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_1545411
_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_formula_moiety         'C22 H22 O6'
_chemical_formula_sum            'C22 H22 O6'
_chemical_formula_weight         382.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.92797(19)
_cell_length_b                   14.3084(3)
_cell_length_c                   37.5013(19)
_cell_measurement_reflns_used    2854
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.5620
_cell_measurement_theta_min      4.7030
_cell_volume                     3717.4(2)
_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 10.3953
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega -115.00  -14.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676  -57.0000   30.0000 101

  2 omega -125.00  -91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000 -111.0000  150.0000 34

  3 omega   35.00   87.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -29.0000  177.0000 52

  4 omega   36.00  111.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   30.0000 75

  5 omega   49.00  157.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000    0.0000 108
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0169317000
_diffrn_orient_matrix_UB_12      -0.0036352000
_diffrn_orient_matrix_UB_13      -0.0409433000
_diffrn_orient_matrix_UB_21      -0.0808285000
_diffrn_orient_matrix_UB_22      -0.1000979000
_diffrn_orient_matrix_UB_23      0.0024250000
_diffrn_orient_matrix_UB_31      -0.2064249000
_diffrn_orient_matrix_UB_32      0.0395064000
_diffrn_orient_matrix_UB_33      0.0023996000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            7589
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         76.525
_diffrn_reflns_theta_min         4.717
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.4329
_exptl_crystal_size_mid          0.0656
_exptl_crystal_size_min          0.0358
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3745
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0596P)^2^+1.5833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3128
_reflns_number_total             3745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00839_si_002.cif
_cod_data_source_block           9
_cod_database_code               1545411
_chemical_oxdiff_formula         'C20 H21 O6'
_reflns_odcompleteness_completeness 98.60
_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, All O(H) groups
2. Restrained distances
 C21B-C12 \\sim C17-C12
 with sigma of 0.01
 C20B-C18B \\sim C19B-C18B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C21B) \\sim Ueq, Uanis(C17B) \\sim Ueq, Uanis(C18B) \\sim Ueq,
Uanis(C19B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C17B)=Sof(H17C)=Sof(C18B)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21B)=Sof(H21D)=Sof(H21E)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21B(H21D,H21E)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C6(H6), C7(H7), C11(H11), C15(H15), C18(H18), C17B(H17C)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C19B(H19A,H19B,H19C), C20B(H20D,H20E,H20F)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_shelx_res_checksum              1978
_shelx_hkl_checksum              21109
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'