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_1560163
_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
_audit_creation_date             2020-09-22
_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                83.100(2)
_cell_angle_beta                 81.166(2)
_cell_angle_gamma                76.913(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3088(3)
_cell_length_b                   11.3689(3)
_cell_length_c                   19.3307(4)
_cell_measurement_reflns_used    19027
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      75.9540
_cell_measurement_theta_min      3.9360
_cell_volume                     2382.63(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      213
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9556
_diffrn_measured_fraction_theta_max 0.9556
_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    -64.00 -35.00   0.50    0.05    --  -46.57 130.00 139.00   58
  2  \w    -85.00 -59.00   0.50    0.12    -- -102.00 130.00 139.00   52
  3  \w    -75.00 -31.00   0.50    0.12    -- -102.00 125.00  60.00   88
  4  \w    -69.00 -37.00   0.50    0.12    -- -102.00  61.00   0.00   64
  5  \w    -68.00 -30.00   0.50    0.12    -- -102.00  61.00 -60.00   76
  6  \w    -61.00 -35.00   0.50    0.12    -- -102.00  77.00 -60.00   52
  7  \w    -22.00  27.00   0.50    0.05    --  -46.57  19.00   0.00   98
  8  \w    -18.00  24.00   0.50    0.05    --  -46.57  19.00 -60.00   84
  9  \w     69.00  95.00   0.50    0.05    --   46.57 139.00 -46.00   52
 10  \w     97.00 122.00   0.50    0.12    --  104.61 139.00 -46.00   50
 11  \w    146.00 172.00   0.50    0.12    --  104.61  77.00  30.00   52
 12  \w    104.00 174.00   0.50    0.12    --  104.61 130.00 139.00  140
 13  \w     92.00 172.00   0.50    0.12    --  104.61  45.00 -30.00  160
 14  \w     82.00 111.00   0.50    0.12    --  104.61  77.00  30.00   58
 15  \w     25.00 117.00   0.50    0.05    --   46.57  77.00 120.00  184
 16  \w     47.00  73.00   0.50    0.12    --  104.61 -61.00 -60.00   52
 17  \w     32.00 104.00   0.50    0.12    --  104.61 -94.00 -90.00  144
 18  \w     47.00 108.00   0.50    0.12    --  104.61-109.00-118.37  122
 19  \w     46.00 122.00   0.50    0.12    --  104.61-139.00-106.00  152
 20  \w     50.00 109.00   0.50    0.12    --  104.61-125.00-180.00  118
 21  \w     32.00 101.00   0.50    0.05    --   46.57-139.00-106.00  138
 22  \w     35.00  72.00   0.50    0.12    --  104.61 -61.00  30.00   74
 23  \w     48.00  73.00   0.50    0.12    --  104.61 -77.00  90.00   50
 24  \w     49.00  74.00   0.50    0.12    --  104.61-130.00  67.00   50
 25  \w     27.00  71.00   0.50    0.05    --   46.57-130.00  67.00   88
 26  \w    -26.00  27.00   0.50    0.05    --   46.57 -19.00 150.00  106
 27  \w    -96.00 -70.00   0.50    0.05    --  -46.57 130.00 139.00   52
 28  \w    -63.00 -31.00   0.50    0.12    -- -102.00  61.00 150.00   64
 29  \w    -64.00 -31.00   0.50    0.12    -- -102.00  61.00 120.00   66
 30  \w    -99.00 -60.00   0.50    0.05    --  -46.57 139.00 -46.00   78
 31  \w    -94.00 -69.00   0.50    0.12    -- -102.00  77.00 -30.00   50
 32  \w   -101.00 -76.00   0.50    0.12    -- -102.00  77.00 -60.00   50
 33  \w   -122.00 -33.00   0.50    0.12    -- -102.00 139.00 -46.00  178
 34  \w   -111.00 -83.00   0.50    0.12    -- -102.00 125.00  60.00   56
 35  \w   -107.00 -74.00   0.50    0.12    -- -102.00 105.00 124.57   66
 36  \w   -173.00 -92.00   0.50    0.12    -- -102.00 -45.00 150.00  162
 37  \w   -119.00 -94.00   0.50    0.05    --  -46.57-130.00  67.00   50
 38  \w   -147.00-122.00   0.50    0.12    -- -102.00-130.00  67.00   50
 39  \w   -171.00 -85.00   0.50    0.12    -- -102.00 -61.00  60.00  172
 40  \w   -105.00 -65.00   0.50    0.05    --  -46.57-139.00-106.00   80
 41  \w   -144.00-119.00   0.50    0.12    -- -102.00-139.00-106.00   50
 42  \w   -175.00-105.00   0.50    0.12    -- -102.00 -30.00 -60.00  140
 43  \w     88.00 164.00   0.50    0.12    --  104.61  77.00-150.00  152
;
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       14
_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            33397
_diffrn_reflns_theta_full        76.3417
_diffrn_reflns_theta_max         76.34
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    3.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66572
_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_density_diffrn    1.3963
_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         0.4448
_refine_diff_density_min         -0.4547
_refine_diff_density_rms         0.0519
_refine_ls_d_res_high            0.7934
_refine_ls_d_res_low             11.0300
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0297
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0297
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.8210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_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                8710
_reflns_number_total             9550
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1pf6-a_213k
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560163
_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), C37(H37a,H37b), C36(H36a,H36b), C8(H8a,H8b), C7(H7a,H7b),
 C35(H35a,H35b), C44(H44a,H44b), C45(H45a,H45b), C20(H20a,H20b), C22(H22a,H22b),
  C23(H23a,H23b), C21(H21a,H21b), C31(H31a,H31b), C30(H30a,H30b), C33(H33a,
 H33b), C46(H46a,H46b), C32(H32a,H32b), C47(H47a,H47b)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6), C10(H10), C5(H5), C39(H39), C18(H18), C28(H28), C41(H41),
 C40(H40), C17(H17), C14(H14), C13(H13), C2(H2), C11(H11), C16(H16), C3(H3),
 C12(H12), C15(H15), C27(H27), C25(H25), C26(H26)
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
;