The crystal structure of C19H20O8
Lai, Bao-Long; Zhou, Hai-Ming; Chen, Zan-Hong; Chen, Hui-Ying; Zhang, Qin-Wen; Tao, Yi-Wen; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 175–177; doi:10.1515/ncrs-2021-0405

data_8104993
_publ_section_title
;
 The crystal structure of C19H20O8
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              175
_journal_page_last               177
_journal_paper_doi               10.1515/ncrs-2021-0405
_journal_volume                  237
_journal_year                    2022
_chemical_absolute_configuration .
_chemical_formula_moiety         'C19 H20 O8'
_chemical_formula_sum            'C19 H20 O8'
_chemical_formula_weight         376.35
_chemical_name_common            asperfumin
_chemical_name_systematic
;
methyl 3-hydroxy-6-(2-hydroxy-6-methoxy-4-methylbenzoyl)-2,5-dimethoxybenzoate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                81.252(4)
_cell_angle_beta                 81.500(4)
_cell_angle_gamma                77.890(4)
_cell_formula_units_Z            2
_cell_length_a                   7.0708(4)
_cell_length_b                   8.1261(4)
_cell_length_c                   16.1067(6)
_cell_measurement_reflns_used    4373
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.7150
_cell_measurement_theta_min      2.7800
_cell_volume                     887.88(8)
_computing_cell_refinement       'CrysAlis^Pro^, Ver. 1.171.38.43f [1]'
_computing_data_collection       'CrysAlis^Pro^, Ver. 1.171.38.43f [1]'
_computing_data_reduction        'CrysAlis^Pro^, Ver. 1.171.38.43f [1]'
_computing_molecular_graphics    'Olex2 1.3-alpha [4]'
_computing_publication_material  'Olex2 1.3-alpha [4]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT-2018/2  [2]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5703
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.960
_diffrn_reflns_theta_min         2.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Crystallogr. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_coef       0.0125(10)
_refine_ls_extinction_method     'SHELXL-2018/3 [3]'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0587P)^2^+0.3749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3217
_reflns_number_total             3448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0405_suppl.cif
_cod_data_source_block           sal
_cod_database_code               8104993
_shelx_estimated_absorpt_t_min   0.75717
_shelx_estimated_absorpt_t_max   1.00000