The crystal structure of (6aR,6bS,8aS,8bR,9S,11aS,12aS,12bS)-10-(4-acetoxy-3-methylbutyl)-6a,8a,9-trimethyl-3,4,5,6,6a,6b,7,8,8a,8b,9,10,11a,12,12a,12b-hexadecahydro-1H-naphtho[2′,1′:4,5]indeno[2,1-b]furan-4-yl acetate, C31H48O5
Mou, Xiao-Dong; Wang, Hui-Yun; Sun, Ke-Wei; Luan, Ming-Zhu; Meng, Qing-Guo; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1223–1225; doi:10.1515/ncrs-2020-0275

data_8105427
_publ_section_title
;
 The crystal structure of
 (6aR,6bS,8aS,8bR,9S,11aS,12aS,12bS)-10-(4-acetoxy-3-methylbutyl)-6a,8a,9-trimethyl-3,4,5,6,6a,6b,7,8,8a,8b,9,10,11a,12,12a,12b-hexadecahydro-1H-naphtho[2&#x2032;,1&#x2032;:4,5]indeno[2,1-b]furan-4-yl
 acetate, C31H48O5
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1223
_journal_page_last               1225
_journal_paper_doi               10.1515/ncrs-2020-0275
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C31 H48 O5'
_chemical_formula_sum            'C31 H48 O5'
_chemical_formula_weight         500.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 97.922(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0421(3)
_cell_length_b                   6.49710(16)
_cell_length_c                   20.4687(4)
_cell_measurement_reflns_used    9137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.7880
_cell_measurement_theta_min      4.0100
_cell_volume                     1454.44(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -98.00 -18.00   1.00    1.00    --  -42.20 125.00-120.00   80
  2  \w     18.00 116.00   1.00    1.00    --   42.20  38.00   0.00   98
  3  \w     18.00 116.00   1.00    1.00    --   42.20  38.00 -90.00   98
  4  \w     -3.00  92.00   1.00    1.00    --   42.20-125.00-180.00   95
  5  \w     10.00 118.00   1.00    1.00    --   42.20  77.00   0.00  108
  6  \w     60.00 169.00   1.00    1.25    --   92.50  77.00 -90.00  109
  7  \w     63.00 165.00   1.00    1.25    --   92.50  61.00  30.00  102
  8  \w     63.00 165.00   1.00    1.25    --   92.50  61.00 -30.00  102
  9  \w     63.00 165.00   1.00    1.25    --   92.50  61.00   0.00  102
 10  \w     60.00 169.00   1.00    1.25    --   92.50  77.00 -30.00  109
 11  \w     63.00 165.00   1.00    1.25    --   92.50  61.00 -60.00  102
 12  \w     10.00  85.00   1.00    1.25    --   92.50 -95.00 -30.00   75
 13  \w     60.00 169.00   1.00    1.25    --   92.50  77.00   0.00  109
 14  \w     19.00 118.00   1.00    1.25    --   92.50 -45.00   0.00   99
 15  \w     20.00 122.00   1.00    1.25    --   92.50 -61.00  30.00  102
 16  \w     60.00 169.00   1.00    1.25    --   92.50  77.00-120.00  109
 17  \w     83.00 121.00   1.00    1.25    --   92.50 -61.00-180.00   38
 18  \w     64.00  89.00   1.00    1.25    --   92.50-125.00-150.00   25
 19  \w     60.00 110.00   1.00    1.25    --   92.50  77.00 -60.00   50
 20  \w     14.00  40.00   1.00    1.25    --   92.50 -91.00-168.16   26
 21  \w     69.00  96.00   1.00    1.25    --   92.50 -91.00-168.16   27
 22  \w     23.00  92.00   1.00    1.25    --   92.50-125.00 120.00   69
 23  \w     65.00 123.00   1.00    1.25    --   92.50  61.00 -90.00   58
 24  \w     65.00 118.00   1.00    1.25    --   92.50  30.00 150.00   53
 25  \w    129.00 164.00   1.00    1.25    --   92.50  30.00 150.00   35
 26  \w     43.00  75.00   1.00    1.25    --   92.50 -95.00-120.00   32
 27  \w     60.00 101.00   1.00    1.25    --   92.50  77.00  30.00   41
 28  \w    107.00 132.00   1.00    1.25    --   92.50  77.00  30.00   25
 29  \w     20.00  58.00   1.00    1.25    --   92.50 -45.00 120.00   38
 30  \w     25.00  55.00   1.00    1.25    --   92.50 -95.00 120.00   30
 31  \w     19.00  53.00   1.00    1.25    --   92.50-125.00  90.00   34
 32  \w     19.00  67.00   1.00    1.25    --   92.50-125.00 -60.00   48
 33  \w     63.00  88.00   1.00    1.25    --   92.50  61.00  60.00   25
 34  \w     20.00  65.00   1.00    1.25    --   92.50 -61.00-180.00   45
 35  \w     20.00  61.00   1.00    1.25    --   92.50 -87.00 -25.30   41
 36  \w     19.00  46.00   1.00    1.25    --   92.50-125.00-120.00   27
 37  \w     79.00 112.00   1.00    1.25    --   92.50 125.00-120.00   33
 38  \w    103.00 128.00   1.00    1.25    --   92.50 -85.00 -16.49   25
 39  \w    116.00 142.00   1.00    1.25    --   92.50  45.00  30.00   26
 40  \w    129.00 172.00   1.00    1.25    --   92.50  15.00-150.00   43
 41  \w     17.00  96.00   1.00    1.25    --   92.50 -85.00 -16.49   79
;
_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      0.0371872000
_diffrn_orient_matrix_UB_12      -0.0729773000
_diffrn_orient_matrix_UB_13      0.0715617000
_diffrn_orient_matrix_UB_21      -0.1287756000
_diffrn_orient_matrix_UB_22      0.0528307000
_diffrn_orient_matrix_UB_23      0.0159166000
_diffrn_orient_matrix_UB_31      -0.0433728000
_diffrn_orient_matrix_UB_32      -0.2193196000
_diffrn_orient_matrix_UB_33      -0.0199857000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25745
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.889
_diffrn_reflns_theta_max         66.889
_diffrn_reflns_theta_min         4.042
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69199
_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    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.154
_refine_diff_density_min         -0.116
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details
;
 Flack x determined using 1709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(10)
_refine_ls_extinction_coef       0.0091(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0533P)^2^+0.1416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                4423
_reflns_number_total             5109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0275_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1454.45(6)
_cod_database_code               8105427
_chemical_oxdiff_formula         'C1 H1 O1'
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.860
_reflns_odcompleteness_completeness 99.20
_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
2.a Ternary CH refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C14(H14), C16(H16), C17(H17), C20(H20), C22(H22),
 C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,
 H12B), C15(H15A,H15B), C23(H23B,H23A), C24(H24A,H24B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C27(H27A,H27B,
 H27C), C29(H29A,H29C,H29B), C31(H31A,H31B,H31C)
;
_olex2_date_sample_data_collection 2019-12-11
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.704