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_2105547
_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           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                88.736(10)
_cell_angle_beta                 101.43(2)
_cell_angle_gamma                93.135(10)
_cell_formula_units_Z            2
_cell_length_a                   14.417(3)
_cell_length_b                   6.0303(4)
_cell_length_c                   17.564(6)
_cell_measurement_reflns_used    69
_cell_measurement_temperature    270
_cell_measurement_theta_max      45
_cell_measurement_theta_min      2
_cell_volume                     1494.4(6)
_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_sigmaI/netI    .019
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4980
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         64.36
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.5340
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .532
_refine_diff_density_min         -.252
_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       5256.552
_refine_ls_extinction_method     'Zachariasen (1968)'
_refine_ls_goodness_of_fit_all   .95
_refine_ls_goodness_of_fit_obs   .952
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     664
_refine_ls_number_reflns         3474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .093
_refine_ls_R_factor_obs          .071
_refine_ls_shift/esd_max         0.060
_refine_ls_shift/esd_mean        .09
_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         .102
_refine_ls_wR_factor_obs         .083
_reflns_number_observed          3474
_reflns_number_total             4980
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm0010.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_Hall     P_1
_cod_original_formula_sum        'C32 H43 N1 O3 '
_cod_database_code               2105547