Structural characterisation of two pharmaceutically important steroids by solid-state NMR
Othman, Abdullah; Harris, Robin K.; Hodgkinson, Paul; Christopher, Elizabeth A.; Lancaster, Robert W.; New Journal of Chemistry 32 (2008) 1796–; doi:10.1039/b803586e

data_7051973
_publ_section_title
;
 Structural characterisation of two pharmaceutically important steroids
 by solid-state NMR
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1796
_journal_paper_doi               10.1039/b803586e
_journal_volume                  32
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H37 Cl O7, C4 H8 O2'
_chemical_formula_sum            'C32 H45 Cl O9'
_chemical_formula_weight         609.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   difmap
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.39630(10)
_cell_length_b                   13.39630(10)
_cell_length_c                   31.0233(5)
_cell_measurement_reflns_used    26389
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      1.75
_cell_volume                     4821.57(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'R-AXIS SPIDER'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            89272
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_correction_T_min  0.9607
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
NUMABS (Rigaku Inc., 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8549
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                7919
_reflns_number_total             8549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803586e.txt
_cod_data_source_block           s199
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     'P 31 2" '
_cod_original_sg_symbol_H-M      'P 31 2 1 '
_cod_database_code               7051973