New bioactive cyclopeptide alkaloids with rare terminal unit from the root bark of Ziziphus cambodiana
Lomchoey, Natthakaln; Panseeta, Panomwan; Boonsri, Pornthip; Apiratikul, Nuttapon; Prabpai, Samran; Kongsaeree, Palangpon; Suksamrarn, Sunit; RSC Advances 8 (2018) 18204–; doi:10.1039/C7RA13050C

data_7230662
_publ_section_title
;
 New bioactive cyclopeptide alkaloids with rare terminal unit from the
 root bark of Ziziphus cambodiana
;
_journal_issue                   33
_journal_name_full               'RSC Advances'
_journal_page_first              18204
_journal_paper_doi               10.1039/C7RA13050C
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_compound_source        'Ziziphus cambodiana'
_chemical_formula_moiety         'C37 H36 N4 O4, H2O'
_chemical_formula_sum            'C37 H38 N4 O5'
_chemical_formula_weight         618.74
_chemical_melting_point          135
_chemical_name_common            'Cambodine E'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-18
_audit_update_record
;
2016-05-02 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3830(1)
_cell_length_b                   9.5920(1)
_cell_length_c                   40.1370(7)
_cell_measurement_reflns_used    4117
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.200
_cell_measurement_theta_min      0.998
_cell_volume                     3227.41(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_device_type  'nonius kappaccd'
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            7931
_diffrn_reflns_theta_full        28.7018
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312.5361
_exptl_crystal_preparation       'slow evaperate'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.1910
_refine_diff_density_min         -0.1709
_refine_diff_density_rms         0.0374
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             7.1037
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0416
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    69
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0416
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.6761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.913
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              54
_reflns_limit_l_min              -53
_reflns_number_gt                7250
_reflns_number_total             7921
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ra13050c2.cif
_cod_data_source_block           shelxl
_cod_database_code               7230662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N3(H3), N6(H6)
2.b Ternary CH refined with riding coordinates:
 C27(H27), C8(H8), C9(H9), C5(H5)
2.c Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b), C17(H17a,H17b), C29(H29a,H29b)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C35(H35), C31(H31), C32(H32), C38(H38), C12(H12), C19(H19),
 C34(H34), C33(H33), C41(H41), C15(H15), C16(H16), C20(H20), C39(H39), C22(H22),
  C42(H42), C40(H40), C21(H21), C23(H23), C13(H13)
2.e Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c)
;
_olex2_submission_special_instructions 'No special instructions were received'