Carapanins A–C: new limonoids from andiroba (Carapa guianensis) fruit oil
Kikuchi, Takashi; Akita, Keiko; Koike, Hiroki; In, Yasuko; Yamada, Takeshi; Tanaka, Reiko; Organic & Biomolecular Chemistry 18 (2020) 9268–9274; doi:10.1039/D0OB01872D

data_7157793
_publ_section_title
;
 Carapanins A--C: new limonoids from andiroba (Carapa guianensis) fruit
 oil
;
_journal_issue                   45
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              9268
_journal_page_last               9274
_journal_paper_doi               10.1039/D0OB01872D
_journal_volume                  18
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C35 H46 O13'
_chemical_formula_weight         674.71
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
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_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-06 deposited with the CCDC.	2020-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
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_cell_length_a                   11.09130(10)
_cell_length_b                   11.09130(10)
_cell_length_c                   92.9928(5)
_cell_measurement_reflns_used    48640
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.3
_cell_measurement_theta_min      2.84
_cell_volume                     9907.06(14)
_computing_cell_refinement       'CrysalisPro (Agilent Technologies,     )'
_computing_data_collection       'CrysalisPro (Agilent Technologies,     )'
_computing_data_reduction        'CrysalisPro (Agilent Technologies,     )'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Agilent Technologies XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       115
_diffrn_reflns_limit_l_min       -115
_diffrn_reflns_number            13315
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.507
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 5682 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13315
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_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+46.3464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                13173
_reflns_number_total             13315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01872d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        9907.06(19)
_cod_original_formula_sum        'C70 H92 O26'
_cod_original_formula_units_Z    6
_cod_original_formula_weight     1349.43
_cod_database_code               7157793
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.889
_shelx_res_checksum              63376