Deciphering composition and connectivity of a natural product with the assistance of MS and 2D NMR
Vinokur, Anastasiya I.; White, Paul B.; Fotsing, Maurice Tagatsing; Arderne, Charmaine; Ndinteh, Derek Tantoh; Vestling, Martha M.; Guzei, Ilia A.; Acta Crystallographica Section C 73 (2017) 994–1002; doi:10.1107/S2053229617014966

data_2020925
_publ_section_title
;
 Deciphering composition and connectivity of a natural product with the
 assistance of MS and 2D NMR
;
_journal_coeditor_code           QS3066
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              994
_journal_page_last               1002
_journal_paper_doi               10.1107/S2053229617014966
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '2C22 H18 O6, C25 H28 O4, 0.13C2 H6 O'
_chemical_formula_moiety         '2(C22 H18 O6), C25 H28 O4, 0.13(C2 H6 O)'
_chemical_formula_sum            'C69.27 H64.81 O16.14'
_chemical_formula_weight         1155.42
_chemical_name_systematic
;3-(2<i>H</i>-1,3-Benzodioxol-5-yl)-6-methoxy-8,8-dimethyl-4<i>H</i>,8<i>H</i>-pyrano[2,3-<i>h</i>]chromen-4-one--
(2<i>E</i>)-1-(4-{[(2<i>E</i>)-3,7-dimethylocta-2,6-dien-1-yl]oxy}-2-hydroxyphenyl)-3-(4-hydroxyphenyl)prop-2-en-1-one--ethanol (2/1/0.13)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                80.12(3)
_cell_angle_beta                 89.69(3)
_cell_angle_gamma                68.02(3)
_cell_formula_units_Z            2
_cell_length_a                   12.519(3)
_cell_length_b                   12.594(3)
_cell_length_c                   19.975(4)
_cell_measurement_reflns_used    6163
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.195
_cell_measurement_theta_min      2.473
_cell_volume                     2871.2(13)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42663
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.470
_diffrn_reflns_theta_min         1.037
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1219
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.547
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         11806
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+0.7244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                7371
_reflns_number_total             11806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qs3066sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2871.3(12)
_cod_database_code               2020925
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.998
_shelx_hkl_checksum              98861
_shelx_res_checksum              99231
_cod_database_fobs_code 2020925