Molecular motion of halogenated ethylammonium/[18]crown-6 supramolecular ions in nickel dithiolate magnetic crystals
Hasuo, Naohiro; Takahashi, Kiyonori; Hisaki, Ichiro; Kokado, Kenta; Nakamura, Takayoshi; CrystEngComm 23 (2021) 2756–2763; doi:10.1039/D1CE00253H

data_7242461
_publ_section_title
;
 Molecular motion of halogenated ethylammonium/[18]crown-6 supramolecular
 ions in nickel dithiolate magnetic crystals
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2756
_journal_page_last               2763
_journal_paper_doi               10.1039/D1CE00253H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.1450(10)
_cell_angle_beta                 110.6780(10)
_cell_angle_gamma                96.4220(10)
_cell_formula_units_Z            2
_cell_length_a                   11.27840(10)
_cell_length_b                   12.34600(10)
_cell_length_c                   12.86190(10)
_cell_measurement_reflns_used    27000
_cell_measurement_temperature    253
_cell_measurement_theta_max      72.0620
_cell_measurement_theta_min      3.5940
_cell_volume                     1661.63(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      253
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.968
_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     16.00  94.00   0.50    0.50    --    5.00  46.00-150.00  156
  2  \w    -83.00  12.00   0.50    0.50    --    5.00  46.00-150.00  190
  3  \w      3.00  50.00   0.50    0.50    --  -38.00  55.00  55.27   94
  4  \w    -54.00 -28.00   0.50    0.50    --  -38.00  55.00  55.27   52
  5  \w   -101.00 -24.00   0.50    0.50    --  -42.00  53.00 -87.93  154
  6  \w   -128.00 -63.00   0.50    0.50    --  -42.00  55.00-162.12  130
  7  \w     -5.00  46.00   0.50    0.50    --  -42.00  55.00-162.12  102
  8  \w     17.00  46.00   0.50    0.50    --  -42.00  53.00 -87.93   58
  9  \w    -75.00 -38.00   0.50    0.50    --  -50.00  54.00 146.87   74
 10  \w      3.00  38.00   0.50    0.50    --  -50.00  54.00 146.87   70
 11  \w     -4.00  38.00   0.50    0.50    --  -50.00  55.00  32.87   84
 12  \w      2.00  31.00   0.50    0.50    --  -58.00  55.00 -86.41   58
 13  \w     -2.00  31.00   0.50    0.50    --  -58.00  55.00 -12.31   66
 14  \w    -14.00  31.00   0.50    0.50    --  -58.00  55.00-125.47   90
 15  \w      5.00  31.00   0.50    0.50    --  -58.00  55.00 108.94   52
 16  \w      1.00  27.00   0.50    0.50    --  -62.00  54.00-151.82   52
 17  \w      2.00  27.00   0.50    0.50    --  -62.00  55.00  24.85   50
 18  \w    -16.00  23.00   0.50    0.50    --  -66.00  55.00  50.44   78
 19  \w     -4.00  22.00   0.50    0.50    --  -66.00  55.00 170.19   52
 20  \w     -2.00  23.00   0.50    0.50    --  -66.00  55.00  98.10   50
 21  \w    -10.00  23.00   0.50    0.50    --  -66.00  55.00 -23.04   66
 22  \w     -9.00  17.00   0.50    0.50    --  -70.00  55.00  68.85   52
 23  \w     -6.00  19.00   0.50    0.50    --  -70.00  55.00 -44.51   50
 24  \w    -14.00  17.00   0.50    0.50    --  -70.00  55.00-151.04   62
 25  \w    -24.00  19.00   0.50    0.50    --  -70.00  53.00 149.79   86
 26  \w    -13.00  13.00   0.50    0.50    --  -74.00  53.00 -61.99   52
 27  \w    -24.00  11.00   0.50    0.50    --  -78.00  55.00-166.49   70
 28  \w    -15.00  11.00   0.50    0.50    --  -78.00  53.00-123.26   52
 29  \w    -15.00  11.00   0.50    0.50    --  -78.00  52.00 -78.58   52
 30  \w    -23.00  11.00   0.50    0.50    --  -78.00  55.00  13.36   68
 31  \w    -78.00 -33.00   0.50    0.50    --  -86.00  55.00 116.24   90
 32  \w   -135.00   3.00   0.50    0.50    --  -86.00  53.00 151.54  276
 33  \w   -147.00-116.00   0.50    0.50    --  -86.00  55.00 116.24   62
 34  \w    -25.00   3.00   0.50    0.50    --  -86.00  54.00 -88.05   56
 35  \w    -22.00   3.00   0.50    0.50    --  -86.00  55.00 116.24   50
 36  \w    -24.00   1.00   0.50    0.50    --  -86.00  53.00 130.23   50
 37  \w    -51.00  -3.00   0.50    0.50    --  -90.00  54.00  81.26   96
 38  \w   -126.00  -6.00   0.50    0.50    --  -90.00  53.00 -42.65  240
 39  \w    -43.00  -2.00   0.50    0.50    --  -90.00  55.00 174.96   82
 40  \w   -162.00-136.00   0.50    0.50    --  -90.00  55.00 174.96   52
 41  \w    -32.00  -3.00   0.50    0.50    --  -90.00  51.00-131.58   58
 42  \w    -40.00  -8.00   0.50    0.50    --  -94.00  53.00 123.38   64
 43  \w   -137.00 -69.00   0.50    0.50    --  -94.00  53.00 123.38  136
 44  \w    -36.00 -11.00   0.50    0.50    --  -95.40  55.00 -96.49   50
 45  \w   -126.00 -48.00   0.50    0.50    --  -95.40  55.00 -96.49  156
 46  \w   -182.00  -7.00   0.50    0.50    --  -95.40  55.00 -58.37  350
 47  \w   -175.00-149.00   0.50    0.50    --  -95.40  55.00 -96.49   52
 48  \w   -134.00 -37.00   0.50    0.50    --  -95.40  53.00 163.19  194
 49  \w   -132.00  -6.00   0.50    0.50    --  -95.40  55.00  -2.05  252
 50  \w   -176.00-139.00   0.50    0.50    --  -95.40  55.00  -2.05   74
 51  \w    -42.00  -6.00   0.50    0.50    --  -95.40  53.00 -25.68   72
 52  \w   -184.00 -66.00   0.50    0.50    --  -95.40  55.00-150.52  236
 53  \w   -183.00  -7.00   0.50    0.50    --  -95.40  55.00  66.98  352
 54  \w   -160.00  -7.00   0.50    0.50    --  -95.40  55.00-109.45  306
 55  \w    -32.00  -6.00   0.50    0.50    --  -95.40  51.00  21.35   52
 56  \w   -105.00  -6.00   0.50    0.50    --  -95.40  54.00-140.30  198
 57  \w    -38.00  -6.00   0.50    0.50    --  -95.40  55.00   8.88   64
 58  \w   -119.00 -45.00   0.50    0.50    --  -95.40  55.00   8.88  148
 59  \w   -126.00  -6.00   0.50    0.50    --  -95.40  55.00 109.14  240
 60  \w   -175.00-140.00   0.50    0.50    --  -95.40  55.00 109.14   70
 61  \w   -137.00  -6.00   0.50    0.50    --  -95.40  54.00  51.05  262
 62  \w    -59.00 -10.00   0.50    0.50    --  -95.40  55.00-150.52   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0848917000
_diffrn_orient_matrix_UB_12      -0.0642460000
_diffrn_orient_matrix_UB_13      -0.0427911000
_diffrn_orient_matrix_UB_21      0.0999032000
_diffrn_orient_matrix_UB_22      0.0057883000
_diffrn_orient_matrix_UB_23      0.1188742000
_diffrn_orient_matrix_UB_31      -0.0669238000
_diffrn_orient_matrix_UB_32      -0.1080356000
_diffrn_orient_matrix_UB_33      0.0222566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41385
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.249
_diffrn_reflns_theta_min         3.610
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00309(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         6340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0421P)^2^+0.3530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5825
_reflns_number_total             6340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           253k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242461
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H31NO6NiS10Cl
_diffrn_oxdiff_digest_frames
;
01abefbb46bbf6e9ace5a09866b9b78568000277976
;
_diffrn_oxdiff_digest_hkl
;
013c9f9f66ccb089a6bf2cad9ff9bffe7760de
;
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H20c)=Sof(H20d)=Sof(C19A)=Sof(H19c)=Sof(H19d)=Sof(Cl)=1-FVAR(1)
 Sof(Cl18)=Sof(H20a)=Sof(H20b)=Sof(C19)=Sof(H19a)=Sof(H19b)=FVAR(1)
 Sof(O1A)=Sof(O23A)=Sof(C22A)=Sof(H22c)=Sof(H22d)=Sof(C27A)=Sof(H27c)=
 Sof(H27d)=Sof(C24A)=Sof(H24c)=Sof(H24d)=Sof(C26A)=Sof(H26c)=Sof(H26d)=Sof(C8A)=
 Sof(H8Aa)=Sof(H8Ab)=Sof(O6A)=Sof(C32A)=Sof(H32c)=Sof(H32d)=Sof(C40A)=Sof(H40c)=
 Sof(H40d)=Sof(O28A)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C31A)=Sof(H31c)=Sof(H31d)=
 Sof(O2A)=Sof(C30A)=Sof(H30c)=Sof(H30d)=Sof(C37A)=Sof(H37c)=Sof(H37d)=Sof(O3A)=
 Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=1-FVAR(2)
 Sof(O23)=Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(C32)=Sof(H32a)=Sof(H32b)=Sof(C22)=
 Sof(H22a)=Sof(H22b)=Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(O28)=Sof(C27)=Sof(H27a)=
 Sof(H27b)=Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(C31)=
 Sof(H31a)=Sof(H31b)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(O6)=Sof(C8)=Sof(H8a)=Sof(H8b)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C1)=Sof(H1a)=
 Sof(H1b)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C20(H20c,H20d), C30(H30a,H30b), C32(H32a,H32b), C22(H22a,
 H22b), C37(H37a,H37b), C19(H19a,H19b), C27(H27a,H27b), C40(H40a,H40b),
 C24(H24a,H24b), C31(H31a,H31b), C26(H26a,H26b), C19A(H19c,H19d), C8(H8a,H8b),
 C4(H4a,H4b), C1(H1a,H1b), C22A(H22c,H22d), C27A(H27c,H27d), C24A(H24c,H24d),
 C26A(H26c,H26d), C8A(H8Aa,H8Ab), C32A(H32c,H32d), C40A(H40c,H40d), C4A(H4Aa,
 H4Ab), C31A(H31c,H31d), C30A(H30c,H30d), C37A(H37c,H37d), C1A(H1Aa,H1Ab)
3.b Idealised Me refined as rotating group:
 N21(H21a,H21b,H21c)
;
_shelx_res_checksum              44764
_olex2_exptl_crystal_mounting_method loop
_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 1.736
_oxdiff_exptl_absorpt_empirical_full_min 0.750