Synthesis and crystal structure of [26,27-2H6] 24-epi-cathasterone
Adelheid Kolbe; Petra Fuchs; Andrea Porzel; Ute Baumeister; Alfred Kolbe; Günter Adam; J. Chem. Soc., Perkin Trans. 1  (2002) 2022–2027; doi:10.1039/b203323b

data_7204429
_publ_section_title
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 Synthesis and crystal structure of [26,27-2H6] 24-epi-cathasterone
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_journal_issue                   17
_journal_name_full               'J. Chem. Soc., Perkin Trans. 1'
_journal_page_first              2022
_journal_page_last               2027
_journal_paper_doi               10.1039/b203323b
_journal_year                    2002
_chemical_formula_moiety         'C28 H42 D6 O3, H2 O'
_chemical_formula_sum            'C28 H44 D6 O4'
_chemical_formula_weight         456.72
_chemical_name_common            '[26,27 ^2^H~6~] 24-epicathasteron'
_chemical_name_systematic
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[26,27-^2^H~6~] (22S,24S)-3\b,22-dihydroxy-5\a-ergostan-6-one 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.376(11)
_cell_angle_beta                 77.377(19)
_cell_angle_gamma                79.801(12)
_cell_formula_units_Z            2
_cell_length_a                   7.4742(10)
_cell_length_b                   14.290(3)
_cell_length_c                   14.776(3)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.05
_cell_measurement_theta_min      5.0
_cell_volume                     1359.2(5)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'Siemens XP/PC'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; 
Scan width (omega) = 1.02 - 1.17, scan ratio 2theta:omega = 1.00 
I(Net) and sigma(I) calculated according to Blessing (1987) 
;
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1791
_diffrn_reflns_av_sigmaI/netI    0.2657
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10882
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        8.2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -5(3)
_refine_ls_extinction_coef       0.0138(11)
_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   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         5359
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.2502
_refine_ls_R_factor_gt           0.0723
_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^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1521
_reflns_limit_h_max              9
_reflns_limit_h_min              -8
_reflns_limit_k_max              17
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1912
_reflns_number_total             5359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203323b.txt
_cod_data_source_block           k383
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1359.2(4)
_cod_database_code               7204429