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_7242450
_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, 1(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             2020-11-24
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.2410(10)
_cell_angle_beta                 110.8230(10)
_cell_angle_gamma                96.4520(10)
_cell_formula_units_Z            2
_cell_length_a                   11.27140(10)
_cell_length_b                   12.34060(10)
_cell_length_c                   12.84520(10)
_cell_measurement_reflns_used    27269
_cell_measurement_temperature    233
_cell_measurement_theta_max      72.6800
_cell_measurement_theta_min      3.7000
_cell_volume                     1655.78(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 (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      233
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.960
_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   -104.00 -41.00   0.50    0.50    --  -16.00  54.00  46.88  126
  2  \w      5.00  71.00   0.50    0.50    --  -16.00  54.00  46.88  132
  3  \w     16.00  49.00   0.50    0.50    --  -40.00  55.00 -70.41   66
  4  \w    -79.00 -53.00   0.50    0.50    --  -40.00  55.00 -70.41   52
  5  \w    -62.00 -37.00   0.50    0.50    --  -44.00  55.00-173.06   50
  6  \w   -132.00-107.00   0.50    0.50    --  -44.00  55.00-173.06   50
  7  \w    -11.00  45.00   0.50    0.50    --  -44.00  55.00-173.06  112
  8  \w     15.00  41.00   0.50    0.50    --  -48.00  55.00 -84.90   52
  9  \w      5.00  37.00   0.50    0.50    --  -52.00  55.00  54.78   64
 10  \w    -57.00 -25.00   0.50    0.50    --  -56.00  55.00 111.80   64
 11  \w     -3.00  32.00   0.50    0.50    --  -56.00  55.00 111.80   70
 12  \w      3.00  29.00   0.50    0.50    --  -60.00  55.00-108.67   52
 13  \w     -4.00  28.00   0.50    0.50    --  -60.00  55.00  44.85   64
 14  \w      4.00  29.00   0.50    0.50    --  -60.00  55.00 155.44   50
 15  \w    -78.00 -26.00   0.50    0.50    --  -60.00  55.00   9.77  104
 16  \w      4.00  29.00   0.50    0.50    --  -60.00  55.00   9.77   50
 17  \w   -122.00  -6.00   0.50    0.50    --  -60.00  55.00-108.67  232
 18  \w    -10.00  28.00   0.50    0.50    --  -60.00  55.00  -1.93   76
 19  \w      0.00  25.00   0.50    0.50    --  -64.00  55.00-143.92   50
 20  \w     -6.00  20.00   0.50    0.50    --  -68.00  53.00 -64.05   52
 21  \w     -4.00  21.00   0.50    0.50    --  -68.00  55.00  14.55   50
 22  \w     -5.00  21.00   0.50    0.50    --  -68.00  55.00 -23.49   52
 23  \w     -4.00  21.00   0.50    0.50    --  -68.00  55.00 141.58   50
 24  \w    -12.00  17.00   0.50    0.50    --  -72.00  55.00 -34.87   58
 25  \w    -13.00  16.00   0.50    0.50    --  -72.00  55.00 -86.14   58
 26  \w    -18.00  13.00   0.50    0.50    --  -76.00  55.00-142.61   62
 27  \w    -82.00   9.00   0.50    0.50    --  -80.00  55.00 133.67  182
 28  \w    -18.00   8.00   0.50    0.50    --  -80.00  54.00  87.07   52
 29  \w    -31.00   5.00   0.50    0.50    --  -84.00  55.00 -93.15   72
 30  \w   -109.00 -37.00   0.50    0.50    --  -84.00  55.00 -93.15  144
 31  \w    -39.00   4.00   0.50    0.50    --  -84.00  54.00-116.85   86
 32  \w   -142.00-117.00   0.50    0.50    --  -84.00  55.00 -93.15   50
 33  \w    -68.00 -42.00   0.50    0.50    --  -84.00  54.00-116.85   52
 34  \w   -173.00   4.00   0.50    0.50    --  -84.00  55.00  68.10  354
 35  \w    -33.00   5.00   0.50    0.50    --  -84.00  55.00 164.80   76
 36  \w   -129.00 -42.00   0.50    0.50    --  -84.00  55.00 164.80  174
 37  \w    -27.00   5.00   0.50    0.50    --  -84.00  55.00 109.95   64
 38  \w    -22.00   4.00   0.50    0.50    --  -84.00  54.00  20.74   52
 39  \w   -116.00 -42.00   0.50    0.50    --  -84.00  55.00 109.95  148
 40  \w    -24.00   1.00   0.50    0.50    --  -88.00  55.00 -39.08   50
 41  \w   -163.00 -39.00   0.50    0.50    --  -88.00  55.00 -39.08  248
 42  \w   -102.00  -3.00   0.50    0.50    --  -92.00  55.00  -2.09  198
 43  \w   -161.00-135.00   0.50    0.50    --  -92.00  55.00  -2.09   52
 44  \w   -121.00  -3.00   0.50    0.50    --  -92.00  53.00-160.89  236
 45  \w   -133.00  -4.00   0.50    0.50    --  -93.60  55.00-139.64  258
 46  \w   -174.00-137.00   0.50    0.50    --  -93.60  55.00-139.64   74
 47  \w   -106.00  -4.00   0.50    0.50    --  -93.60  55.00  55.22  204
 48  \w   -109.00  -6.00   0.50    0.50    --  -93.60  54.00 -51.52  206
 49  \w   -163.00  -4.00   0.50    0.50    --  -93.60  55.00  98.23  318
 50  \w   -174.00-149.00   0.50    0.50    --  -93.60  55.00  55.22   50
 51  \w   -180.00 -17.00   0.50    0.50    --  -93.60  55.00 146.72  326
 52  \w    -29.00  -4.00   0.50    0.50    --  -93.60  55.00 -78.80   50
 53  \w   -173.00 -42.00   0.50    0.50    --  -93.60  55.00 -78.80  262
 54  \w   -133.00  -4.00   0.50    0.50    --  -93.60  54.00  11.79  258
;
_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      0.0759469000
_diffrn_orient_matrix_UB_12      -0.0638953000
_diffrn_orient_matrix_UB_13      -0.0535028000
_diffrn_orient_matrix_UB_21      0.1097172000
_diffrn_orient_matrix_UB_22      0.0039705000
_diffrn_orient_matrix_UB_23      0.1140560000
_diffrn_orient_matrix_UB_31      -0.0627418000
_diffrn_orient_matrix_UB_32      -0.1084195000
_diffrn_orient_matrix_UB_33      0.0258029000
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.960
_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            41408
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.085
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54371
_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    1.597
_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         -0.534
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0516P)^2^+0.3362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5843
_reflns_number_total             6351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           233k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242450
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H31NO6NiS10Cl
_chemical_oxdiff_usercomment     '233K friedel mates as non-equivalent'
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.210
_diffrn_oxdiff_digest_frames
;
010341f349be7fad7c79cb0d6852f66c1d000276335
;
_diffrn_oxdiff_digest_hkl
;
015bc4d3fe33dbbd68afa1e0601d3def6f89e1
;
_reflns_odcompleteness_completeness 98.94
_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
 At 1.5 times of:
  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              14176
_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 1.675
_oxdiff_exptl_absorpt_empirical_full_min 0.778