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_1560175
_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         820.39
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-20
_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                95.673(2)
_cell_angle_beta                 94.963(2)
_cell_angle_gamma                104.636(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6910(3)
_cell_length_b                   11.3787(3)
_cell_length_c                   16.6251(4)
_cell_measurement_reflns_used    15007
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      76.0400
_cell_measurement_theta_min      3.9880
_cell_volume                     1753.22(9)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_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   -115.00 -89.00   0.50    0.05    --  -46.57-153.00 141.00   52
  2  \w    -84.00 -55.00   0.50    0.05    --  -46.57-153.00 141.00   58
  3  \w   -133.00-108.00   0.50    0.05    -- -102.00-153.00 141.00   50
  4  \w   -173.00 -90.00   0.50    0.05    -- -102.00 -45.00 150.00  166
  5  \w    -22.00  12.00   0.50    0.05    --  -46.57  19.00 150.00   68
  6  \w    -23.00  28.00   0.50    0.05    --  -46.57  19.00  90.00  102
  7  \w    -60.00 -33.00   0.50    0.05    -- -102.00 121.00  23.00   54
  8  \w    -75.00 -30.00   0.50    0.05    -- -102.00 125.00  60.00   90
  9  \w    -71.00 -45.00   0.50    0.05    --  -46.57 121.00  23.00   52
 10  \w    -68.00 -36.00   0.50    0.05    -- -102.00  61.00  30.00   64
 11  \w    -64.00 -30.00   0.50    0.05    -- -102.00  61.00  60.00   68
 12  \w    -72.00 -32.00   0.50    0.05    -- -102.00  77.00 -30.00   80
 13  \w    -83.00 -58.00   0.50    0.05    --  -46.57 153.00-177.00   50
 14  \w    -54.00 -29.00   0.50    0.05    -- -102.00 153.00-177.00   50
 15  \w   -107.00 -37.00   0.50    0.05    -- -102.00 125.00 -30.00  140
 16  \w   -107.00 -65.00   0.50    0.05    -- -102.00 121.00  23.00   84
 17  \w   -112.00 -81.00   0.50    0.05    -- -102.00 125.00  60.00   62
 18  \w   -108.00 -45.00   0.50    0.05    -- -102.00 110.00 166.13  126
 19  \w   -124.00 -91.00   0.50    0.05    -- -102.00 -30.00   0.00   66
 20  \w   -159.00-133.00   0.50    0.05    -- -102.00 -30.00   0.00   52
 21  \w   -166.00 -89.00   0.50    0.05    -- -102.00 -15.00-120.00  154
 22  \w   -119.00 -37.00   0.50    0.05    --  -46.57 -77.00-150.00  164
 23  \w    -17.00  20.00   0.50    0.05    --  -46.57  19.00-180.00   74
 24  \w     31.00  87.00   0.50    0.05    --   46.57-121.00 -59.00  112
 25  \w     73.00  99.00   0.50    0.05    --  104.61-121.00 -59.00   52
 26  \w     32.00  57.00   0.50    0.05    --  104.61 -61.00-180.00   50
 27  \w     33.00 102.00   0.50    0.05    --  104.61-125.00-150.00  138
 28  \w     37.00  62.00   0.50    0.05    --  104.61 -61.00 -60.00   50
 29  \w    144.00 171.00   0.50    0.05    --  104.61  45.00   0.00   54
 30  \w    128.00 154.00   0.50    0.05    --  104.61 121.00  23.00   52
 31  \w     89.00 114.00   0.50    0.05    --  104.61 121.00  23.00   50
 32  \w     96.00 129.00   0.50    0.05    --  104.61  45.00   0.00   66
 33  \w     92.00 164.00   0.50    0.05    --  104.61  45.00 -60.00  144
 34  \w     98.00 124.00   0.50    0.05    --  104.61 153.00-177.00   52
 35  \w     60.00  88.00   0.50    0.05    --   46.57 153.00-177.00   56
 36  \w     35.00  69.00   0.50    0.05    --  104.61 -61.00  90.00   68
 37  \w     79.00 104.00   0.50    0.05    --  104.61 -77.00  90.00   50
 38  \w     73.00 108.00   0.50    0.05    --  104.61 -77.00 150.00   70
 39  \w     81.00 106.00   0.50    0.05    --  104.61-153.00 141.00   50
 40  \w     73.00  98.00   0.50    0.05    --   46.57-153.00 141.00   50
 41  \w     39.00  72.00   0.50    0.05    --  104.61 -77.00  90.00   66
 42  \w   -116.00 -88.00   0.50    0.05    --  -46.57-125.00-180.00   56
 43  \w   -147.00 -92.00   0.50    0.05    -- -102.00 -45.00-150.00  110
 44  \w   -120.00 -95.00   0.50    0.05    -- -102.00-121.00 -59.00   50
 45  \w   -108.00 -57.00   0.50    0.05    -- -102.00 115.00 -94.58  102
 46  \w   -125.00 -60.00   0.50    0.05    -- -102.00 153.00-177.00  130
;
_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      -0.0644651000
_diffrn_orient_matrix_UB_12      -0.0483315000
_diffrn_orient_matrix_UB_13      -0.0886867000
_diffrn_orient_matrix_UB_21      -0.0934081000
_diffrn_orient_matrix_UB_22      -0.1156853000
_diffrn_orient_matrix_UB_23      0.0285566000
_diffrn_orient_matrix_UB_31      -0.1203355000
_diffrn_orient_matrix_UB_32      0.0646030000
_diffrn_orient_matrix_UB_33      0.0104203000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_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            21543
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.316
_diffrn_reflns_theta_min         4.047
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40564
_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_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, diethylether'
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.597
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1381P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6566
_reflns_number_total             7022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           200317_horie_1_-180
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_original_cell_volume        1753.22(8)
_cod_database_code               1560175
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20O8FePF6Cl
_shelx_estimated_absorpt_t_max   0.460
_shelx_estimated_absorpt_t_min   0.215
_diffrn_oxdiff_digest_frames
;
01a9357df5f57df434707e553f0940fff3000524756
;
_diffrn_oxdiff_digest_hkl
;
0100c5c0fa17579dc290ff6c0d3136f8f7f07c
;
_reflns_odcompleteness_completeness 99.92
_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), C15(H15A,H15B), C27(H27A,H27B), C14(H14A,H14B), C43(H43A,H43B),
 C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C18(H18A,H18B), C17(H17A,H17B),
  C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C42(H42), C37(H37), C48(H48), C35(H35), C21(H21), C41(H41),
 C39(H39), C23(H23), C36(H36), C24(H24), C47(H47), C40(H40), C22(H22), C46(H46),
  C49(H49), C50(H50)
2.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              82730
_shelx_hkl_checksum              15497
_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 4.988
_oxdiff_exptl_absorpt_empirical_full_min 0.496