Synthetic Studies toward 5,6,7,3',4'-Monomethoxytetrahydroxyflavones: Synthesis of Pedalitin.
Kamma, Koteswara Rao; Cho, Joungmo; Won, Hyo Jun; Nam, So-Yeon; Le, Ngan Hong; Jung, Je Hyeong; Lee, Kee-In; Molecules (Basel, Switzerland) 29 (2024) 513–; doi:10.3390/molecules29020513

data_1570918
_publ_section_title
;
 Synthetic Studies toward 5,6,7,3',4'-Monomethoxytetrahydroxyflavones:
 Synthesis of Pedalitin.
;
_journal_issue                   2
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              513
_journal_paper_doi               10.3390/molecules29020513
_journal_volume                  29
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_sum            'C19 H18 O8'
_chemical_formula_weight         374.33
_chemical_name_common            Bat-intermediate-down
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2312(19)
_cell_length_b                   16.306(3)
_cell_length_c                   12.099(3)
_cell_measurement_reflns_used    4917
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      27.4284
_cell_measurement_theta_min      2.4982
_cell_volume                     1623.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'f and w scans'
_diffrn_radiation_monochromator  'Graphite crystal'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22072
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.206
_refine_ls_abs_structure_details
;

Flack x determined using 1185 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0432P)^2^+0.7303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                3236
_reflns_number_total             3543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4_CIF.cif
_cod_data_source_block           20220418LT
_cod_database_code               1570918
_shelx_res_checksum              94581
_shelx_hkl_checksum              52552