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_1560172
_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             2020-09-21
_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                95.109(2)
_cell_angle_beta                 95.249(2)
_cell_angle_gamma                104.806(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8091(3)
_cell_length_b                   11.5747(4)
_cell_length_c                   16.7136(5)
_cell_measurement_reflns_used    13696
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      75.7460
_cell_measurement_theta_min      4.4560
_cell_volume                     1814.42(10)
_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      273(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9570
_diffrn_measured_fraction_theta_max 0.9570
_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    -82.00 -56.00   0.50    0.05    --  -46.57 152.00-176.00   52
  2  \w    -99.00 -73.00   0.50    0.10    -- -102.00  77.00-150.00   52
  3  \w   -107.00 -30.00   0.50    0.10    -- -102.00 108.00-178.12  154
  4  \w    -23.00  29.00   0.50    0.05    --  -46.57  19.00-150.00  104
  5  \w    -24.00  18.00   0.50    0.05    --  -46.57  19.00-180.00   84
  6  \w     64.00  93.00   0.50    0.05    --   46.57 152.00-176.00   58
  7  \w     60.00 163.00   0.50    0.10    --  104.61 152.00-176.00  206
  8  \w    110.00 135.00   0.50    0.10    --  104.61 121.00  23.00   50
  9  \w     92.00 168.00   0.50    0.10    --  104.61  45.00 120.00  152
 10  \w     74.00 100.00   0.50    0.10    --  104.61 -94.00 -30.00   52
 11  \w     47.00  72.00   0.50    0.10    --  104.61-121.00 -59.00   50
 12  \w     35.00  61.00   0.50    0.10    --  104.61 -61.00 -60.00   52
 13  \w     35.00  69.00   0.50    0.10    --  104.61 -61.00 -30.00   68
 14  \w     32.00 100.00   0.50    0.10    --  104.61 -94.00 -60.00  136
 15  \w     33.00  59.00   0.50    0.10    --  104.61 -61.00   0.00   52
 16  \w     32.00  68.00   0.50    0.10    --  104.61 -61.00  90.00   72
 17  \w     37.00 104.00   0.50    0.10    --  104.61 -94.00 150.00  134
 18  \w     67.00  93.00   0.50    0.10    --  104.61 -77.00 150.00   52
 19  \w     40.00  71.00   0.50    0.10    --  104.61 -61.00 150.00   62
 20  \w     32.00  57.00   0.50    0.10    --  104.61 -77.00 150.00   50
 21  \w     32.00  88.00   0.50    0.10    --  104.61-125.00  90.00  112
 22  \w    104.00 129.00   0.50    0.10    --  104.61-152.00 140.00   50
 23  \w     57.00  97.00   0.50    0.05    --   46.57-152.00 140.00   80
 24  \w     28.00  53.00   0.50    0.05    --   46.57-121.00 -59.00   50
 25  \w     -8.00  28.00   0.50    0.05    --   46.57 -19.00-150.00   72
 26  \w     95.00 121.00   0.50    0.10    --  104.61  15.00-150.00   52
 27  \w    138.00 178.00   0.50    0.10    --  104.61  15.00-150.00   80
 28  \w    -22.00  21.00   0.50    0.05    --  -46.57  19.00  90.00   86
 29  \w    -27.00  25.00   0.50    0.05    --   46.57 -19.00   0.00  104
 30  \w    -89.00 -63.00   0.50    0.05    --  -46.57-152.00 140.00   52
 31  \w    -86.00 -58.00   0.50    0.10    -- -102.00-152.00 140.00   56
 32  \w   -118.00 -82.00   0.50    0.05    --  -46.57-125.00  90.00   72
 33  \w   -100.00 -74.00   0.50    0.05    --  -46.57-125.00 -30.00   52
 34  \w   -132.00 -89.00   0.50    0.10    -- -102.00 -30.00   0.00   86
 35  \w   -150.00-125.00   0.50    0.10    -- -102.00-121.00 -59.00   50
 36  \w   -168.00 -90.00   0.50    0.10    -- -102.00 -45.00 -60.00  156
 37  \w   -159.00-134.00   0.50    0.10    -- -102.00 -30.00   0.00   50
 38  \w    -68.00 -35.00   0.50    0.10    -- -102.00  61.00  30.00   66
 39  \w    -92.00 -12.00   0.50    0.05    --  -46.57 121.00  23.00  160
 40  \w    -69.00 -44.00   0.50    0.10    -- -102.00  61.00 150.00   50
 41  \w   -105.00 -80.00   0.50    0.10    -- -102.00 121.00  23.00   50
 42  \w   -106.00 -58.00   0.50    0.10    -- -102.00 105.00 -80.91   96
 43  \w   -127.00 -80.00   0.50    0.10    -- -102.00 152.00-176.00   94
 44  \w   -173.00 -89.00   0.50    0.10    -- -102.00 -45.00-150.00  168
 45  \w   -120.00 -89.00   0.50    0.10    -- -102.00-152.00 140.00   62
;
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23738
_diffrn_reflns_theta_full        76.2193
_diffrn_reflns_theta_max         76.22
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    5.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09426
_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    1.5016
_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         0.6804
_refine_diff_density_min         -0.6006
_refine_diff_density_rms         0.0805
_refine_ls_d_res_high            0.7938
_refine_ls_d_res_low             11.1138
_refine_ls_goodness_of_fit_ref   1.0059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    71
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0059
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.0076
_refine_ls_shift/su_mean         0.0015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+0.7265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1535
_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              21
_reflns_limit_l_min              0
_reflns_number_gt                6430
_reflns_number_total             7286
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           200317_horie_7_0
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560172
_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), C00M(H00m,H00n), C00Q(H00a,H00b), C00R(H00c,H00d), C00U(H00e,
 H00f), C00W(H00g,H00h), C010(H01a,H01b), C016(H01c,H01d), C017(H01e,H01f),
 C01E(H01k,H01l), C00Z(H00i,H00j)
2.b Aromatic/amide H refined with riding coordinates:
 C00J(H00k), C00L(H00L), C00O(H00O), C00T(H00T), C00V(H00V), C00X(H00X),
 C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C018(H018),
 C019(H019), C01A(H01h), C01B(H01i), C01C(H01j), C01D(H01g)
2.c Idealised Me refined as rotating group:
 C00S(H00p,H00q,H00r)
;
_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
;