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_1560177
_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                95.266(2)
_cell_angle_beta                 95.190(2)
_cell_angle_gamma                104.874(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7922(2)
_cell_length_b                   11.5185(3)
_cell_length_c                   16.7041(4)
_cell_measurement_reflns_used    13299
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      75.6590
_cell_measurement_theta_min      3.9690
_cell_volume                     1800.49(8)
_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      243(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9549
_diffrn_measured_fraction_theta_max 0.9549
_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 -12.00   0.50    0.05    --  -46.57 121.00  23.00  126
  2  \w    -59.00 -29.00   0.50    0.07    -- -102.00  61.00  60.00   60
  3  \w    -68.00 -31.00   0.50    0.07    -- -102.00  61.00   0.00   74
  4  \w    -77.00 -51.00   0.50    0.07    -- -102.00 107.00 -75.48   52
  5  \w   -107.00 -68.00   0.50    0.05    --  -46.57 152.00-176.00   78
  6  \w   -124.00 -97.00   0.50    0.07    -- -102.00 152.00-176.00   54
  7  \w   -107.00 -81.00   0.50    0.07    -- -102.00 107.00 -75.48   52
  8  \w   -106.00 -65.00   0.50    0.07    -- -102.00 125.00 -30.00   82
  9  \w   -109.00 -29.00   0.50    0.07    -- -102.00 121.00  23.00  160
 10  \w    -24.00  13.00   0.50    0.05    --  -46.57  19.00 150.00   74
 11  \w    -73.00 -31.00   0.50    0.07    -- -102.00 106.00 175.88   84
 12  \w   -107.00 -77.00   0.50    0.07    -- -102.00 106.00 175.88   60
 13  \w   -150.00 -90.00   0.50    0.07    -- -102.00 -45.00 150.00  120
 14  \w   -115.00 -56.00   0.50    0.05    --  -46.57-152.00 140.00  118
 15  \w   -139.00 -63.00   0.50    0.07    -- -102.00-152.00 140.00  152
 16  \w   -158.00 -89.00   0.50    0.07    -- -102.00 -30.00   0.00  138
 17  \w   -126.00-101.00   0.50    0.07    -- -102.00-121.00 -59.00   50
 18  \w   -118.00 -85.00   0.50    0.07    -- -102.00 -94.00-120.00   66
 19  \w   -119.00 -25.00   0.50    0.05    --  -46.57 -77.00-150.00  188
 20  \w    -17.00  11.00   0.50    0.05    --  -46.57  19.00-180.00   56
 21  \w    -69.00 -44.00   0.50    0.07    -- -102.00  61.00-180.00   50
 22  \w   -118.00 -93.00   0.50    0.05    --  -46.57-125.00-120.00   50
 23  \w     -1.00  28.00   0.50    0.05    --   46.57 -19.00 -60.00   58
 24  \w     41.00  67.00   0.50    0.07    --  104.61 -61.00 -30.00   52
 25  \w     32.00 105.00   0.50    0.07    --  104.61-121.00 -59.00  146
 26  \w     32.00 105.00   0.50    0.07    --  104.61 -77.00  90.00  146
 27  \w     87.00 124.00   0.50    0.07    --  104.61-152.00 140.00   74
 28  \w     47.00  72.00   0.50    0.05    --   46.57-152.00 140.00   50
 29  \w     40.00  69.00   0.50    0.07    --  104.61 -61.00  90.00   58
 30  \w     18.00  67.00   0.50    0.05    --   46.57-121.00 -59.00   98
 31  \w     32.00 110.00   0.50    0.07    --  104.61-125.00-120.00  156
 32  \w     33.00  92.00   0.50    0.07    --  104.61 -94.00 -60.00  118
 33  \w     99.00 178.00   0.50    0.07    --  104.61  30.00-150.00  158
 34  \w    110.00 136.00   0.50    0.07    --  104.61 121.00  23.00   52
 35  \w     92.00 164.00   0.50    0.07    --  104.61  45.00 -60.00  144
 36  \w     80.00 115.00   0.50    0.07    --  104.61 152.00-176.00   70
 37  \w     60.00  88.00   0.50    0.05    --   46.57 152.00-176.00   56
 38  \w   -174.00-143.00   0.50    0.07    -- -102.00 -15.00 120.00   62
 39  \w   -175.00-129.00   0.50    0.07    -- -102.00 -94.00-120.00   92
;
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0582
_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       -20
_diffrn_reflns_number            21920
_diffrn_reflns_theta_full        76.0232
_diffrn_reflns_theta_max         76.02
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    5.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32286
_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    1.5132
_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         0.6670
_refine_diff_density_min         -1.0321
_refine_diff_density_rms         0.1143
_refine_ls_d_res_high            0.7944
_refine_ls_d_res_low             11.0528
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0484
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    71
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0484
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.1151
_refine_ls_shift/su_mean         0.0227
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1897
_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                6290
_reflns_number_total             7197
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           200317_horie_6_-30
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_database_code               1560177
_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:
 N44(H44a,H44b), C43(H43a,H43b), C14(H14a,H14b), C15(H15a,H15b), C18(H18a,
 H18b), C27(H27a,H27b), C31(H31a,H31b), C17(H17a,H17b), C28(H28a,H28b),
 C30(H30a,H30b), C10(H10a,H10b)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C37(H37), C40(H40), C34(H34), C39(H39), C36(H36), C21(H21),
 C41(H41), C49(H49), C24(H24), C35(H35), C23(H23), C47(H47), C22(H22), C46(H46),
  C50(H50), C48(H48)
2.c Idealised Me refined as rotating group:
 C45(H45a,H45b,H45c)
;
_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
;