Cynarine monohydrate from synchrotron powder X-ray diffraction data
Kaduk, James A.; Boaz, Nicholas C.; Markun, Emma L.; Gindhart, Amy M.; Blanton, Thomas N.; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S2053229622000687

data_2022527
_publ_section_title
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 Cynarine monohydrate from synchrotron powder X-ray diffraction data
;
_journal_coeditor_code           CU3179
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622000687
_journal_volume                  78
_journal_year                    2022
_chemical_formula_analytical     C25H26O13
_chemical_formula_iupac          'C25 H24 O12, H2 O'
_chemical_formula_moiety         'C25 H24 O12, H2 O'
_chemical_formula_structural     (C25H24O12)(H2O)
_chemical_formula_sum            'C25 H26 O13'
_chemical_formula_weight         534.47
_chemical_name_common            'cynarine monohydrate'
_chemical_name_systematic
'1,3-Bis{[(<i>E</i>)-3-(3,4-dihydroxyphenyl)prop-2-enoyl]oxy}-4,5-dihydroxycyclohexane-1-carboxylic acid monohydrate'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           'created in GSAS-II'
_cell_angle_alpha                90
_cell_angle_beta                 94.9763(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.88124(12)
_cell_length_b                   15.36081(4)
_cell_length_c                   5.59335(2)
_cell_volume                     1188.158(12)
_computing_molecular_graphics    'Mercury, Diamond'
_computing_publication_material  publCIF
_computing_structure_refinement
;
GSAS-II (Toby & Von Dreele, 2013)
;
_computing_structure_solution    FOX
_diffrn_ambient_temperature      295
_diffrn_detector                 'multiple scintillation counters'
_diffrn_measurement_device_type
'11-BM, Advanced Photon Source, Argonne National Laboratory'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.45815
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.009
_exptl_crystal_density_diffrn    1.4939
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  tan
_pd_instr_dist_spec/anal         1000
_pd_instr_location               '11-BM, APS, Argonne National Laboratory'
_pd_meas_2theta_range_inc        0.00100
_pd_meas_2theta_range_max        49.99654
_pd_meas_2theta_range_min        0.50000
_pd_meas_number_of_points        49575
_pd_meas_scan_method             step
_pd_phase_name                   'cynarine hydrate, C25 H24 O12 (H2 O)'
_pd_proc_info_datetime           2021-09-19T15:39
_pd_proc_info_excluded_regions
;
0.5-1.8 and 30-50
;
_pd_proc_ls_background_function
;
Background function: "chebyschev-1" function with 12 terms:
    162.64(21), -76.0(3), 19.23(28), -0.00(28), -10.09(26), -3.82(25),
    18.77(23), -18.02(24), 22.04(22), -19.66(22), 8.17(19), 0.80(16),
;
_pd_proc_ls_pref_orient_corr
;
Simple spherical harmonic correction Order = 2
    Coefficients:  0:0:C(2,-2) = 0.1271(31); 0:0:C(2,0) = 0.050(4);
    0:0:C(2,2) = 0.0186(27);
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_pd_proc_ls_profile_function
;
Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L:
  peak variance(Gauss) = Utan(Th)^2^+Vtan(Th)+W:
  peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L
  U, V, W in (centideg)^2^, X & Y in centideg
    1.163, -0.126, 0.063, 0.000, 0.000, 0.002,
  Crystallite size in microns with "isotropic" model:
  parameters: Size, G/L mix
    1.000, 1.000,
  Microstrain, "generalized" model (10^6^ * delta Q/Q)
  parameters: S400, S040, S004, S220, S202, S022, S301, S103, S121, G/L mix
    256.163, 72.076, 15203.783, 86.451, 2030.750, 984.854, 953.498,
    297.185, -466.993, 1.000,
;
_pd_proc_ls_prof_R_factor        0.05663
_pd_proc_ls_prof_wR_expected     0.05885
_pd_proc_ls_prof_wR_factor       0.07008
_pd_spec_mounting                'Kapton capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              3.0
_pd_spec_size_equat              1.5
_pd_spec_size_thick              1.5
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.246
_refine_ls_goodness_of_fit_all   1.226
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     146
_refine_ls_number_restraints     95
_refine_ls_shift/su_max          0.9104
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.07197
_reflns_number_total             1881
_cod_data_source_file            cu3179sup1.cif
_cod_data_source_block           cynarine_5
_cod_original_cell_volume        1188.158(6)
_cod_database_code               2022527
_cod_database_fobs_code 2022527