Diterpenoids from Euphorbia dulcis with Potassium Ion Channel Inhibitory Activity with Selective G Protein-Activated Inwardly Rectifying Ion Channel (GIRK) Blocking Effect.
Kúsz, Norbert; Orvos, Péter; Bereczki, Laura; Fertey, Pierre; Bombicz, Petra; Csorba, Attila; Tálosi, László; Jakab, Gusztáv; Hohmann, Judit; Rédei, Dóra; Journal of natural products 81 (2018) 2483–2492; doi:10.1021/acs.jnatprod.8b00500

data_1553398
_publ_section_title
;
 Diterpenoids from Euphorbia dulcis with Potassium Ion Channel Inhibitory
 Activity with Selective G Protein-Activated Inwardly Rectifying Ion
 Channel (GIRK) Blocking Effect.
;
_journal_issue                   11
_journal_name_full               'Journal of natural products'
_journal_page_first              2483
_journal_page_last               2492
_journal_paper_doi               10.1021/acs.jnatprod.8b00500
_journal_volume                  81
_journal_year                    2018
_chemical_formula_moiety         'C36 H48 O9'
_chemical_formula_sum            'C36 H48 O9'
_chemical_formula_weight         624.74
_chemical_name_common            EUD15
_chemical_name_systematic        EUD15
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.024(3)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   14.1355(4)
_cell_length_b                   18.3034(4)
_cell_length_c                   20.5777(6)
_cell_measurement_reflns_used    31964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9450
_cell_measurement_theta_min      1.7040
_cell_volume                     5284.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (Sheldrick, G.M. (2008). Acta Cryst. A64,112-122)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'PILATUS 6M'
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f      0.00 360.00   0.10    0.50   0.00   0.00   0.00    --  3600
;
_diffrn_measurement_device
;SOLEIL PROXIMA 1 beamline
3 circle \k goniostat (10 \mm sphere of confusion)
;
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator
;
Kirkpatrick-Baez pair of bi-morph mirrors plus channel 
cut cryogenically cooled monochromator crystal
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79990
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55224
_diffrn_reflns_point_group_measured_fraction_full 0.95
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         31.198
_diffrn_reflns_theta_min         1.682
_diffrn_source
;U20 In-vacuum undulator
beam size HxV = 40 x 30 \mm^2^
;
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 7135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(5)
_refine_ls_extinction_coef       0.0017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         19397
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.167
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1316P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.793
_reflns_number_gt                17001
_reflns_number_total             19397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np8b00500_si_002.cif
_cod_data_source_block           F:\EUD15
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2022-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_moiety     '3(C36 H48 O9)'
_cod_original_formula_sum        'C108 H144 O27'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1874.22
_cod_database_code               1553398
_shelx_shelxl_version_number     2014/7
_oxdiff_exptl_absorpt_empirical_full_min 0.379
_oxdiff_exptl_absorpt_empirical_full_max 2.833
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              28404
_shelx_hkl_checksum              9736