Temperature-dependent crystal structure of the isopropanol clathrate of Dianin's compound
Jackson J. Lee; Rebecca O. Fuller; Alexandre N. Sobolev; Henrik F. Clausen; Jacob Overgaard; George A. Koutsantonis; Bo B. Iversen; Mark A. Spackman; Chem.Commun. 47 (2011) 2029–; doi:10.1039/c0cc04418k

data_7105974
_publ_section_title
;
 Temperature-dependent crystal structure of the isopropanol clathrate of
 Dianin's compound
;
_journal_name_full               Chem.Commun.
_journal_page_first              2029
_journal_paper_doi               10.1039/c0cc04418k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         '3(C18 H20 O2), C3 H8 O'
_chemical_formula_sum            'C57 H68 O7'
_chemical_formula_weight         865.11
_chemical_name_systematic
;
4-p-Hydroxyphenyl-2,2,4-trimethylchroman isopropanol clathrate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            24
_cell_length_a                   53.7098(13)
_cell_length_b                   53.7098
_cell_length_c                   10.9911(3)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      18.54
_cell_measurement_theta_min      2.26
_cell_volume                     27458.6(10)
_computing_cell_refinement       'Bruker SAINT V7.68A'
_computing_data_collection       'Bruker Diffractometer control software'
_computing_data_reduction        'Bruker SAINT V7.68A'
_computing_molecular_graphics    'Mercury CSD v. 2.3 (2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      15(2)
_diffrn_detector_area_resol_mean 15.0
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Bruker SMART 6000, APEX II'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'diamond double-crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       121
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -122
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            835170
_diffrn_reflns_theta_full        28.57
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.052
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             11184
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.910
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         70274
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+52.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1811
_reflns_number_gt                53909
_reflns_number_total             70274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04418K.TXT
_cod_data_source_block           cmpnd05
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7105974