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_1560153
_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   mixed
_audit_creation_date             2020-09-23
_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                82.951(2)
_cell_angle_beta                 80.729(2)
_cell_angle_gamma                77.436(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3327(2)
_cell_length_b                   11.4193(2)
_cell_length_c                   19.3877(4)
_cell_measurement_reflns_used    13872
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      76.0930
_cell_measurement_theta_min      3.9060
_cell_volume                     2406.89(8)
_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      273(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.926
_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   -106.00 -65.00   0.50    0.07    --  -46.57-139.00-106.00   82
  2  \w   -120.00 -95.00   0.50    0.27    -- -102.00-139.00-106.00   50
  3  \w   -112.00 -76.00   0.50    0.27    -- -102.00-125.00-180.00   72
  4  \w   -119.00 -94.00   0.50    0.07    --  -46.57-125.00-180.00   50
  5  \w   -161.00-119.00   0.50    0.27    -- -102.00-125.00-180.00   84
  6  \w   -174.00 -80.00   0.50    0.27    -- -102.00 -77.00   0.00  188
  7  \w   -124.00 -97.00   0.50    0.27    -- -102.00-130.00  67.00   54
  8  \w   -119.00 -94.00   0.50    0.07    --  -46.57-130.00  67.00   50
  9  \w   -170.00-127.00   0.50    0.27    -- -102.00-130.00  67.00   86
 10  \w   -119.00 -91.00   0.50    0.27    -- -102.00 -30.00 120.00   56
 11  \w    -69.00 -34.00   0.50    0.27    -- -102.00  61.00 120.00   70
 12  \w    -66.00 -41.00   0.50    0.07    --  -46.57 130.00 139.00   50
 13  \w    -96.00 -71.00   0.50    0.27    -- -102.00 130.00 139.00   50
 14  \w   -108.00 -30.00   0.50    0.27    -- -102.00 112.00 145.52  156
 15  \w    -85.00 -49.00   0.50    0.07    --  -46.57 139.00 -46.00   72
 16  \w    -70.00 -30.00   0.50    0.27    -- -102.00 125.00 -90.00   80
 17  \w    -59.00 -29.00   0.50    0.27    -- -102.00 125.00-180.00   60
 18  \w    -23.00  29.00   0.50    0.07    --  -46.57  19.00 -30.00  104
 19  \w     69.00 118.00   0.50    0.07    --   46.57 139.00 -46.00   98
 20  \w     95.00 121.00   0.50    0.27    --  104.61 139.00 -46.00   52
 21  \w     88.00 169.00   0.50    0.27    --  104.61  61.00  30.00  162
 22  \w    101.00 126.00   0.50    0.27    --  104.61 130.00 139.00   50
 23  \w    102.00 176.00   0.50    0.27    --  104.61  61.00 150.00  148
 24  \w     92.00 173.00   0.50    0.27    --  104.61  45.00  60.00  162
 25  \w     78.00 103.00   0.50    0.27    --  104.61 -77.00  60.00   50
 26  \w     78.00 111.00   0.50    0.27    --  104.61-125.00 -30.00   66
 27  \w     67.00 105.00   0.50    0.27    --  104.61 -94.00 -60.00   76
 28  \w     53.00  78.00   0.50    0.27    --  104.61-139.00-106.00   50
 29  \w     45.00  71.00   0.50    0.27    --  104.61-125.00 -30.00   52
 30  \w     52.00  94.00   0.50    0.27    --  104.61-125.00 -90.00   84
 31  \w     39.00  72.00   0.50    0.27    --  104.61 -61.00-150.00   66
 32  \w     42.00  72.00   0.50    0.27    --  104.61 -61.00-120.00   60
 33  \w     59.00  84.00   0.50    0.07    --   46.57-139.00-106.00   50
 34  \w     34.00  66.00   0.50    0.27    --  104.61 -61.00  60.00   64
 35  \w     58.00 105.00   0.50    0.27    --  104.61 -94.00  90.00   94
 36  \w     38.00  66.00   0.50    0.27    --  104.61 -77.00  60.00   56
 37  \w     52.00 115.00   0.50    0.27    --  104.61-130.00  67.00  126
;
_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      -0.0617362000
_diffrn_orient_matrix_UB_12      -0.1095558000
_diffrn_orient_matrix_UB_13      0.0185741000
_diffrn_orient_matrix_UB_21      0.0098715000
_diffrn_orient_matrix_UB_22      -0.0158088000
_diffrn_orient_matrix_UB_23      -0.0786377000
_diffrn_orient_matrix_UB_31      0.1259743000
_diffrn_orient_matrix_UB_32      -0.0837355000
_diffrn_orient_matrix_UB_33      0.0027416000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.926
_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       -21
_diffrn_reflns_number            26322
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.420
_diffrn_reflns_theta_min         3.983
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68154
_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    1.382
_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         0.602
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9348
_refine_ls_number_restraints     798
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0888P)^2^+1.1302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8254
_reflns_number_total             9348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           1pf6-a_273k
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560153
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         FeC47H62O10NPF6
_diffrn_oxdiff_digest_frames
;
01f2c57c370b715a07efeebba119b7735700082d7b2
;
_diffrn_oxdiff_digest_hkl
;
01c7e224d8de3131933692fc243331859ca854
;
_reflns_odcompleteness_completeness 96.96
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 N1(H1B,H1C), C8(H8A,H8B), C9(H9A,H9B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C1D(H1DA,H1DB), C1E(H1EA,H1EB), C1H(H1HA,H1HB), C1M(H1MA,H1MB),
  C1S(H1SA,H1SB), C27(H27A,H27B), C29(H29A,H29B), C28(H28A,H28B), C32(H32A,
 H32B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C17(H17), C19(H19), C1A(H1A), C1F(H1F), C1G(H1G),
 C1I(H1I), C11(H11), C1K(H1K), C1L(H1L), C1N(H1N), C1O(H1O), C1Q(H1Q), C1R(H1R),
  C1T(H1T), C1V(H1V), C23(H23), C1Z(H1Z), C21(H21), C24(H24)
3.c Idealised Me refined as rotating group:
 C1U(H1UA,H1UB,H1UC)
;
_shelx_res_checksum              313
_shelx_hkl_checksum              64425
_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 1.685
_oxdiff_exptl_absorpt_empirical_full_min 0.597