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_1560154
_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, C28 H40 O10, F6 P'
_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   geom
_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                83.4320(10)
_cell_angle_beta                 81.5860(10)
_cell_angle_gamma                76.3350(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2781(2)
_cell_length_b                   11.2893(2)
_cell_length_c                   19.2130(3)
_cell_measurement_reflns_used    20674
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      76.4790
_cell_measurement_theta_min      3.9600
_cell_volume                     2343.29(7)
_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      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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   -101.00 -65.00   0.50    0.05    --  -46.57-139.00-106.00   72
  2  \w   -120.00 -95.00   0.50    0.10    -- -102.00-139.00-106.00   50
  3  \w   -159.00-110.00   0.50    0.10    -- -102.00 -94.00   0.00   98
  4  \w   -147.00-122.00   0.50    0.10    -- -102.00-130.00  67.00   50
  5  \w   -113.00 -87.00   0.50    0.05    --  -46.57-130.00  67.00   52
  6  \w   -119.00 -88.00   0.50    0.10    -- -102.00 -15.00 -60.00   62
  7  \w    -85.00 -29.00   0.50    0.10    -- -102.00  77.00 -90.00  112
  8  \w    -63.00 -37.00   0.50    0.10    -- -102.00 125.00-120.00   52
  9  \w    -90.00 -40.00   0.50    0.05    --  -46.57 139.00 -46.00  100
 10  \w    -69.00 -44.00   0.50    0.10    -- -102.00  61.00-180.00   50
 11  \w   -112.00 -74.00   0.50    0.10    -- -102.00 125.00-120.00   76
 12  \w   -122.00 -30.00   0.50    0.10    -- -102.00 139.00 -46.00  184
 13  \w    -63.00 -32.00   0.50    0.10    -- -102.00  61.00 120.00   62
 14  \w    -81.00 -56.00   0.50    0.05    --  -46.57 130.00 139.00   50
 15  \w   -111.00 -29.00   0.50    0.10    -- -102.00 125.00 120.00  164
 16  \w   -112.00 -30.00   0.50    0.10    -- -102.00 130.00 139.00  164
 17  \w   -174.00 -98.00   0.50    0.10    -- -102.00 -45.00-120.00  152
 18  \w   -175.00-134.00   0.50    0.10    -- -102.00 -15.00 -60.00   82
 19  \w     24.00  96.00   0.50    0.05    --   46.57-130.00  67.00  144
 20  \w     73.00  98.00   0.50    0.10    --  104.61-130.00  67.00   50
 21  \w     67.00 110.00   0.50    0.10    --  104.61-125.00   0.00   86
 22  \w     80.00 108.00   0.50    0.10    --  104.61 -77.00  60.00   56
 23  \w     38.00  73.00   0.50    0.10    --  104.61 -61.00 -60.00   70
 24  \w     33.00  68.00   0.50    0.10    --  104.61 -94.00-120.00   70
 25  \w     37.00  71.00   0.50    0.10    --  104.61 -61.00-150.00   68
 26  \w     32.00  73.00   0.50    0.10    --  104.61 -61.00 -90.00   82
 27  \w     66.00  92.00   0.50    0.10    --  104.61-139.00-106.00   52
 28  \w     40.00  65.00   0.50    0.05    --   46.57-139.00-106.00   50
 29  \w     41.00 105.00   0.50    0.10    --  104.61 -94.00  30.00  128
 30  \w     48.00  96.00   0.50    0.10    --  104.61 -94.00  60.00   96
 31  \w     35.00  75.00   0.50    0.10    --  104.61 -77.00  60.00   80
 32  \w     92.00 173.00   0.50    0.10    --  104.61  45.00 120.00  162
 33  \w    105.00 131.00   0.50    0.10    --  104.61 130.00 139.00   52
 34  \w     92.00 176.00   0.50    0.10    --  104.61  45.00  60.00  168
 35  \w     85.00 129.00   0.50    0.10    --  104.61 139.00 -46.00   88
 36  \w     69.00 114.00   0.50    0.05    --   46.57 139.00 -46.00   90
 37  \w     34.00 116.00   0.50    0.05    --   46.57  77.00 120.00  164
 38  \w    -26.00  27.00   0.50    0.05    --   46.57 -19.00-120.00  106
 39  \w    -22.00  41.00   0.50    0.05    --   46.57 -37.00-150.00  126
 40  \w    -26.00  28.00   0.50    0.05    --   46.57 -19.00 150.00  108
;
_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      -0.0603277000
_diffrn_orient_matrix_UB_12      -0.1104211000
_diffrn_orient_matrix_UB_13      0.0188415000
_diffrn_orient_matrix_UB_21      0.0082328000
_diffrn_orient_matrix_UB_22      -0.0173591000
_diffrn_orient_matrix_UB_23      -0.0790734000
_diffrn_orient_matrix_UB_31      0.1279110000
_diffrn_orient_matrix_UB_32      -0.0858222000
_diffrn_orient_matrix_UB_33      0.0028421000
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_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            31533
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.651
_diffrn_reflns_theta_min         4.044
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60387
_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    1.420
_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         0.368
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00099(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         9414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0600P)^2^+1.0555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8917
_reflns_number_total             9414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1pf6-a_123k
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         FeCHONPF
_diffrn_oxdiff_digest_frames
;
019048314a605c2b2a7c1978695c4339d800072ff22
;
_diffrn_oxdiff_digest_hkl
;
0135c564717ae82c78ee463d3ddf92263d62a0
;
_reflns_odcompleteness_completeness 99.95
_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), C35(H35A,H35B), C8(H8A,H8B),
 C34(H34A,H34B), C44(H44A,H44B), C7(H7A,H7B), C23(H23A,H23B), C20(H20A,H20B),
 C45(H45A,H45B), C21(H21A,H21B), C33(H33A,H33B), C22(H22A,H22B), C31(H31A,H31B),
  C30(H30A,H30B), C46(H46A,H46B), C47(H47A,H47B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C6(H6), C10(H10), C17(H17), C14(H14), C39(H39), C18(H18), C28(H28),
 C5(H5), C41(H41), C13(H13), C40(H40), C16(H16), C12(H12), C2(H2), C3(H3),
 C11(H11), C15(H15), C25(H25), C27(H27), C26(H26)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              84067
_shelx_hkl_checksum              76357
_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 1.651
_oxdiff_exptl_absorpt_empirical_full_min 0.644