Crystal structure of (3R,5R,8R,9R,10R,12R,13R,14R)-4,4,8,10,14-pentamethyl-17-((R)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl)hexadecahydro-1H-cyclopenta[a]phenanthrene-3,12-diol, C30H52O3
Zhao, Ruo-Lin; Wang, Hui-Yun; Luan, Ming-Zhu; Zheng, Xia; Zhao, Feng-Lan; Meng, Qing-Guo; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 129–131; doi:10.1515/ncrs-2019-0533

data_8105037
_publ_section_title
;
 Crystal structure of
 (3R,5R,8R,9R,10R,12R,13R,14R)-4,4,8,10,14-pentamethyl-17-((R)-2,6,6-trimethyltetrahydro-2H-pyran-2-yl)hexadecahydro-1H-cyclopenta[a]phenanthrene-3,12-diol,
 C30H52O3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              129
_journal_page_last               131
_journal_paper_doi               10.1515/ncrs-2019-0533
_journal_volume                  235
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H52 O3'
_chemical_formula_sum            'C30 H52 O3'
_chemical_formula_weight         460.71
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.71147(14)
_cell_length_b                   16.6565(4)
_cell_length_c                   25.0815(6)
_cell_measurement_reflns_used    8405
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.2050
_cell_measurement_theta_min      3.5240
_cell_volume                     2803.85(11)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.971
_diffrn_measured_fraction_theta_max 0.999
_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     35.00 130.00   1.00    1.00    --   41.55 178.00-180.00   95
  2  \w     17.00 116.00   1.00    1.00    --   41.55  38.00 120.00   99
  3  \w     19.00 118.00   1.00    2.35    --   92.50 -45.00 120.00   99
  4  \w     10.00  85.00   1.00    2.35    --   92.50 -95.00   0.00   75
  5  \w     60.00 169.00   1.00    2.35    --   92.50  77.00  60.00  109
  6  \w     19.00  93.00   1.00    2.35    --   92.50-125.00 -90.00   74
  7  \w     19.00  93.00   1.00    2.35    --   92.50-125.00-150.00   74
  8  \w      4.00 128.00   1.00    2.35    --   92.50   0.00  60.00  124
  9  \w     17.00  80.00   1.00    2.35    --   92.50 -95.00  90.00   63
 10  \w    124.00 164.00   1.00    2.35    --   92.50  77.00-120.00   40
 11  \w     37.00  93.00   1.00    2.35    --   92.50-125.00-180.00   56
 12  \w     68.00  93.00   1.00    2.35    --   92.50-125.00  90.00   25
 13  \w     78.00 105.00   1.00    2.35    --   92.50 -61.00  90.00   27
 14  \w     61.00  86.00   1.00    2.35    --   92.50  77.00-120.00   25
 15  \w     38.00  71.00   1.00    2.35    --   92.50-125.00 -60.00   33
 16  \w    133.00 169.00   1.00    2.35    --   92.50  30.00   0.00   36
;
_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      0.0872748000
_diffrn_orient_matrix_UB_12      -0.0592029000
_diffrn_orient_matrix_UB_13      -0.0410030000
_diffrn_orient_matrix_UB_21      0.0110362000
_diffrn_orient_matrix_UB_22      -0.0654143000
_diffrn_orient_matrix_UB_23      0.0433156000
_diffrn_orient_matrix_UB_31      -0.2120485000
_diffrn_orient_matrix_UB_32      -0.0277486000
_diffrn_orient_matrix_UB_33      -0.0146407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19751
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.517
_diffrn_reflns_theta_min         3.524
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71642
_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    1.091
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1718 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(10)
_refine_ls_extinction_coef       0.0230(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0589P)^2^+0.2613P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                4341
_reflns_number_total             4891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0533_suppl.cif
_cod_data_source_block           pd1
_cod_database_code               8105037
_chemical_oxdiff_formula         'C1 H1 O1'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.877
_reflns_odcompleteness_completeness 98.45
_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:
 C3(H3), C5(H5), C9(H9), C12(H12), C13(H13), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C15(H15A,
 H15B), C16(H16A,H16B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;