Ring rotation of ferrocene in interlocked molecules in single crystals
Wang, Chi-Hsien; Chen, Kai-Jen; Wu, Tsung-Huan; Chang, Hung-Kai; Tsuchido, Yoshitaka; Sei, Yoshihisa; Chen, Pei-Lin; Horie, Masaki; Chemical Science 12 (2021) 3871–3875; doi:10.1039/D0SC06876D

data_1560164
_publ_section_title
;
 Ring rotation of ferrocene in interlocked molecules in single crystals
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3871
_journal_page_last               3875
_journal_paper_doi               10.1039/D0SC06876D
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C12 H16 Fe N, F6 P, C H2 Cl2, C20 H24 O6'
_chemical_formula_sum            'C33 H42 Cl2 F6 Fe N O6 P'
_chemical_formula_weight         820.42
_chemical_name_systematic
'[ferrocenylmethyl(methy) ammonium hexafluorophosphate][dibenzo[18]crown-6 ether]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2020-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-24 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                94.740(2)
_cell_angle_beta                 95.623(2)
_cell_angle_gamma                104.722(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8440(3)
_cell_length_b                   11.6767(3)
_cell_length_c                   16.7383(5)
_cell_measurement_reflns_used    7182
_cell_measurement_temperature    333(2)
_cell_measurement_theta_max      70.2770
_cell_measurement_theta_min      2.6700
_cell_volume                     1840.28(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      333(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9755
_diffrn_measured_fraction_theta_max 0.9755
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00 -40.00   0.50    0.05    --    0.00 122.00  22.00   50
  2  \w    -85.00 -60.00   0.50    0.08    --  -55.36 122.00  22.00   50
  3  \w    -88.00 -63.00   0.50    0.08    -- -102.00 122.00  22.00   50
  4  \w    -55.00 -21.00   0.50    0.08    -- -102.00  50.00 -30.00   68
  5  \w    -17.00  12.00   0.50    0.08    --  -55.36  15.00   0.00   58
  6  \w      2.00  27.00   0.50    0.08    --  -55.36  30.00   0.00   50
  7  \w     25.00  70.00   0.50    0.05    --    0.00  19.00 -60.00   90
  8  \w     41.00  70.00   0.50    0.05    --    0.00  19.00-150.00   58
  9  \w     -4.00  32.00   0.50    0.05    --    0.00  19.00-150.00   72
 10  \w    -21.00  15.00   0.50    0.05    --    0.00  19.00 -60.00   72
 11  \w    -33.00  -7.00   0.50    0.08    --  -55.36  30.00   0.00   52
 12  \w    -33.00  25.00   0.50    0.08    --  -55.36  30.00 -60.00  116
 13  \w     -2.00  27.00   0.50    0.08    --  -55.36  15.00-120.00   58
 14  \w    -19.00  12.00   0.50    0.08    --  -55.36  15.00 -90.00   62
 15  \w    -33.00  25.00   0.50    0.08    --  -55.36  30.00  30.00  116
 16  \w    -16.00  10.00   0.50    0.08    --  -55.36  15.00 150.00   52
 17  \w     19.00  44.00   0.50    0.05    --    0.00-122.00 -59.00   50
 18  \w     54.00  97.00   0.50    0.08    --   55.36-122.00 -59.00   86
 19  \w     66.00  91.00   0.50    0.08    --  110.71-122.00 -59.00   50
 20  \w     51.00 106.00   0.50    0.08    --  110.71-111.00   0.00  110
 21  \w     56.00  81.00   0.50    0.08    --   55.36-150.00 138.00   50
 22  \w     33.00  58.00   0.50    0.05    --    0.00-150.00 138.00   50
 23  \w     77.00 129.00   0.50    0.08    --  110.71-150.00 138.00  104
 24  \w     26.00  55.00   0.50    0.08    --  110.71 -50.00  60.00   58
 25  \w     26.00  51.00   0.50    0.08    --  110.71 -50.00  90.00   50
 26  \w     28.00  53.00   0.50    0.08    --  110.71-111.00  30.00   50
 27  \w     33.00  58.00   0.50    0.08    --  110.71 -50.00 -30.00   50
 28  \w     30.00  59.00   0.50    0.08    --  110.71 -50.00   0.00   58
 29  \w     31.00 107.00   0.50    0.08    --  110.71-111.00 -60.00  152
 30  \w     26.00  57.00   0.50    0.08    --  110.71 -50.00-180.00   62
 31  \w     26.00  58.00   0.50    0.08    --  110.71 -50.00-150.00   64
 32  \w     21.00 107.00   0.50    0.08    --  110.71-111.00-150.00  172
 33  \w     26.00  59.00   0.50    0.08    --  110.71 -50.00 -90.00   66
 34  \w     89.00 160.00   0.50    0.08    --  110.71 111.00-120.00  142
 35  \w    111.00 143.00   0.50    0.08    --  110.71 178.00-150.00   64
 36  \w     90.00 138.00   0.50    0.08    --  110.71 178.00 -90.00   96
 37  \w     83.00 137.00   0.50    0.08    --   55.36 122.00  22.00  108
 38  \w     81.00 111.00   0.50    0.08    --  110.71 122.00  22.00   60
 39  \w     98.00 132.00   0.50    0.08    --  110.71 111.00  60.00   68
 40  \w    145.00 171.00   0.50    0.08    --  110.71 111.00   0.00   52
 41  \w    113.00 138.00   0.50    0.08    --  110.71 178.00 120.00   50
 42  \w     87.00 175.00   0.50    0.08    --  110.71 111.00  90.00  176
 43  \w     93.00 124.00   0.50    0.08    --  110.71 111.00   0.00   62
 44  \w     79.00 111.00   0.50    0.08    --   55.36 125.00 -90.00   64
 45  \w     82.00 138.00   0.50    0.08    --   55.36 125.00 -60.00  112
 46  \w     63.00 137.00   0.50    0.08    --   55.36 150.00-175.00  148
 47  \w     61.00 125.00   0.50    0.08    --  110.71 150.00-175.00  128
 48  \w     49.00  83.00   0.50    0.08    --  110.71 178.00 -90.00   68
 49  \w     48.00  74.00   0.50    0.08    --  110.71 178.00-150.00   52
 50  \w     48.00 145.00   0.50    0.08    --  110.71 178.00-120.00  194
 51  \w     48.00  97.00   0.50    0.08    --  110.71 178.00  30.00   98
 52  \w     53.00  80.00   0.50    0.08    --  110.71 178.00 120.00   54
 53  \w    -82.00 -57.00   0.50    0.05    --    0.00 150.00-175.00   50
 54  \w   -110.00 -61.00   0.50    0.08    --  -55.36 150.00-175.00   98
 55  \w    -96.00 -20.00   0.50    0.08    -- -102.00  77.00-120.00  152
 56  \w    -53.00 -26.00   0.50    0.08    -- -102.00  50.00-120.00   54
 57  \w   -122.00 -79.00   0.50    0.08    -- -102.00 150.00-175.00   86
 58  \w   -136.00 -77.00   0.50    0.08    -- -102.00 -63.00   0.00  118
 59  \w   -113.00 -84.00   0.50    0.08    -- -102.00-122.00 -59.00   58
 60  \w   -118.00 -87.00   0.50    0.08    -- -102.00 -91.00-120.00   62
 61  \w   -137.00 -81.00   0.50    0.08    --  -55.36-122.00 -59.00  112
 62  \w   -107.00 -82.00   0.50    0.08    --  -55.36-125.00-120.00   50
 63  \w   -142.00-116.00   0.50    0.08    --  -55.36-125.00-120.00   52
 64  \w   -174.00-118.00   0.50    0.08    -- -102.00-122.00 -59.00  112
 65  \w   -138.00-111.00   0.50    0.08    --  -55.36-125.00  30.00   54
 66  \w    -86.00 -61.00   0.50    0.08    --  -55.36-150.00 138.00   50
 67  \w   -107.00 -82.00   0.50    0.08    -- -102.00 -91.00  60.00   50
 68  \w   -148.00-122.00   0.50    0.08    -- -102.00 -91.00  60.00   52
 69  \w   -175.00-150.00   0.50    0.08    -- -102.00 -63.00   0.00   50
 70  \w   -174.00-147.00   0.50    0.08    -- -102.00 -91.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18575
_diffrn_reflns_theta_full        71.3071
_diffrn_reflns_theta_max         71.31
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    5.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.4805
_exptl_crystal_description       Lump
_exptl_crystal_F_000             850.6197
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, diethylether'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.7457
_refine_diff_density_min         -0.5512
_refine_diff_density_rms         0.0774
_refine_ls_d_res_high            0.8139
_refine_ls_d_res_low             16.5535
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    71
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9914
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.0703
_refine_ls_shift/su_mean         0.0038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1549P)^2^+0.6871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2246
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5571
_reflns_number_total             6963
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           200317_horie_9_+60
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560164
_olex2_refinement_description
;
1. Restrained distances
 C27-C28
 1.54 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;