NMR Structure Elucidation of Naphthoquinones from Quambalaria cyanescens
Procházková, Eliška; Kucherak, Oleksandr; Stodůlková, Eva; Tošner, Zdeněk; Císařová, Ivana; Flieger, Miroslav; Kolařík, Miroslav; Baszczyňski, Ondřej; Journal of Natural Products  (2020) –; doi:10.1021/acs.jnatprod.0c00930

data_1559813
_publ_section_title
;
 NMR Structure Elucidation of Naphthoquinones from Quambalaria cyanescens
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.0c00930
_journal_year                    2020
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C16 H16 O6, O'
_chemical_formula_sum            'C16 H16 O7'
_chemical_formula_weight         320.29
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                68.899(3)
_cell_angle_beta                 86.272(3)
_cell_angle_gamma                81.935(3)
_cell_formula_units_Z            12
_cell_length_a                   10.4098(5)
_cell_length_b                   21.2446(11)
_cell_length_c                   21.6607(12)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.3720
_cell_measurement_theta_min      2.1866
_cell_volume                     4424.4(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52063
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        64.995
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_min         2.186
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            red-yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1269
_refine_ls_number_reflns         14994
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.2350
_refine_ls_R_factor_gt           0.1091
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2562
_refine_ls_wR_factor_ref         0.3120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5384
_reflns_number_total             14994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00930_si_002.cif
_cod_data_source_block           cu_mk_w3a_flieger
_cod_database_code               1559813
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              32480
_shelx_hkl_checksum              7180