β-Dihydroentandrophragmin–Ethyl Acetate (1/0.355)
Baxter, Robert L.; Dijksma, Fokke J. J.; Gould, Robert O.; Parsons, Simon; Acta Crystallographica Section C 54 (1998) 1182–1184; doi:10.1107/S0108270198006076

data_2007501
_publ_section_title
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 \b-Dihydroentandrophragmin--Ethyl Acetate (1/0.355)
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_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1182
_journal_page_last               1184
_journal_paper_doi               10.1107/S0108270198006076
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C43 H58 O17, 0.355C4 H8 O2'
_chemical_formula_sum            'C44.42 H60.84 O17.71'
_chemical_formula_weight         878.17
_chemical_name_common            \b-dihydroentandrophragmin
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.0341(8)
_cell_length_b                   11.0341(8)
_cell_length_c                   62.874(9)
_cell_measurement_reflns_used    59
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     6629.4(12)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELX97
_computing_structure_solution    'SHELX97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device
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Stoe Stadi-4 four-circle diffractometer equipped with an Oxford Cryosystems
low-temperature device (Cosier & Glazer, 1986)
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_diffrn_measurement_method
'\w scans with learnt-profile method (Clegg, 1981)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            5589
_diffrn_reflns_theta_full        60.09
_diffrn_reflns_theta_max         60.09
_diffrn_reflns_theta_min         4.22
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   'integration (see below)'
_exptl_absorpt_process_details
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 The approximate crystal shape was refined using X-SHAPE, (Sto\"e and
 Cie., 1997) and symmetry related data to give a shape bounded by eight
 crystal faces.  This crystal shape was then used to calculate
 absorption corrections using SHELXTL (Sheldrick, 1997).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             2815
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.50
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.9(5)
_refine_ls_extinction_coef       0.00076(12)
_refine_ls_extinction_method     SHELX97
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     828
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.093
_refine_ls_R_factor_gt           0.075
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1102P)^2^+12.5558P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.210
_reflns_number_gt                3746
_reflns_number_total             4548
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1227.cif
_cod_data_source_block           entand
_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 
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_cod_original_sg_symbol_H-M      'P 31 21'
_cod_database_code               2007501