Selective solvent inclusion as a tool for mapping molecular properties in crystal structures: a diethylstilbestrol example
Görbitz, Carl Henrik; Hersleth, Hans-Petter; Acta Crystallographica Section B 56 (2000) 1094–1102; doi:10.1107/S0108768100012805

data_2102210
_publ_section_title
;
 Selective solvent inclusion as a tool for mapping molecular properties
 in crystal structures: a diethylstilbestrol example
;
_journal_coeditor_code           OS0062
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1094
_journal_page_last               1102
_journal_paper_doi               10.1107/S0108768100012805
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         'C18 H20 O2,4(C4 H10 O)'
_chemical_formula_sum            'C34 H60 O6'
_chemical_formula_weight         564.84
_chemical_name_systematic
; 
 diethylstilbestrol tert-butanol solvate (1/4)
;
_space_group_IT_number           2
_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                85.140(2)
_cell_angle_beta                 85.031(2)
_cell_angle_gamma                82.626(2)
_cell_formula_units_Z            1
_cell_length_a                   6.2717(6)
_cell_length_b                   7.4330(8)
_cell_length_c                   20.364(2)
_cell_measurement_reflns_used    3903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.8
_cell_volume                     935.32(16)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method
'Sets of exposures each taken over 0.3\% \w rotation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7061
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       0.032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         3281
_refine_ls_number_restraints     1428
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.2702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                2514
_reflns_number_total             3281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            os0062.cif
_cod_data_source_block           dtbut
_cod_depositor_comments
;1. In the initial file, disorder assemblies were all given given
different
 names, and thus, according to my understanding
 of
_arom_site_disorder_{assembly,group} definition of
 IUCr
(http://www.iucr.org/__data/iucr/cifdic_html/1/cif_core.dic/Iatom_site_disorder_assembly.html,
http://www.iucr.org/__data/iucr/cifdic_html/1/cif_core.dic/Iatom_site_disorder_group.html)
could
 all be accupied simultaniously in any combinations, resulting in
multiple
 atomic clahes.

I have renamed disorder assemblies so that assemblies having
 different
groups specified have the same name. Such renaming gives
 reasonable
molecules when simultaniously occupied disorder groups are picked
 for
all assemblies.

2. The structure has one long C-C bond (C73A C73A
 1.81(3), reported in
the _geom_bond_distance list.

Saulius
 Gra\<zulis
2010.02.17
;
_cod_original_cell_volume        935.34(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2102210