Thermally-Induced Phase Transition of Pseudorotaxane Crystals: Changes in Conformation and Interaction of the Molecules and Optical Properties of the Crystals
Masaki Horie; Yuji Suzaki; Daisuke Hashizume; Tomoko Abe; Tiendi Wu; Takafumi Sassa; Takuya Hosokai; Kohtaro Osakada; Journal of the American Chemical Society 134 (2012) 17932–17944; doi:10.1021/ja304406c

data_4118833
_publ_section_title
;
 Thermally-Induced Phase Transition of Pseudorotaxane Crystals: Changes in
 Conformation and Interaction of the Molecules and Optical Properties of
 the Crystals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17932
_journal_page_last               17944
_journal_paper_doi               10.1021/ja304406c
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C19 H22 Fe N, C24 H32 O8, P F6'
_chemical_formula_sum            'C43 H54 F6 Fe N O8 P'
_chemical_formula_weight         913.69
_chemical_name_systematic
; 
 ? 
;
_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                87.288(10)
_cell_angle_beta                 81.024(7)
_cell_angle_gamma                88.600(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3858(17)
_cell_length_b                   11.276(2)
_cell_length_c                   19.379(3)
_cell_measurement_reflns_used    5203
_cell_measurement_temperature    373.2(1)
_cell_measurement_theta_max      28.4543
_cell_measurement_theta_min      1.8083
_cell_volume                     2238.8(6)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 The refined structure at 30 deg. was used as an initial model.
;
_diffrn_ambient_temperature      373.2(1)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
scan:
        Number of images: 120
                   Slice: -20.0000 - 40.0000
             Image width: 0.5000
                Exp time: 2.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 0.0000
                     Phi: 0.0000
                     XTD: 40.0060
                  2theta: 10.0423
scan:
        Number of images: 180
                   Slice: -80.0000 - 10.0000
             Image width: 0.5000
                Exp time: 2.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 40.0000
                     Phi: 270.0000
                     XTD: 40.0060

                  2theta: 10.0423
scan:
        Number of images: 328
                   Slice: -80.0000 - 84.0000
             Image width: 0.5000
                Exp time: 2.0000
           Rotation axis: Omega
                   Omega: 0.0000
                     Chi: 50.0000
                     Phi: 90.0000
                     XTD: 40.0060
                  2theta: 10.0423

;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0198
_diffrn_orient_matrix_UB_12      -0.0311
_diffrn_orient_matrix_UB_13      -0.0903
_diffrn_orient_matrix_UB_21      -0.0858
_diffrn_orient_matrix_UB_22      0.0102
_diffrn_orient_matrix_UB_23      -0.0207
_diffrn_orient_matrix_UB_31      0.0100
_diffrn_orient_matrix_UB_32      0.0509
_diffrn_orient_matrix_UB_33      -0.0066
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16953
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1073P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                4087
_reflns_number_total             7822
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja304406c_si_003.cif
_cod_data_source_block           100deg
_cod_original_cell_volume        2238.8(7)
_cod_database_code               4118833