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_1560156
_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         1001.79
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-09-24 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                83.024(2)
_cell_angle_beta                 80.932(2)
_cell_angle_gamma                77.121(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3259(3)
_cell_length_b                   11.3917(3)
_cell_length_c                   19.3628(5)
_cell_measurement_reflns_used    19063
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      76.1150
_cell_measurement_theta_min      3.9700
_cell_volume                     2395.24(11)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      243(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_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   -119.00 -75.00   0.50    0.05    --  -46.57-139.00-106.00   88
  2  \w   -144.00-119.00   0.50    0.21    -- -102.00-139.00-106.00   50
  3  \w   -173.00 -91.00   0.50    0.21    -- -102.00 -45.00 -30.00  164
  4  \w   -118.00 -31.00   0.50    0.05    --  -46.57 -77.00  60.00  174
  5  \w    -23.00  29.00   0.50    0.05    --  -46.57  19.00 -30.00  104
  6  \w     70.00 119.00   0.50    0.05    --   46.57 139.00 -46.00   98
  7  \w     75.00 101.00   0.50    0.21    --  104.61 139.00 -46.00   52
  8  \w     32.00 117.00   0.50    0.05    --   46.57  57.00   0.00  170
  9  \w    101.00 126.00   0.50    0.21    --  104.61 130.00 139.00   50
 10  \w     92.00 176.00   0.50    0.21    --  104.61  45.00  30.00  168
 11  \w     92.00 164.00   0.50    0.21    --  104.61  45.00  60.00  144
 12  \w     73.00  99.00   0.50    0.21    --  104.61 -77.00  60.00   52
 13  \w     64.00  91.00   0.50    0.21    --  104.61-130.00  67.00   54
 14  \w     64.00 103.00   0.50    0.21    --  104.61 -94.00  30.00   78
 15  \w     59.00 101.00   0.50    0.05    --   46.57-139.00-106.00   84
 16  \w     53.00 119.00   0.50    0.21    --  104.61-139.00-106.00  132
 17  \w     78.00 103.00   0.50    0.21    --  104.61 -77.00-120.00   50
 18  \w     33.00  70.00   0.50    0.21    --  104.61 -77.00-120.00   74
 19  \w     33.00  64.00   0.50    0.21    --  104.61 -61.00-120.00   62
 20  \w     33.00 101.00   0.50    0.21    --  104.61 -94.00 -90.00  136
 21  \w     36.00 107.00   0.50    0.21    --  104.61-125.00  30.00  142
 22  \w     59.00  84.00   0.50    0.05    --   46.57-130.00  67.00   50
 23  \w     34.00  59.00   0.50    0.21    --  104.61 -77.00  60.00   50
 24  \w     41.00  70.00   0.50    0.21    --  104.61 -61.00  60.00   58
 25  \w     33.00  73.00   0.50    0.21    --  104.61 -61.00  90.00   80
 26  \w    -27.00  22.00   0.50    0.05    --   46.57 -19.00  60.00   98
 27  \w    -85.00 -60.00   0.50    0.05    --  -46.57 139.00 -46.00   50
 28  \w    -68.00 -42.00   0.50    0.21    -- -102.00  61.00   0.00   52
 29  \w    -69.00 -42.00   0.50    0.21    -- -102.00  61.00 -30.00   54
 30  \w    -68.00 -43.00   0.50    0.21    -- -102.00  61.00 -90.00   50
 31  \w    -59.00 -34.00   0.50    0.21    -- -102.00 107.00-126.94   50
 32  \w   -107.00 -70.00   0.50    0.21    -- -102.00 107.00-126.94   74
 33  \w   -122.00 -31.00   0.50    0.21    -- -102.00 139.00 -46.00  182
 34  \w    -98.00 -68.00   0.50    0.21    -- -102.00  77.00 120.00   60
 35  \w    -55.00 -30.00   0.50    0.21    -- -102.00  77.00 120.00   50
 36  \w    -80.00 -55.00   0.50    0.21    -- -102.00 130.00 139.00   50
 37  \w    -67.00 -33.00   0.50    0.05    --  -46.57 130.00 139.00   68
 38  \w   -108.00 -29.00   0.50    0.21    -- -102.00 109.00 134.13  158
 39  \w   -151.00-109.00   0.50    0.21    -- -102.00 -45.00 150.00   84
 40  \w   -105.00 -71.00   0.50    0.05    --  -46.57-130.00  67.00   68
 41  \w   -147.00-122.00   0.50    0.21    -- -102.00-130.00  67.00   50
 42  \w   -172.00 -99.00   0.50    0.21    -- -102.00 -30.00 -60.00  146
 43  \w   -175.00 -97.00   0.50    0.21    -- -102.00 -15.00-180.00  156
;
_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      -0.0612943000
_diffrn_orient_matrix_UB_12      -0.1097628000
_diffrn_orient_matrix_UB_13      0.0184622000
_diffrn_orient_matrix_UB_21      0.0095409000
_diffrn_orient_matrix_UB_22      -0.0158380000
_diffrn_orient_matrix_UB_23      -0.0787135000
_diffrn_orient_matrix_UB_31      0.1264186000
_diffrn_orient_matrix_UB_32      -0.0842741000
_diffrn_orient_matrix_UB_33      0.0027353000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_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            33262
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.580
_diffrn_reflns_theta_min         3.997
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62878
_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    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_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         0.452
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.7846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8740
_reflns_number_total             9609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1pf6-a_243k
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560156
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         FeCHONPF
_diffrn_oxdiff_digest_frames
;
01f4f5956d43c94d8ecf62532d0d9c17350008809a2
;
_diffrn_oxdiff_digest_hkl
;
0106ab308fa6fb57ae4b277306168827cf4670
;
_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), C37(H37A,H37B), C36(H36A,H36B), C8(H8A,H8B), C44(H44A,H44B),
 C7(H7A,H7B), C35(H35A,H35B), C45(H45A,H45B), C23(H23A,H23B), C22(H22A,H22B),
 C21(H21A,H21B), C20(H20A,H20B), C46(H46A,H46B), C30(H30A,H30B), C47(H47A,H47B),
  C33(H33A,H33B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6), C10(H10), C39(H39), C5(H5), C2(H2), C41(H41), C3(H3),
 C28(H28), C13(H13), C11(H11), C14(H14), C18(H18), C17(H17), C40(H40), C16(H16),
  C12(H12), C15(H15), C27(H27), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              443
_shelx_hkl_checksum              21567
_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 1.791
_oxdiff_exptl_absorpt_empirical_full_min 0.620