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_1560167
_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         1001.83
_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                82.907(2)
_cell_angle_beta                 80.580(2)
_cell_angle_gamma                77.690(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3456(3)
_cell_length_b                   11.4668(3)
_cell_length_c                   19.4140(5)
_cell_measurement_reflns_used    15559
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      76.1320
_cell_measurement_theta_min      3.8710
_cell_volume                     2424.07(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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      303(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9612
_diffrn_measured_fraction_theta_max 0.9612
_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    -75.00 -49.00   0.50    0.08    --  -46.57 139.00 -46.00   52
  2  \w   -105.00 -76.00   0.50    0.33    -- -102.00 103.00-139.01   58
  3  \w   -109.00 -33.00   0.50    0.33    -- -102.00 125.00 -60.00  152
  4  \w    -24.00  29.00   0.50    0.08    --  -46.57  19.00 -30.00  106
  5  \w     69.00 119.00   0.50    0.08    --   46.57 139.00 -46.00  100
  6  \w     99.00 125.00   0.50    0.33    --  104.61 139.00 -46.00   52
  7  \w     93.00 173.00   0.50    0.33    --  104.61  45.00  60.00  160
  8  \w    101.00 126.00   0.50    0.33    --  104.61 130.00 139.00   50
  9  \w     90.00 170.00   0.50    0.33    --  104.61  61.00 150.00  160
 10  \w     71.00 116.00   0.50    0.08    --   46.57  77.00 120.00   90
 11  \w     92.00 153.00   0.50    0.33    --  104.61  45.00 -60.00  122
 12  \w     96.00 176.00   0.50    0.33    --  104.61  45.00-180.00  160
 13  \w     79.00 105.00   0.50    0.33    --  104.61 -94.00-150.00   52
 14  \w     76.00 102.00   0.50    0.33    --  104.61 -77.00-150.00   52
 15  \w     79.00 104.00   0.50    0.33    --  104.61 -94.00-120.00   50
 16  \w     96.00 122.00   0.50    0.33    --  104.61-139.00-107.00   52
 17  \w     56.00 100.00   0.50    0.08    --   46.57-139.00-107.00   88
 18  \w     35.00  73.00   0.50    0.33    --  104.61 -61.00 -90.00   76
 19  \w     32.00  74.00   0.50    0.33    --  104.61 -77.00-150.00   84
 20  \w     35.00  67.00   0.50    0.33    --  104.61 -61.00-150.00   64
 21  \w     36.00  73.00   0.50    0.33    --  104.61 -61.00 -60.00   74
 22  \w     32.00  62.00   0.50    0.33    --  104.61 -61.00  30.00   60
 23  \w     80.00 105.00   0.50    0.33    --  104.61 -94.00  90.00   50
 24  \w     66.00 104.00   0.50    0.33    --  104.61 -94.00  60.00   76
 25  \w     53.00 111.00   0.50    0.33    --  104.61-130.00  67.00  116
 26  \w     33.00  65.00   0.50    0.33    --  104.61 -94.00  90.00   64
 27  \w     26.00  97.00   0.50    0.08    --   46.57-130.00  67.00  142
 28  \w    -26.00  28.00   0.50    0.08    --   46.57 -19.00 150.00  108
 29  \w    -24.00  28.00   0.50    0.08    --   46.57 -19.00  60.00  104
 30  \w    -86.00 -61.00   0.50    0.08    --  -46.57 130.00 139.00   50
 31  \w   -108.00 -44.00   0.50    0.33    -- -102.00 130.00 139.00  128
 32  \w    -63.00 -33.00   0.50    0.33    -- -102.00  61.00 120.00   60
 33  \w   -105.00 -31.00   0.50    0.33    -- -102.00 103.00 114.87  148
 34  \w   -121.00 -95.00   0.50    0.33    -- -102.00 139.00 -46.00   52
 35  \w   -165.00 -91.00   0.50    0.33    -- -102.00 -30.00-120.00  148
 36  \w   -119.00 -94.00   0.50    0.08    --  -46.57-125.00-180.00   50
 37  \w   -106.00 -66.00   0.50    0.08    --  -46.57-139.00-107.00   80
 38  \w   -139.00-108.00   0.50    0.33    -- -102.00-139.00-107.00   62
 39  \w   -173.00 -99.00   0.50    0.33    -- -102.00 -94.00   0.00  148
 40  \w   -101.00 -72.00   0.50    0.08    --  -46.57-130.00  67.00   58
 41  \w   -147.00-122.00   0.50    0.33    -- -102.00-130.00  67.00   50
 42  \w   -175.00-130.00   0.50    0.33    -- -102.00 -30.00 120.00   90
;
_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      -0.0620122000
_diffrn_orient_matrix_UB_12      -0.1091929000
_diffrn_orient_matrix_UB_13      0.0184216000
_diffrn_orient_matrix_UB_21      0.0099840000
_diffrn_orient_matrix_UB_22      -0.0152470000
_diffrn_orient_matrix_UB_23      -0.0786097000
_diffrn_orient_matrix_UB_31      0.1255629000
_diffrn_orient_matrix_UB_32      -0.0831557000
_diffrn_orient_matrix_UB_33      0.0025538000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0297
_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       -24
_diffrn_reflns_number            32171
_diffrn_reflns_theta_full        76.3474
_diffrn_reflns_theta_max         76.35
_diffrn_reflns_theta_min         3.96
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42102
_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    1.3724
_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         0.5769
_refine_diff_density_min         -0.5269
_refine_diff_density_rms         0.0553
_refine_ls_d_res_high            0.7933
_refine_ls_d_res_low             11.1557
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0292
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0292
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+0.7063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8295
_reflns_number_total             9766
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1PF6-A_303K
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_original_cell_volume        2424.06(10)
_cod_database_code               1560167
_chemical_oxdiff_formula         FeC47H62O10NPF6
_diffrn_oxdiff_digest_frames
;
0129afcdea2435b7c0fdc3ada87c5021b900052fff2
;
_diffrn_oxdiff_digest_hkl
;
01932c5cb0c5e4decd486111e30bc4bc9c9587
;
_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), C36(H36a,H36b), C37(H37a,H37b), C7(H7a,H7b), C8(H8a,H8b),
 C44(H44a,H44b), C45(H45a,H45b), C21(H21a,H21b), C23(H23a,H23b), C22(H22a,H22b),
  C35(H35a,H35b), C46(H46a,H46b), C47(H47a,H47b), C30(H30a,H30b), C31(H31a,
 H31b), C33(H33a,H33b), C32(H32a,H32b)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C39(H39), C42(H42), C11(H11), C5(H5), C13(H13), C18(H18),
 C41(H41), C16(H16), C3(H3), C17(H17), C40(H40), C2(H2), C28(H28), C12(H12),
 C14(H14), 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 1.902
_oxdiff_exptl_absorpt_empirical_full_min 0.553