Temperature-Dependent Phase Transitions in Two Crystalline Host–Guest Complexes Derived from Mandelic Acid
Hager, O.; Foces-Foces, C.; Llamas-Saiz, A. L.; Weber, E.; Acta Crystallographica Section B 54 (1998) 82–93; doi:10.1107/S0108768197010471

data_2105546
_publ_section_title
;
 Temperature-Dependent Phase Transitions in Two Crystalline Host--Guest
 Complexes Derived from Mandelic Acid
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              82
_journal_page_last               93
_journal_paper_doi               10.1107/S0108768197010471
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C29 H36 O2 . C3 H7 N O'
_chemical_formula_sum            'C32 H43 N O3'
_chemical_formula_weight         489.70
_chemical_name_systematic
;(R)-1,1-bis(4-tert-butylphenyl)-2-(4-methylphenyl)ethan-1,2-diol
 dimethylformamide 1:1 complex
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 101.954(12)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   24.446(4)
_cell_length_b                   5.9519(6)
_cell_length_c                   20.461(4)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    170
_cell_measurement_theta_max      45
_cell_measurement_theta_min      2
_cell_volume                     2912.5(8)
_computing_cell_refinement       'LSUCRE (Appleman, 1984)'
_computing_data_collection       'Philips PW1100'
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF
_computing_molecular_graphics    xtal_ORTEP
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Philips PW1100'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .042
_diffrn_reflns_av_sigmaI/netI    .019
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5596
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         65.24
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.5480
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.41
_refine_diff_density_max         .320
_refine_diff_density_min         -.275
_refine_ls_abs_structure_details
;     The absolute configuration was assigned to agree
      with the known chirality at C2 obtained from a
      previous determitation (Weber et al., 1997b)
;
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       2588.270
_refine_ls_extinction_method     'Zachariasen (1968)'
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_obs   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     941
_refine_ls_number_reflns         4500
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .067
_refine_ls_R_factor_obs          .054
_refine_ls_shift/esd_max         .098
_refine_ls_shift/esd_mean        .033
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
; Weighting scheme: empirical to
  give no trends in <wF^2^> vs
  <|F~obs~|> and <sin\q/\l>
;
_refine_ls_wR_factor_all         .071
_refine_ls_wR_factor_obs         .063
_reflns_number_observed          4500
_reflns_number_total             5457
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm0010.cif
_cod_data_source_block           2a
_cod_original_sg_symbol_Hall     P_2y1
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C32 H43 N1 O3 '
_cod_database_code               2105546