/C6RA27786A

data_7227550
_publ_section_title
;
 Anti-neuroinflammatory asarone derivatives from the rhizomes of Acorus
 tatarinowii
;
_journal_issue                   14
_journal_name_full               'RSC Adv.'
_journal_page_first              8512
_journal_paper_doi               10.1039/C6RA27786A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '2(C24 H34 O9), 3(H2 O), C H4 O, 1.9(O)'
_chemical_formula_sum            'C49 H78 O23.9'
_chemical_formula_weight         1049.51
_chemical_name_systematic        'asarolignan B'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-03-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.16 svn.r3037 for OlexSys, GUI svn.r4914)
;
_audit_update_record
;
2016-11-22 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3231(5)
_cell_length_b                   23.3774(6)
_cell_length_c                   16.4367(5)
_cell_measurement_reflns_used    4654
_cell_measurement_temperature    107.0
_cell_measurement_theta_max      29.5695
_cell_measurement_theta_min      2.9688
_cell_volume                     5503.6(3)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      107.0
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega  -69.00   -8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2647  -37.0000 -180.0000 61

  2 omega  -61.00  -36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2647  115.0000  166.0000 25

  3 omega   17.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2647   37.0000 -150.0000 32

  4 omega  -35.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2647  -77.0000  -90.0000 31

  5 omega  -49.00   28.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772  -37.0000 -120.0000 77

  6 omega  -61.00  -36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.1085  115.0000  -77.0000 25

  7 omega  -37.00    7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4210  -37.0000  -60.0000 44
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0260023000
_diffrn_orient_matrix_UB_12      -0.0013914000
_diffrn_orient_matrix_UB_13      -0.0366724000
_diffrn_orient_matrix_UB_21      0.0413879000
_diffrn_orient_matrix_UB_22      0.0048484000
_diffrn_orient_matrix_UB_23      -0.0226465000
_diffrn_orient_matrix_UB_31      0.0079207000
_diffrn_orient_matrix_UB_32      -0.0299273000
_diffrn_orient_matrix_UB_33      -0.0019709000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33662
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.635
_diffrn_reflns_theta_min         2.988
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85770
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       needle
_exptl_crystal_F_000             2253
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 3340 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12501
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0872P)^2^+1.1110P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1815
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.737
_reflns_number_gt                9471
_reflns_number_total             12501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra27786a2.cif
_cod_data_source_block           exp_2223
_cod_original_formula_sum        'C49 H78 O23.90'
_cod_database_code               7227550
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.985
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H23D-O22
 2 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(O1B)=0.9*(1-FVAR(2))
 Sof(O1A)=0.9*FVAR(2)
5.a Free rotating group:
 O20(H20A,H20B), O22(H22D,H22E), O23(H23D,H23E)
5.b Ternary CH refined with riding coordinates:
 C15(H15A), C39(H39), C27(H27), C3(H3), C38(H38), C14(H14), C2(H2A), C26(H26)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6A), C45(H45), C30(H30), C18(H18), C33(H33), C21(H21), C9(H9)
5.d Tetrahedral OH refined with riding coordinates:
 O11(H11), O2(H2)
5.e Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C46(H46A,H46B,H46C), C10(H10A,H10B,
 H10C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C22(H22A,
 H22B,H22C), C36(H36A,H36B,H36C), C47(H47A,H47B,H47C), C1(H1A,H1B,H1C),
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C12(H12A,H12B,
 H12C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
5.f Idealised tetrahedral OH refined as rotating group:
 O6(H6), O15(H15), O19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'