Synergistic use of NMR computation and quantitative interproton distance analysis in the structural determination of neokadcoccitane A, a rearranged triterpenoid featuring an aromatic ring D from Kadsura coccinea
Xu, Hou-Chao; Hu, Kun; Shi, Xiao-Huo; Tang, Jian-Wei; Li, Xiao-Nian; Sun, Han-Dong; Puno, Pema-Tenzin; Organic Chemistry Frontiers 6 (2019) 1619–; doi:10.1039/C9QO00281B

data_1554823
_publ_section_title
;
 Synergistic use of NMR computation and quantitative interproton distance
 analysis in the structural determination of neokadcoccitane A, a
 rearranged triterpenoid featuring an aromatic ring D from Kadsura
 coccinea
;
_journal_issue                   10
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1619
_journal_paper_doi               10.1039/C9QO00281B
_journal_volume                  6
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H40 O4'
_chemical_formula_sum            'C27 H40 O4'
_chemical_formula_weight         428.59
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-26 deposited with the CCDC.	2019-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0610(2)
_cell_length_b                   10.8588(2)
_cell_length_c                   27.7356(6)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.13
_cell_measurement_theta_min      4.37
_cell_volume                     2427.77(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.986
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14256
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.195
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.930
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.5221
_exptl_transmission_factor_min   0.1803
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1757 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.19(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0612P)^2^+0.4221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                4383
_reflns_number_total             4413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00281b2.cif
_cod_data_source_block           cu_skr45_0m
_cod_original_cell_volume        2427.78(9)
_cod_database_code               1554823
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.603
_shelx_estimated_absorpt_t_max   0.915
_shelx_res_checksum              76956
_shelx_hkl_checksum              82911