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_7242455
_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             2020-11-25
_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                91.8320(10)
_cell_angle_beta                 111.4310(10)
_cell_angle_gamma                96.2430(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2452(2)
_cell_length_b                   12.3442(2)
_cell_length_c                   12.8113(2)
_cell_measurement_reflns_used    29080
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.0580
_cell_measurement_theta_min      3.6060
_cell_volume                     1640.65(5)
_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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.964
_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   -106.00   0.00   0.50    0.50    --  -18.00  54.00 173.51  212
  2  \w     11.00  71.00   0.50    0.50    --  -18.00  54.00 173.51  120
  3  \w     16.00  55.00   0.50    0.50    --  -34.00  54.00 -62.82   78
  4  \w    -90.00 -52.00   0.50    0.50    --  -42.00  54.00  61.65   76
  5  \w     18.00  44.00   0.50    0.50    --  -42.00  54.00  61.65   52
  6  \w    -71.00 -12.00   0.50    0.50    --  -42.00  55.00 113.27  118
  7  \w   -126.00 -77.00   0.50    0.50    --  -42.00  55.00 113.27   98
  8  \w      1.00  46.00   0.50    0.50    --  -42.00  55.00 113.27   90
  9  \w     19.00  45.00   0.50    0.50    --  -42.00  55.00-168.97   52
 10  \w     11.00  40.00   0.50    0.50    --  -46.00  55.00 -92.15   58
 11  \w    -57.00 -30.00   0.50    0.50    --  -46.00  55.00 -92.15   54
 12  \w    -90.00 -63.00   0.50    0.50    --  -46.00  55.00 -92.15   54
 13  \w     -1.00  29.00   0.50    0.50    --  -58.00  55.00  -7.06   60
 14  \w    -94.00 -68.00   0.50    0.50    --  -58.00  55.00  -7.06   52
 15  \w    -14.00  30.00   0.50    0.50    --  -58.00  52.00-103.43   88
 16  \w     -5.00  30.00   0.50    0.50    --  -58.00  55.00  72.15   70
 17  \w     -3.00  27.00   0.50    0.50    --  -62.00  54.00-173.21   60
 18  \w     -8.00  27.00   0.50    0.50    --  -62.00  55.00  49.22   70
 19  \w     -4.00  27.00   0.50    0.50    --  -62.00  54.00  19.35   62
 20  \w     -9.00  26.00   0.50    0.50    --  -62.00  55.00 175.69   70
 21  \w     -2.00  27.00   0.50    0.50    --  -62.00  55.00 -31.81   58
 22  \w     -9.00  22.00   0.50    0.50    --  -66.00  54.00 136.19   62
 23  \w    -38.00  18.00   0.50    0.50    --  -70.00  55.00 -53.49  112
 24  \w    -15.00  19.00   0.50    0.50    --  -70.00  55.00 -97.79   68
 25  \w     -9.00  19.00   0.50    0.50    --  -70.00  55.00 163.61   56
 26  \w    -12.00  19.00   0.50    0.50    --  -70.00  55.00 115.56   62
 27  \w    -12.00  14.00   0.50    0.50    --  -74.00  55.00   1.40   52
 28  \w    -99.00  15.00   0.50    0.50    --  -74.00  55.00-118.39  228
 29  \w    -14.00  11.00   0.50    0.50    --  -78.00  55.00 104.38   50
 30  \w    -26.00   5.00   0.50    0.50    --  -82.00  51.00 -64.52   62
 31  \w    -44.00   3.00   0.50    0.50    --  -86.00  53.00 154.54   94
 32  \w    -91.00 -65.00   0.50    0.50    --  -86.00  53.00 154.54   52
 33  \w    -24.00   1.00   0.50    0.50    --  -86.00  53.00  41.86   50
 34  \w    -24.00   2.00   0.50    0.50    --  -86.00  54.00 -10.03   52
 35  \w    -28.00   3.00   0.50    0.50    --  -86.00  54.00  82.53   62
 36  \w   -173.00 -40.00   0.50    0.50    --  -86.00  54.00  82.53  266
 37  \w   -137.00  -1.00   0.50    0.50    --  -90.00  54.00-179.33  272
 38  \w    -37.00  -1.00   0.50    0.50    --  -90.00  52.00-110.37   72
 39  \w   -144.00  -4.00   0.50    0.50    --  -90.00  55.00 133.70  280
 40  \w    -87.00  -5.00   0.50    0.50    --  -94.00  49.00-159.14  164
 41  \w    -92.00 -62.00   0.50    0.50    --  -95.40  55.00-116.86   60
 42  \w   -117.00  -8.00   0.50    0.50    --  -95.40  55.00 -14.52  218
 43  \w   -164.00-138.00   0.50    0.50    --  -95.40  55.00 -14.52   52
 44  \w   -131.00-101.00   0.50    0.50    --  -95.40  55.00-116.86   60
 45  \w    -68.00  -8.00   0.50    0.50    --  -95.40  55.00 159.09  120
 46  \w   -101.00 -73.00   0.50    0.50    --  -95.40  55.00 159.09   56
 47  \w    -98.00  -6.00   0.50    0.50    --  -95.40  53.00  19.94  184
 48  \w   -115.00 -13.00   0.50    0.50    --  -95.40  55.00 114.58  204
 49  \w   -180.00  -7.00   0.50    0.50    --  -95.40  55.00 -79.54  346
 50  \w   -165.00-134.00   0.50    0.50    --  -95.40  55.00 114.58   62
 51  \w   -179.00-138.00   0.50    0.50    --  -95.40  55.00 159.09   82
 52  \w   -183.00  -6.00   0.50    0.50    --  -95.40  55.00-134.94  354
 53  \w   -161.00  -7.00   0.50    0.50    --  -95.40  55.00 -66.26  308
 54  \w   -105.00  -6.00   0.50    0.50    --  -95.40  55.00  72.31  198
 55  \w    -31.00  -6.00   0.50    0.50    --  -95.40  53.00  35.64   50
 56  \w   -184.00-146.00   0.50    0.50    --  -95.40  55.00  72.31   76
 57  \w   -128.00 -41.00   0.50    0.50    --  -95.40  53.00  35.64  174
 58  \w   -137.00  -7.00   0.50    0.50    --  -95.40  54.00 -29.55  260
 59  \w    -59.00  -6.00   0.50    0.50    --  -95.40  55.00-116.86  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0782058000
_diffrn_orient_matrix_UB_12      -0.0641238000
_diffrn_orient_matrix_UB_13      -0.0513367000
_diffrn_orient_matrix_UB_21      0.1048803000
_diffrn_orient_matrix_UB_22      -0.0015381000
_diffrn_orient_matrix_UB_23      0.1177421000
_diffrn_orient_matrix_UB_31      -0.0700921000
_diffrn_orient_matrix_UB_32      -0.1083629000
_diffrn_orient_matrix_UB_33      0.0170393000
_diffrn_radiation_collimation    0.3
_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  0.0930
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39675
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.485
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53799
_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    1.612
_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          0.157
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.4591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5869
_reflns_number_total             6266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           173k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242455
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHNONiSCl
_shelx_estimated_absorpt_t_max   0.371
_shelx_estimated_absorpt_t_min   0.208
_reflns_odcompleteness_completeness 98.67
_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(Cl1A)=Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H11C)=Sof(H11D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O3A)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1BC,H1BD), C1(H1AA,H1AB), C3(H3AA,H3AB), C3(H3BC,H3BD), C9(H9A,H9B),
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,
 H2B), C12(H12A,H12B), C6(H6A,H6B), C2A(H2AA,H2AB), C8(H8A,H8B), C10(H10A,H10B),
  C10A(H10C,H10D), C9A(H9AA,H9AB), C11(H11A,H11B), C11(H11C,H11D), C8A(H8AA,
 H8AB), C12A(H12C,H12D), C13A(H13C,H13D), C6A(H6AA,H6AB), C14A(H14C,H14D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7A(H7AA,H7AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              30473
_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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.759