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_1560174
_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         'C12 H16 Fe N, F6 P, C H2 Cl2, C20 H24 O6'
_chemical_formula_sum            'C33 H42 Cl2 F6 Fe N O6 P'
_chemical_formula_weight         820.42
_chemical_name_systematic
'[ferrocenylmethyl(methy) ammonium hexafluorophosphate][dibenzo[18]crown-6 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
_audit_creation_date             2020-09-22
_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                94.613(3)
_cell_angle_beta                 95.802(3)
_cell_angle_gamma                104.684(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8649(3)
_cell_length_b                   11.7188(4)
_cell_length_c                   16.7606(6)
_cell_measurement_reflns_used    6251
_cell_measurement_temperature    358(2)
_cell_measurement_theta_max      71.0030
_cell_measurement_theta_min      2.6950
_cell_volume                     1853.36(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      358
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9741
_diffrn_measured_fraction_theta_max 0.9741
_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     19.00  44.00   0.50    0.05    --    0.00-122.00 -59.00   50
  2  \w     40.00  66.00   0.50    0.11    --   55.36-122.00 -59.00   52
  3  \w     27.00  52.00   0.50    0.11    --  110.71-122.00 -59.00   50
  4  \w     35.00 106.00   0.50    0.11    --  110.71-111.00 -30.00  142
  5  \w     79.00 107.00   0.50    0.11    --  110.71-111.00 -60.00   56
  6  \w     57.00 107.00   0.50    0.11    --  110.71-111.00-150.00  100
  7  \w     46.00  73.00   0.50    0.11    --  110.71 -63.00 -30.00   54
  8  \w     33.00  59.00   0.50    0.11    --  110.71 -50.00   0.00   52
  9  \w     28.00  58.00   0.50    0.11    --  110.71 -50.00  30.00   60
 10  \w     67.00  98.00   0.50    0.11    --  110.71 -91.00  90.00   62
 11  \w     65.00 130.00   0.50    0.11    --  110.71-150.00 138.00  130
 12  \w     56.00  81.00   0.50    0.11    --   55.36-150.00 138.00   50
 13  \w     33.00  58.00   0.50    0.05    --    0.00-150.00 138.00   50
 14  \w     48.00  77.00   0.50    0.05    --    0.00  19.00 -60.00   58
 15  \w     36.00  61.00   0.50    0.05    --    0.00  19.00-150.00   50
 16  \w     -4.00  29.00   0.50    0.05    --    0.00  19.00-150.00   66
 17  \w    -22.00  42.00   0.50    0.05    --    0.00  19.00 -60.00  128
 18  \w    -15.00  11.00   0.50    0.11    --  -55.36  15.00 -30.00   52
 19  \w    -19.00  11.00   0.50    0.11    --  -55.36  15.00 -90.00   60
 20  \w    -13.00  24.00   0.50    0.11    --  -55.36  15.00-120.00   74
 21  \w    -33.00  27.00   0.50    0.11    --  -55.36  30.00 -60.00  120
 22  \w    -29.00  19.00   0.50    0.11    --  -55.36  30.00  30.00   96
 23  \w    -22.00  14.00   0.50    0.11    --  -55.36  15.00   0.00   72
 24  \w    -54.00 -20.00   0.50    0.11    -- -102.00  50.00 -30.00   68
 25  \w    -59.00 -30.00   0.50    0.11    -- -102.00 122.00  22.00   58
 26  \w    -89.00 -55.00   0.50    0.11    --  -55.36 122.00  22.00   68
 27  \w    -65.00 -40.00   0.50    0.05    --    0.00 122.00  22.00   50
 28  \w    -82.00 -57.00   0.50    0.05    --    0.00 150.00-175.00   50
 29  \w   -112.00 -54.00   0.50    0.11    --  -55.36 150.00-175.00  116
 30  \w   -102.00 -77.00   0.50    0.11    -- -102.00 150.00-175.00   50
 31  \w   -102.00 -20.00   0.50    0.11    -- -102.00 111.00-150.00  164
 32  \w    -55.00 -19.00   0.50    0.11    -- -102.00  50.00-120.00   72
 33  \w   -106.00 -64.00   0.50    0.11    -- -102.00 122.00  22.00   84
 34  \w   -126.00 -72.00   0.50    0.11    -- -102.00 -63.00   0.00  108
 35  \w   -123.00 -81.00   0.50    0.11    --  -55.36-122.00 -59.00   84
 36  \w   -103.00 -75.00   0.50    0.11    --  -55.36-125.00  30.00   56
 37  \w    -85.00 -60.00   0.50    0.11    --  -55.36-150.00 138.00   50
 38  \w   -142.00-110.00   0.50    0.11    --  -55.36-125.00  30.00   64
 39  \w   -116.00 -81.00   0.50    0.11    -- -102.00-122.00 -59.00   70
 40  \w   -116.00 -91.00   0.50    0.11    -- -102.00 -91.00-120.00   50
 41  \w   -123.00 -98.00   0.50    0.11    --  -55.36 -94.00-180.00   50
 42  \w   -150.00-125.00   0.50    0.11    --  -55.36 -94.00-180.00   50
 43  \w   -175.00-150.00   0.50    0.11    -- -102.00 -91.00-120.00   50
 44  \w   -175.00-148.00   0.50    0.11    -- -102.00 -63.00   0.00   54
 45  \w     65.00 137.00   0.50    0.11    --   55.36 150.00-175.00  144
 46  \w     89.00 114.00   0.50    0.11    --  110.71 150.00-175.00   50
 47  \w     87.00 136.00   0.50    0.11    --  110.71 111.00-120.00   98
 48  \w    142.00 175.00   0.50    0.11    --  110.71 111.00-120.00   66
 49  \w     99.00 128.00   0.50    0.11    --  110.71 122.00  22.00   58
 50  \w    114.00 173.00   0.50    0.11    --  110.71 111.00  90.00  118
 51  \w    116.00 141.00   0.50    0.11    --  110.71 178.00 120.00   50
 52  \w     94.00 138.00   0.50    0.11    --   55.36 125.00 150.00   88
 53  \w     82.00 107.00   0.50    0.11    --   55.36 122.00  22.00   50
 54  \w     87.00 133.00   0.50    0.11    --   55.36 125.00 -60.00   92
 55  \w     84.00 127.00   0.50    0.11    --   55.36 125.00 -90.00   86
 56  \w     88.00 113.00   0.50    0.11    --  110.71 178.00-120.00   50
 57  \w     47.00 141.00   0.50    0.11    --  110.71 178.00 -90.00  188
 58  \w     88.00 174.00   0.50    0.11    --  110.71 111.00   0.00  172
 59  \w     57.00  82.00   0.50    0.11    --  110.71 178.00 120.00   50
 60  \w     49.00  81.00   0.50    0.11    --  110.71 178.00-120.00   64
 61  \w     13.00 173.00   0.50    0.11    --  110.71  12.00 -60.00  320
 62  \w     42.00  68.00   0.50    0.11    --  110.71-111.00 -60.00   52
 63  \w     31.00  56.00   0.50    0.11    --  110.71 -50.00 -90.00   50
 64  \w     28.00  59.00   0.50    0.11    --  110.71 -50.00 -60.00   62
 65  \w     28.00  53.00   0.50    0.11    --  110.71 -50.00 -30.00   50
 66  \w     32.00  57.00   0.50    0.11    --  110.71 -50.00  60.00   50
 67  \w     30.00  55.00   0.50    0.11    --  110.71 -50.00  90.00   50
 68  \w     34.00  59.00   0.50    0.11    --  110.71 -50.00 120.00   50
 69  \w     27.00  59.00   0.50    0.11    --  110.71 -63.00-180.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18185
_diffrn_reflns_theta_full        71.3856
_diffrn_reflns_theta_max         71.39
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    5.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.4700
_exptl_crystal_description       Lump
_exptl_crystal_F_000             850.6197
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, diethylether'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.9709
_refine_diff_density_min         -0.6438
_refine_diff_density_rms         0.0928
_refine_ls_d_res_high            0.8135
_refine_ls_d_res_low             16.5732
_refine_ls_goodness_of_fit_ref   1.0035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    71
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0035
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1971P)^2^+0.0724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2456
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5174
_reflns_number_total             7020
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           200317_horie_11_+85
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_original_cell_volume        1853.35(11)
_cod_database_code               1560174
_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), C00H(H00k,H00l), C00M(H00a,H00b), C00R(H00c,H00d), C00U(H00e,
 H00f), C00V(H00g,H00h), C00X(H00i,H00j), C011(H01a,H01b), C01E(H01g,H01h),
 C4(H4a,H4b), C01C(H01d,H01e)
2.b Aromatic/amide H refined with riding coordinates:
 C00I(H00m), C00J(H00o), C00N(H00N), C00P(H00P), C00S(H00t), C00Z(H00Z),
 C010(H010), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019), C01A(H01f), C01B(H01c)
2.c Idealised Me refined as rotating group:
 C00Q(H00q,H00r,H00s)
;
_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
;