(±)-Uncarilins A and B, Dimeric Isoechinulin-Type Alkaloids from Uncaria rhynchophylla
Geng, Chang-An; Huang, Xiao-Yan; Ma, Yun-Bao; Hou, Bo; Li, Tian-Ze; Zhang, Xue-Mei; Chen, Ji-Jun; Journal of Natural Products  (2017) –; doi:10.1021/acs.jnatprod.6b00938

data_1545310
_publ_section_title
;
 (+-)-Uncarilins A and B, Dimeric Isoechinulin-Type Alkaloids from Uncaria
 rhynchophylla
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.6b00938
_journal_year                    2017
_chemical_formula_moiety         'C38 H42 N6 O4, 0.5(C2 H3 N), 0.5(H2 O)'
_chemical_formula_sum            'C39 H44.5 N6.5 O4.5'
_chemical_formula_weight         676.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                77.6050(10)
_cell_angle_beta                 80.4720(10)
_cell_angle_gamma                76.4160(10)
_cell_formula_units_Z            4
_cell_length_a                   10.7266(2)
_cell_length_b                   15.3359(3)
_cell_length_c                   22.6051(4)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.03
_cell_measurement_theta_min      3.02
_cell_volume                     3504.26(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53555
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.406
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.7533
_exptl_transmission_factor_min   0.5181
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         12491
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1924P)^2^+2.1331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10855
_reflns_number_total             12491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00938_si_001.cif
_cod_data_source_block           cu_jad8a_0m
_cod_depositor_comments
;

2019-08-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H89 N13 O9'
_cod_original_formula_weight         1352.62
_cod_original_formula_moiety         '2(C38 H42 N6 O4), C2 H3 N, H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3504.26(12)
_cod_database_code               1545310
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.716
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              35032
_shelx_hkl_checksum              35942