<i>Ab initio</i> X-ray structural characterization of an inclusion compound with a compositionally disordered chiral guest: no prior knowledge of the crystal composition
Guzei, Ilia A.; Miles, Kelsey C.; Acta Crystallographica Section C 72 (2016) 179–183; doi:10.1107/S2053229616001972

data_2020414
_publ_section_title
;
 <i>Ab initio</i> X-ray structural characterization of an inclusion
 compound with a compositionally disordered chiral guest: no prior
 knowledge of the crystal composition
;
_journal_coeditor_code           FN3214
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              179
_journal_page_last               183
_journal_paper_doi               10.1107/S2053229616001972
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'C31 H30 O4, 0.85(C10 H14 O1), 0.15(C10 H14 O3)'
_chemical_formula_moiety         'C31 H30 O4, 0.85C10 H14 O1, 0.15C10 H14 O3'
_chemical_formula_sum            'C41 H44 O5.3'
_chemical_formula_weight         621.56
_chemical_name_systematic
;(4<i>R</i>,5<i>R</i>)-4,5-Bis(hydroxydiphenylmethyl)-2,2-dimethyl-1,3-dioxolane--4,4a,5,6,7,8-hexahydronaphthalen-2(3<i>H</i>)-one--4a-(hydroperoxymethyl)-4,4a,5,6,7,8-hexahydronaphthalen-2(3<i>H</i>)-one
(1/0.85/0.15)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5183(5)
_cell_length_b                   9.5950(7)
_cell_length_c                   36.207(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.907
_cell_measurement_theta_min      3.663
_cell_volume                     3306.7(5)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXTL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      99.95
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII area-detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            50756
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.351
_diffrn_reflns_theta_min         2.441
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.7537
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1330
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.253
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2716 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6592
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.9649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6442
_reflns_number_total             6592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3214sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020414.cif.'
_cod_original_formula_sum        'C41 H44 O5.30'
_cod_database_code               2020414
_cod_database_fobs_code          2020414
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.882
_shelx_hkl_checksum              19453
_shelx_res_checksum              15194