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_7242458
_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                92.083(2)
_cell_angle_beta                 111.733(2)
_cell_angle_gamma                96.128(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2185(3)
_cell_length_b                   12.3084(3)
_cell_length_c                   12.7536(3)
_cell_measurement_reflns_used    28564
_cell_measurement_temperature    153
_cell_measurement_theta_max      30.9790
_cell_measurement_theta_min      2.2800
_cell_volume                     1621.02(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_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    -56.00  18.00   0.50    0.35    --    5.18 -31.00  -4.02  148
  2  \w     39.00  78.00   0.50    0.35    --    5.18  51.00 -81.00   78
  3  \w     -8.00  19.00   0.50    0.35    --    5.18 -28.00 -96.36   54
  4  \w    -69.00 -22.00   0.50    0.35    --    5.18 -28.00 -96.36   94
  5  \w    -63.00 -34.00   0.50    0.35    --    5.18 -27.00-127.27   58
  6  \w    -28.00  19.00   0.50    0.35    --    5.18 -28.00-177.36   94
  7  \w    -17.00  18.00   0.50    0.35    --    5.18 -27.00-127.27   70
  8  \w    -69.00 -43.00   0.50    0.35    --    5.18 -19.00 -60.00   52
  9  \w    -31.00  18.00   0.50    0.35    --    5.18 -19.00 -60.00   98
 10  \w    -61.00  18.00   0.50    0.35    --    5.18 -37.00  60.00  158
 11  \w    -67.00  19.00   0.50    0.35    --    5.18 -51.00 132.00  172
 12  \w    -64.00  18.00   0.50    0.35    --    5.18 -37.00 150.00  164
 13  \w    -17.00  29.00   0.50    0.35    --   -4.95 -99.00-180.00   92
 14  \w    -16.00  28.00   0.50    0.35    --   -4.95 -99.00 -30.00   88
 15  \w    -76.00 -31.00   0.50    0.35    --   -4.95 -51.00 132.00   90
 16  \w     40.00  67.00   0.50    0.35    --   -4.95  51.00 -81.00   54
 17  \w    -10.00  16.00   0.50    0.35    --   -4.95  51.00 -81.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_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      -0.0551059000
_diffrn_orient_matrix_UB_12      -0.0324577000
_diffrn_orient_matrix_UB_13      0.0021433000
_diffrn_orient_matrix_UB_21      -0.0212035000
_diffrn_orient_matrix_UB_22      -0.0154803000
_diffrn_orient_matrix_UB_23      -0.0588008000
_diffrn_orient_matrix_UB_31      0.0350067000
_diffrn_orient_matrix_UB_32      -0.0457038000
_diffrn_orient_matrix_UB_33      0.0121152000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.920
_diffrn_reflns_theta_min         2.073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
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    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0819P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6920
_reflns_number_total             8598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           153k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242458
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.454
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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              93233
_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 7.274
_oxdiff_exptl_absorpt_empirical_full_min 0.402