Betulin 3,28-di-<i>O</i>-tosylate
Peipiņš, Uldis; Freimanis, Niks; Stepanovs, Dmitrijs; Mishnev, Anatoly; Turks, Māris; Acta Crystallographica Section E 70 (2014) o879–o880; doi:10.1107/S1600536814016602

data_2239806
_publ_section_title
;
 Betulin 3,28-di-<i>O</i>-tosylate
;
_journal_coeditor_code           FY2116
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o879
_journal_page_last               o880
_journal_paper_doi               10.1107/S1600536814016602
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C44 H62 O6 S2'
_chemical_formula_moiety         'C44 H62 O6 S2'
_chemical_formula_sum            'C44 H62 O6 S2'
_chemical_formula_weight         751.08
_chemical_melting_point          403
_chemical_name_common            'Betulin 3,28-di-O-tosylate'
_chemical_name_systematic
'(1<i>R</i>,3a<i>S</i>,5a<i>R</i>,5b<i>R</i>,7a<i>R</i>,9<i>S</i>,11a<i>R</i>,11b<i>R</i>,13a<i>R</i>,13b<i>R</i>)-5a,5b,8,8,11a-Pentamethyl-1-(prop-1-en-2-yl)-3a-[(tosyloxy)methyl]icosahydro-1<i>H</i>-cyclopenta[<i>a</i>]chrysen-9-yl 4-methylbenzenesulfonate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.98240(10)
_cell_length_b                   18.2035(4)
_cell_length_c                   31.4449(9)
_cell_measurement_reflns_used    35297
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.998
_cell_volume                     3996.78(16)
_computing_cell_refinement       'SCALEPACK (Otwinovski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction
'DENZO (Otwinovski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla <i>et al.</i>, 2012)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_sigmaI/netI    0.1882
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            9235
_diffrn_reflns_theta_full        27.77
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.327
_refine_ls_abs_structure_details 'Flack (1983), 3968 Friedel pairs'
_refine_ls_abs_structure_Flack   0.07(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1815
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+1.1649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                4887
_reflns_number_total             9235
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fy2116sup1.cif
_cod_data_source_block           I
_cod_database_code               2239806
_cod_database_fobs_code          2239806