(±)-Quassidines I and J, Two Pairs of Cytotoxic Bis-β-carboline Alkaloid Enantiomers from Picrasma quassioides.
Jiao, Wei-Hua; Chen, Guo-Dong; Gao, Hao; Li, Jing; Gu, Bin-Bin; Xu, Ting-Ting; Yu, Hao-Bing; Shi, Guo-Hua; Yang, Fan; Yao, Xin-Sheng; Lin, Hou-Wen; Journal of natural products 78 (2015) 125–130; doi:10.1021/np500801s

data_1518453
_publ_section_title
;
 (+-)-Quassidines I and J, Two Pairs of Cytotoxic Bis-\b-carboline
 Alkaloid Enantiomers from Picrasma quassioides.
;
_journal_issue                   1
_journal_name_full               'Journal of natural products'
_journal_page_first              125
_journal_page_last               130
_journal_paper_doi               10.1021/np500801s
_journal_volume                  78
_journal_year                    2015
_chemical_formula_moiety         'C29 H27 N4 O3, C2 F3 O2, C H4 O'
_chemical_formula_sum            'C32 H31 F3 N4 O6'
_chemical_formula_weight         624.61
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.1062(3)
_cell_length_b                   28.1062(3)
_cell_length_c                   14.7090(2)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    140.15
_cell_measurement_theta_max      69.14
_cell_measurement_theta_min      4.63
_cell_volume                     11619.5(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28762
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.726
_diffrn_reflns_theta_min         4.627
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0748 before and 0.0412 after correction.
The Ratio of minimum to maximum transmission is 0.8546.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             5216
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+18.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4995
_reflns_number_total             5416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np500801s_si_002.cif
_cod_data_source_block           cu_dm13186_0m
_cod_depositor_comments          'Adding full bibliography for 1518453.cif.'
_cod_original_cell_volume        11619.5(3)
_cod_database_code               1518453
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 N9(H9), N9'(H9'), C3(H3), C5(H5), C6(H6), C7(H7), C3'(H3'), C5'(H5'),
 C6'(H6'), C7'(H7'), C8'(H8')
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C1S(H1SA,H1SB,
 H1SC)
2.e Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              26116
_shelx_hkl_checksum              64447
_olex2_submission_special_instructions 'No special instructions were received'