Flavonoids from Erythrina schliebenii.
Nyandoro, Stephen S.; Munissi, Joan J. E.; Kombo, Msim; Mgina, Clarence A.; Pan, Fangfang; Gruhonjic, Amra; Fitzpatrick, Paul; Lu, Yu; Wang, Bin; Rissanen, Kari; Erdélyi, Máté; Journal of natural products 80 (2017) 377–383; doi:10.1021/acs.jnatprod.6b00839

data_1545410
_publ_section_title
;
 Flavonoids from Erythrina schliebenii.
;
_journal_issue                   2
_journal_name_full               'Journal of natural products'
_journal_page_first              377
_journal_page_last               383
_journal_paper_doi               10.1021/acs.jnatprod.6b00839
_journal_volume                  80
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H20 O6'
_chemical_formula_sum            'C19 H20 O6'
_chemical_formula_weight         344.35
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.571(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3072(2)
_cell_length_b                   8.03313(19)
_cell_length_c                   12.8765(3)
_cell_measurement_reflns_used    4318
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.5010
_cell_measurement_theta_min      5.5040
_cell_volume                     841.82(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -26.00    9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7216  -77.0000  -90.0000 35

  2 omega -135.00  -88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7216  -77.0000  -90.0000 47

  3 omega  -85.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7216  -77.0000  -90.0000 51

  4 omega -134.00  -87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7216  -99.0000 -150.0000 47

  5 omega  -81.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7216   70.0000 -170.0000 116

  6 omega   56.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.7216   70.0000 -170.0000 25

  7 omega -176.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -74.0705  -50.0000  -60.0000 159

  8 omega  -48.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -74.0705   37.0000 -120.0000 76

  9 omega  -49.00   22.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -74.0705   25.0000  -30.0000 71

 10 omega -136.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -74.0705  -12.0000  -30.0000 167

 11 omega  127.00  168.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0705  111.0000 -150.0000 41

 12 omega  116.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0705   77.0000  -90.0000 61

 13 omega  148.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0705  111.0000 -120.0000 30

 14 omega  102.00  136.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0705  111.0000 -120.0000 34

 15 omega  126.00  176.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0705  111.0000  -30.0000 50

 16 omega  -43.00   17.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -86.5000   43.0000    0.0000 60

 17 omega   20.00   89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195   21.0000 -120.0000 69

 18 omega   91.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  138.0000  -90.0000 39

 19 omega   67.00  169.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195   54.0000  -90.0000 102

 20 omega   14.00  140.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  -70.0000   57.0000 126

 21 omega  105.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  104.0000   90.0000 73

 22 omega   15.00  108.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195 -104.0000   60.0000 93

 23 omega  103.00  148.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  104.0000  120.0000 45

 24 omega  153.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  138.0000  -90.0000 25

 25 omega   56.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195   43.0000  -30.0000 114

 26 omega   14.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  -32.0000   60.0000 58

 27 omega  110.00  168.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195   21.0000 -120.0000 58

 28 omega   89.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  138.0000  120.0000 89

 29 omega  146.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      122.4195  -70.0000   57.0000 31
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1061937000
_diffrn_orient_matrix_UB_12      -0.0839100000
_diffrn_orient_matrix_UB_13      -0.0978202000
_diffrn_orient_matrix_UB_21      0.0628248000
_diffrn_orient_matrix_UB_22      0.1263944000
_diffrn_orient_matrix_UB_23      -0.0726399000
_diffrn_orient_matrix_UB_31      0.1434640000
_diffrn_orient_matrix_UB_32      -0.1173918000
_diffrn_orient_matrix_UB_33      -0.0083507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4520
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         73.666
_diffrn_reflns_theta_min         7.020
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 1412 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3211
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0531P)^2^+0.1215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                3187
_reflns_number_total             3211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00839_si_004.cif
_cod_data_source_block           21
_cod_database_code               1545410
_chemical_oxdiff_formula         'C19 H20 O6'
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.545
_reflns_odcompleteness_completeness 97.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C12(H12), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              97576
_shelx_hkl_checksum              3166
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'