The crystal structure of 3-oxo-urs-12-en-28-oic acid, C30H46O3·1/6H2O
Wang, Xiao-Hui; Wang, Hui-yun; Wang, Jia-Zhen; Zhang, Mei; Chen, Xiao-Qian; Zhao, Feng-Lan; Meng, Qing-Guo; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1–5; doi:10.1515/ncrs-2020-0423

data_8104866
_publ_section_title
;
 The crystal structure of 3-oxo-urs-12-en-28-oic acid,
 C30H46O3&#x00B7;1/6H2O
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1
_journal_page_last               5
_journal_paper_doi               10.1515/ncrs-2020-0423
_journal_volume                  236
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H46 O3,0.167(H2O)'
_chemical_formula_sum            'C30 H46.234 O3.167'
_chemical_formula_weight         457.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 104.4652(12)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   29.4307(4)
_cell_length_b                   15.42797(17)
_cell_length_c                   18.4667(2)
_cell_measurement_reflns_used    16160
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.7530
_cell_measurement_theta_min      4.2940
_cell_volume                     8119.11(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4674
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     32.00 110.00   1.00    4.50    --   42.08  38.00-120.00   78
  2  \w     17.00 108.00   1.00    4.50    --   42.08  57.00 150.00   91
  3  \w     25.00  51.00   1.00    4.50    --   42.08-125.00 -90.00   26
  4  \w    138.00 169.00   1.00   14.00    --   92.50  30.00  60.00   31
  5  \w    120.00 168.00   1.00   14.00    --   92.50  30.00   0.00   48
  6  \w     22.00  57.00   1.00   14.00    --   92.50 -61.00 -90.00   35
  7  \w    109.00 140.00   1.00   14.00    --   92.50  61.00 -90.00   31
  8  \w     95.00 121.00   1.00   14.00    --   92.50 -91.00 -18.72   26
  9  \w     68.00 160.00   1.00   14.00    --   92.50  61.00-150.00   92
 10  \w     71.00  97.00   1.00   14.00    --   92.50 128.00 -37.00   26
 11  \w    135.00 161.00   1.00   14.00    --   92.50 128.00 -37.00   26
 12  \w     19.00  82.00   1.00   14.00    --   92.50-125.00-150.00   63
 13  \w     67.00  93.00   1.00   14.00    --   92.50  61.00-180.00   26
 14  \w     71.00 122.00   1.00   14.00    --   92.50 -61.00 -90.00   51
 15  \w     62.00  87.00   1.00   14.00    --   92.50-125.00-120.00   25
 16  \w     16.00  89.00   1.00   14.00    --   92.50 -30.00 -90.00   73
 17  \w     41.00  68.00   1.00   14.00    --   92.50 -91.00-127.91   27
 18  \w     94.00 119.00   1.00   14.00    --   92.50 -91.00-127.91   25
 19  \w     21.00  46.00   1.00   14.00    --   92.50 -91.00 -82.47   25
 20  \w     59.00  85.00   1.00   14.00    --   92.50 -91.00 -82.47   26
 21  \w     94.00 130.00   1.00   14.00    --   92.50 -91.00 -82.47   36
 22  \w     27.00  53.00   1.00   14.00    --   92.50 -91.00 -18.72   26
 23  \w     76.00 111.00   1.00   14.00    --   92.50 125.00  90.00   35
 24  \w     35.00  88.00   1.00   14.00    --   92.50 -45.00  60.00   53
 25  \w     23.00  49.00   1.00   14.00    --   92.50 -45.00 150.00   26
 26  \w     67.00  92.00   1.00   14.00    --   92.50 -45.00 150.00   25
 27  \w     63.00  98.00   1.00   14.00    --   92.50  61.00 -90.00   35
 28  \w    111.00 137.00   1.00   14.00    --   92.50  61.00-180.00   26
 29  \w     63.00  88.00   1.00   14.00    --   92.50  61.00  90.00   25
 30  \w     88.00 114.00   1.00   14.00    --   92.50  30.00  60.00   26
 31  \w     92.00 117.00   1.00   14.00    --   92.50  45.00 120.00   25
 32  \w     98.00 125.00   1.00   14.00    --   92.50 -83.00-107.37   27
 33  \w     48.00  74.00   1.00   14.00    --   92.50 -45.00   0.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146636000
_diffrn_orient_matrix_UB_12      -0.0800222000
_diffrn_orient_matrix_UB_13      -0.0504120000
_diffrn_orient_matrix_UB_21      0.0519745000
_diffrn_orient_matrix_UB_22      -0.0196042000
_diffrn_orient_matrix_UB_23      0.0045835000
_diffrn_orient_matrix_UB_31      0.0026791000
_diffrn_orient_matrix_UB_32      -0.0564470000
_diffrn_orient_matrix_UB_33      0.0696823000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34354
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        66.816
_diffrn_reflns_theta_max         66.816
_diffrn_reflns_theta_min         3.450
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 4144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_extinction_coef       0.00035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         12647
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0698P)^2^+1.2820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.696
_reflns_Friedel_fraction_full    0.751
_reflns_Friedel_fraction_max     0.751
_reflns_number_gt                11372
_reflns_number_total             12647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0423_suppl.cif
_cod_data_source_block           ua2-2
_cod_database_code               8104866
_chemical_oxdiff_formula         'C1 H1 O1'
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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:
 C5(H5), C9(H9), C18(H18), C19(H19), C20(H20), C5B(H5B), C9B(H9B), C18B(H18B),
 C19B(H19B), C20B(H20B), C5C(H5C), C9C(H9C), C18C(H18C), C19C(H19C), C20C(H20C)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11E,H11F), C15(H15E,
 H15F), C16(H16E,H16F), C21(H21E,H21F), C22(H22E,H22F), C1B(H1BA,H1BB),
 C2B(H2BA,H2BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB), C11B(H11C,H11D), C15B(H15C,
 H15D), C16B(H16C,H16D), C21B(H21C,H21D), C22B(H22C,H22D), C1C(H1CA,H1CB),
 C2C(H2CA,H2CB), C6C(H6CA,H6CB), C7C(H7CA,H7CB), C11C(H11A,H11B), C15C(H15A,
 H15B), C16C(H16A,H16B), C21C(H21A,H21B), C22C(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C12B(H12B), C12C(H12C)
2.d Idealised Me refined as rotating group:
 C23(H23G,H23H,H23I), C24(H24G,H24H,H24I), C25(H25G,H25H,H25I), C26(H26G,H26H,
 H26I), C27(H27G,H27H,H27I), C29(H29G,H29H,H29I), C30(H30G,H30H,H30I),
 C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C26B(H26D,
 H26E,H26F), C27B(H27D,H27E,H27F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F),
 C23C(H23A,H23B,H23C), C24C(H24A,H24B,H24C), C25C(H25A,H25B,H25C), C26C(H26A,
 H26B,H26C), C27C(H27A,H27B,H27C), C29C(H29A,H29B,H29C), C30C(H30A,H30B,H30C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O3B(H3B), O2C(H2C)
;