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_1560162
_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             2019-09-14
_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                83.330(2)
_cell_angle_beta                 81.460(2)
_cell_angle_gamma                76.478(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2892(2)
_cell_length_b                   11.3208(3)
_cell_length_c                   19.2519(4)
_cell_measurement_reflns_used    20371
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      76.3930
_cell_measurement_theta_min      3.9980
_cell_volume                     2357.22(9)
_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      153(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9564
_diffrn_measured_fraction_theta_max 0.9564
_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   -114.00 -72.00   0.50    0.05    --  -46.57-139.00-106.00   84
  2  \w   -108.00 -83.00   0.50    0.05    --  -46.57-125.00 -60.00   50
  3  \w   -120.00 -89.00   0.50    0.11    -- -102.00 -45.00 -30.00   62
  4  \w   -129.00-103.00   0.50    0.11    -- -102.00 -30.00 -30.00   52
  5  \w   -127.00-100.00   0.50    0.11    -- -102.00 -30.00 -60.00   54
  6  \w   -153.00-125.00   0.50    0.11    -- -102.00 -45.00 -30.00   56
  7  \w   -174.00 -90.00   0.50    0.11    -- -102.00 -45.00-120.00  168
  8  \w   -144.00-119.00   0.50    0.11    -- -102.00-139.00-106.00   50
  9  \w   -175.00-131.00   0.50    0.11    -- -102.00 -30.00 -60.00   88
 10  \w    -67.00 -39.00   0.50    0.11    -- -102.00  61.00   0.00   56
 11  \w    -85.00 -60.00   0.50    0.05    --  -46.57 139.00 -46.00   50
 12  \w   -112.00 -80.00   0.50    0.11    -- -102.00 125.00-120.00   64
 13  \w    -66.00 -41.00   0.50    0.11    -- -102.00 125.00-120.00   50
 14  \w    -69.00 -34.00   0.50    0.11    -- -102.00  61.00-180.00   70
 15  \w    -24.00  29.00   0.50    0.05    --  -46.57  19.00 -30.00  106
 16  \w     69.00 119.00   0.50    0.05    --   46.57 139.00 -46.00  100
 17  \w     97.00 122.00   0.50    0.11    --  104.61 139.00 -46.00   50
 18  \w     93.00 173.00   0.50    0.11    --  104.61  45.00  60.00  160
 19  \w     83.00 108.00   0.50    0.11    --  104.61 -77.00  60.00   50
 20  \w     74.00 105.00   0.50    0.11    --  104.61 -94.00  90.00   62
 21  \w     42.00  71.00   0.50    0.11    --  104.61 -61.00  60.00   58
 22  \w     41.00  71.00   0.50    0.11    --  104.61 -77.00  60.00   60
 23  \w     32.00 110.00   0.50    0.11    --  104.61-130.00  67.00  156
 24  \w     53.00  93.00   0.50    0.11    --  104.61-125.00 -30.00   80
 25  \w     56.00 107.00   0.50    0.11    --  104.61 -77.00-120.00  102
 26  \w     56.00  95.00   0.50    0.05    --   46.57-139.00-106.00   78
 27  \w     34.00 117.00   0.50    0.11    --  104.61-139.00-106.00  166
 28  \w     28.00  96.00   0.50    0.05    --   46.57-130.00  67.00  136
 29  \w     33.00  73.00   0.50    0.11    --  104.61 -61.00  90.00   80
 30  \w     32.00  71.00   0.50    0.11    --  104.61 -61.00 150.00   78
 31  \w     45.00 111.00   0.50    0.11    --  104.61-125.00  90.00  132
 32  \w     34.00  80.00   0.50    0.11    --  104.61 -77.00-150.00   92
 33  \w    -27.00   8.00   0.50    0.05    --   46.57 -19.00 -90.00   70
 34  \w    -23.00  28.00   0.50    0.05    --   46.57 -19.00 120.00  102
 35  \w    -79.00 -54.00   0.50    0.05    --  -46.57 130.00 139.00   50
 36  \w   -111.00 -70.00   0.50    0.11    -- -102.00 130.00 139.00   82
 37  \w   -122.00 -45.00   0.50    0.11    -- -102.00 139.00 -46.00  154
 38  \w   -107.00 -45.00   0.50    0.11    -- -102.00 125.00 -90.00  124
 39  \w   -123.00 -92.00   0.50    0.11    -- -102.00 -45.00 150.00   62
 40  \w   -118.00 -46.00   0.50    0.05    --  -46.57 -77.00  90.00  144
 41  \w   -104.00 -76.00   0.50    0.05    --  -46.57-130.00  67.00   56
 42  \w   -132.00 -99.00   0.50    0.11    -- -102.00-130.00  67.00   66
 43  \w   -175.00 -89.00   0.50    0.11    -- -102.00 -15.00 120.00  172
 44  \w     81.00 106.00   0.50    0.11    --  104.61 130.00 139.00   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      -0.0605047000
_diffrn_orient_matrix_UB_12      -0.1101816000
_diffrn_orient_matrix_UB_13      0.0187490000
_diffrn_orient_matrix_UB_21      0.0085864000
_diffrn_orient_matrix_UB_22      -0.0170529000
_diffrn_orient_matrix_UB_23      -0.0789638000
_diffrn_orient_matrix_UB_31      0.1275960000
_diffrn_orient_matrix_UB_32      -0.0854408000
_diffrn_orient_matrix_UB_33      0.0028899000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0354
_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       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32523
_diffrn_reflns_theta_full        76.4212
_diffrn_reflns_theta_max         76.42
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67347
_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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4114
_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         0.2891
_refine_diff_density_min         -0.4457
_refine_diff_density_rms         0.0521
_refine_ls_d_res_high            0.7931
_refine_ls_d_res_low             10.9674
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.8828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    103
_refine_ls_number_parameters     597
_refine_ls_number_reflns         9485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8828
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.0113
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+0.9474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0988
_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              24
_reflns_limit_l_min              0
_reflns_number_gt                8895
_reflns_number_total             9485
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1PF6-A_153K
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560162
_diffrn_oxdiff_digest_frames
;
01af902563cf4016f4e9233bcb41a1253e00083d064
;
_diffrn_oxdiff_digest_hkl
;
01ee72defb7a2bc5505ae0eba4758ba83719bc
;
_reflns_odcompleteness_completeness 99.94
_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), C36(H36a,H36b), C37(H37a,H37b), C35(H35a,H35b), C8(H8a,H8b),
 C44(H44a,H44b), C7(H7a,H7b), C34(H34a,H34b), C22(H22a,H22b), C45(H45a,H45b),
 C23(H23a,H23b), C20(H20a,H20b), C21(H21a,H21b), C33(H33a,H33b), C31(H31a,H31b),
  C32(H32a,H32b), C46(H46a,H46b), C47(H47a,H47b), C30(H30a,H30b)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6), C10(H10), C5(H5), C39(H39), C18(H18), C17(H17), C41(H41),
 C40(H40), C14(H14), C28(H28), C13(H13), C16(H16), C3(H3), C11(H11), C2(H2),
 C12(H12), C15(H15), C25(H25), C27(H27), 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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.544
_oxdiff_exptl_absorpt_empirical_full_min 0.576