The crystal structure of (3S,12R,20R,24S)-3,12-diacetyl-20,24-epoxy-dammarane-3,12,25-triol acetone solvate, C34H56O6
Hongzhang, Liu; Yingting, Wang; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 437–439; doi:10.1515/ncrs-2017-0331

data_8106175
_publ_section_title
;
 The crystal structure of
 (3S,12R,20R,24S)-3,12-diacetyl-20,24-epoxy-dammarane-3,12,25-triol
 acetone solvate, C34H56O6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              437
_journal_page_last               439
_journal_paper_doi               10.1515/ncrs-2017-0331
_journal_volume                  233
_journal_year                    2018
_chemical_absolute_configuration .
_chemical_formula_moiety         'C34 H56 O6'
_chemical_formula_sum            'C34 H56 O6'
_chemical_formula_weight         560.78
_chemical_name_systematic
;
(3<i>S</i>,12<i>R</i>,20<i>R</i>,24<i>S</i>)-3,12-diacetyl-20,24-epoxy-
dammarane-3,12,25-triol
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0343(8)
_cell_length_b                   17.7992(16)
_cell_length_c                   24.153(3)
_cell_measurement_reflns_used    1134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      43.2010
_cell_measurement_theta_min      4.4110
_cell_volume                     3454.0(6)
_computing_cell_refinement       'Bruker FRAMBO [1]'
_computing_data_collection       'Bruker FRAMBO [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'Diamond 3.2i [4]'
_computing_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'SHELXL-2014/7 [3]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990) [2]'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0990
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7716
_diffrn_reflns_point_group_measured_fraction_full 0.840
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        66.039
_diffrn_reflns_theta_max         66.039
_diffrn_reflns_theta_min         3.084
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.8802
_exptl_absorpt_correction_T_min  0.8042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 380 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(5)
_refine_ls_extinction_coef       0.00022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0433P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.481
_reflns_Friedel_fraction_full    0.632
_reflns_Friedel_fraction_max     0.632
_reflns_number_gt                2090
_reflns_number_total             5067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0331_suppl.cif
_cod_data_source_block           b
_cod_original_cell_volume        3453.9(6)
_cod_database_code               8106175
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.804
_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), C24(H24)
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)
2.c Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C)
2.d Tetrahedral OH refined with riding coordinates:
 O4(H4)
2.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              91788
_shelx_hkl_checksum              72526
_shelx_fab_checksum              93514
_olex2_submission_special_instructions 'No special instructions were received'