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_1560165
_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         'C19 H22 Fe N, F6 P, C28 H40 O10'
_chemical_formula_sum            'C47 H62 F6 Fe N O10 P'
_chemical_formula_weight         1001.83
_chemical_name_systematic
'[N-(4-methylbenzyl)ammoniumethylferrocene hexafluorophosphate][dibenzo[30]crown-10 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
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-15
_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                82.910(2)
_cell_angle_beta                 80.543(2)
_cell_angle_gamma                77.861(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3611(2)
_cell_length_b                   11.5447(3)
_cell_length_c                   19.4228(5)
_cell_measurement_reflns_used    8954
_cell_measurement_temperature    333(2)
_cell_measurement_theta_max      70.5820
_cell_measurement_theta_min      2.3130
_cell_volume                     2446.24(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      333(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9781
_diffrn_measured_fraction_theta_max 0.9781
_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    -49.00 -24.00   0.50    0.06    --    0.00 131.00 136.00   50
  2  \w     10.00  82.00   0.50    0.06    --    0.00  19.00  60.00  144
  3  \w     89.00 115.00   0.50    0.25    --   55.36 131.00 136.00   52
  4  \w     80.00 127.00   0.50    0.25    --  110.71 131.00 136.00   94
  5  \w    120.00 146.00   0.50    0.25    --  110.71 178.00  90.00   52
  6  \w     93.00 119.00   0.50    0.25    --   55.36 125.00  30.00   52
  7  \w     72.00 130.00   0.50    0.25    --   55.36 137.00 -47.00  116
  8  \w    111.00 136.00   0.50    0.25    --   55.36 125.00-120.00   50
  9  \w    152.00 178.00   0.50    0.25    --  110.71  63.00-120.00   52
 10  \w     90.00 120.00   0.50    0.25    --  110.71 111.00 -60.00   60
 11  \w     77.00 130.00   0.50    0.25    --  110.71  63.00-120.00  106
 12  \w     87.00 136.00   0.50    0.25    --  110.71 111.00-180.00   98
 13  \w     72.00 107.00   0.50    0.25    --  110.71 137.00 -47.00   70
 14  \w     56.00 126.00   0.50    0.25    --  110.71 178.00  30.00  140
 15  \w     48.00  89.00   0.50    0.25    --  110.71 178.00  90.00   82
 16  \w     48.00 135.00   0.50    0.25    --  110.71 178.00  60.00  174
 17  \w     27.00  59.00   0.50    0.06    --    0.00  19.00-180.00   64
 18  \w     -3.00  25.00   0.50    0.25    --  -55.36  15.00-180.00   56
 19  \w    -23.00  22.00   0.50    0.06    --    0.00  19.00-180.00   90
 20  \w    -18.00  25.00   0.50    0.25    --  -55.36  15.00 -90.00   86
 21  \w    -17.00  27.00   0.50    0.25    --  -55.36  15.00 -60.00   88
 22  \w    -13.00  24.00   0.50    0.25    --  -55.36  15.00   0.00   74
 23  \w    -29.00   1.00   0.50    0.25    --  -55.36  30.00   0.00   60
 24  \w    -29.00  13.00   0.50    0.25    --  -55.36  30.00  60.00   84
 25  \w    -13.00  12.00   0.50    0.25    --  -55.36  15.00  90.00   50
 26  \w    -16.00  24.00   0.50    0.25    --  -55.36  15.00 150.00   80
 27  \w     -9.00  33.00   0.50    0.06    --    0.00 -99.00  60.00   84
 28  \w     24.00  49.00   0.50    0.06    --    0.00-131.00  65.00   50
 29  \w     49.00 110.00   0.50    0.25    --   55.36-131.00  65.00  122
 30  \w     57.00 117.00   0.50    0.25    --  110.71-131.00  65.00  120
 31  \w     68.00 104.00   0.50    0.25    --  110.71 -91.00  60.00   72
 32  \w     54.00 178.00   0.50    0.25    --  110.71   0.00 -30.00  248
 33  \w     74.00 111.00   0.50    0.25    --  110.71-137.00-110.00   74
 34  \w     78.00 107.00   0.50    0.25    --  110.71-111.00-180.00   58
 35  \w     66.00 106.00   0.50    0.25    --   55.36-137.00-110.00   80
 36  \w     36.00 107.00   0.50    0.25    --  110.71-111.00 -90.00  142
 37  \w     31.00  74.00   0.50    0.25    --  110.71 -63.00  60.00   86
 38  \w     31.00  56.00   0.50    0.25    --  110.71 -50.00  60.00   50
 39  \w     27.00  76.00   0.50    0.25    --  110.71 -63.00 120.00   98
 40  \w     27.00  98.00   0.50    0.25    --  110.71 -77.00  60.00  142
 41  \w     31.00  58.00   0.50    0.25    --  110.71 -63.00 -90.00   54
 42  \w     28.00  75.00   0.50    0.25    --  110.71 -63.00 -30.00   94
 43  \w     27.00  52.00   0.50    0.25    --  110.71 -50.00-120.00   50
 44  \w     29.00  74.00   0.50    0.25    --  110.71 -63.00-180.00   90
 45  \w     27.00  52.00   0.50    0.25    --  110.71-111.00-180.00   50
 46  \w     14.00  46.00   0.50    0.25    --  110.71   0.00 -30.00   64
 47  \w     21.00  64.00   0.50    0.25    --  110.71 -91.00  60.00   86
 48  \w     28.00  71.00   0.50    0.25    --  110.71 -63.00 150.00   86
 49  \w     28.00  53.00   0.50    0.06    --    0.00-137.00-110.00   50
 50  \w    -22.00  16.00   0.50    0.25    --  -55.36  15.00-150.00   76
 51  \w    -47.00 -19.00   0.50    0.25    -- -102.00  50.00-180.00   56
 52  \w    -52.00 -19.00   0.50    0.25    -- -102.00  50.00 -90.00   66
 53  \w    -53.00 -27.00   0.50    0.25    -- -102.00  50.00 -60.00   52
 54  \w    -44.00 -19.00   0.50    0.25    -- -102.00  50.00   0.00   50
 55  \w    -53.00 -21.00   0.50    0.25    -- -102.00 131.00 136.00   64
 56  \w    -65.00 -40.00   0.50    0.25    -- -102.00 178.00 150.00   50
 57  \w    -73.00 -48.00   0.50    0.06    --    0.00 137.00 -47.00   50
 58  \w   -119.00 -52.00   0.50    0.25    -- -102.00 137.00 -47.00  134
 59  \w   -147.00-100.00   0.50    0.25    -- -102.00 178.00 150.00   94
 60  \w    -87.00 -62.00   0.50    0.25    -- -102.00 -63.00 -60.00   50
 61  \w   -133.00 -75.00   0.50    0.25    --  -55.36-137.00-110.00  116
 62  \w   -142.00 -74.00   0.50    0.25    --  -55.36-125.00 -30.00  136
 63  \w   -140.00 -72.00   0.50    0.25    --  -55.36-131.00  65.00  136
 64  \w   -108.00 -83.00   0.50    0.25    --  -55.36-125.00 150.00   50
 65  \w   -140.00-115.00   0.50    0.25    --  -55.36-125.00 150.00   50
 66  \w   -171.00-104.00   0.50    0.25    -- -102.00 -63.00 -60.00  134
 67  \w   -145.00-120.00   0.50    0.25    -- -102.00-137.00-110.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0618906000
_diffrn_orient_matrix_UB_12      -0.1088797000
_diffrn_orient_matrix_UB_13      0.0150200000
_diffrn_orient_matrix_UB_21      0.0117642000
_diffrn_orient_matrix_UB_22      -0.0098295000
_diffrn_orient_matrix_UB_23      -0.0793196000
_diffrn_orient_matrix_UB_31      0.1251734000
_diffrn_orient_matrix_UB_32      -0.0826984000
_diffrn_orient_matrix_UB_33      0.0019891000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25365
_diffrn_reflns_theta_full        71.2819
_diffrn_reflns_theta_max         71.28
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.3600
_exptl_crystal_description       block
_exptl_crystal_F_000             1054.0329
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone, CH2Cl2, diethylether'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.5156
_refine_diff_density_min         -0.3837
_refine_diff_density_rms         0.0571
_refine_ls_d_res_high            0.8140
_refine_ls_d_res_low             19.0773
_refine_ls_goodness_of_fit_ref   1.0375
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    103
_refine_ls_number_parameters     596
_refine_ls_number_reflns         9289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0375
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1217P)^2^+0.7534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7518
_reflns_number_total             9289
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1PF6-A_333K
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560165
_chemical_oxdiff_formula         FeC47H62NOPF6
_diffrn_oxdiff_digest_frames
;
013fd1001ca0e8396d6457f30a3f7d180f000501c3e
;
_diffrn_oxdiff_digest_hkl
;
01fa085c53ab132bf0ef97540a6e122747fe7a
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1a,H1b), C7(H7a,H7b), C37(H37a,H37b), C8(H8a,H8b), C36(H36a,H36b),
 C23(H23a,H23b), C44(H44a,H44b), C21(H21a,H21b), C45(H45a,H45b), C20(H20a,H20b),
  C22(H22a,H22b), C47(H47a,H47b), C35(H35a,H35b), C46(H46a,H46b), C34(H34a,
 H34b), C30(H30a,H30b), C33(H33a,H33b), C31(H31a,H31b), C32(H32a,H32b)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6), C39(H39), C10(H10), C5(H5), C3(H3), C2(H2), C11(H11),
 C41(H41), C13(H13), C28(H28), C14(H14), C18(H18), C17(H17), C12(H12), C40(H40),
  C16(H16), C27(H27), C25(H25), C26(H26), C15(H15)
2.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.483
_oxdiff_exptl_absorpt_empirical_full_min 0.668