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_7242457
_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             2020-11-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.103(2)
_cell_angle_beta                 110.634(2)
_cell_angle_gamma                96.375(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2803(3)
_cell_length_b                   12.3375(2)
_cell_length_c                   12.8611(3)
_cell_measurement_reflns_used    26461
_cell_measurement_temperature    273
_cell_measurement_theta_max      30.8120
_cell_measurement_theta_min      2.1050
_cell_volume                     1661.43(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-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.830
_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     39.00  78.00   0.50    0.17    --    5.18  28.00-126.00   78
  2  \w    -28.00  19.00   0.50    0.17    --    5.18 -28.00-145.15   94
  3  \w    -69.00 -40.00   0.50    0.17    --    5.18 -28.00-145.15   58
  4  \w    -68.00  19.00   0.50    0.17    --    5.18 -28.00 -97.58  174
  5  \w    -66.00  19.00   0.50    0.17    --    5.18 -28.00 -48.73  170
  6  \w    -69.00  19.00   0.50    0.17    --    5.18 -28.00  -2.06  176
  7  \w    -68.00  19.00   0.50    0.17    --    5.18 -28.00  71.00  174
  8  \w    -70.00  18.00   0.50    0.17    --    5.18 -25.00 132.92  176
  9  \w    -78.00 -40.00   0.50    0.17    --   -5.03 -28.00  71.00   76
 10  \w    -39.00   5.00   0.50    0.17    --   -5.03 -37.00-150.00   88
 11  \w    -75.00 -42.00   0.50    0.17    --   -5.03 -37.00-150.00   66
 12  \w    -11.00  28.00   0.50    0.17    --   -5.03 -99.00 -60.00   78
 13  \w    -18.00  27.00   0.50    0.17    --   -5.03 -99.00-180.00   90
 14  \w      3.00  39.00   0.50    0.17    --    5.18 -99.00-150.00   72
 15  \w     -2.00  24.00   0.50    0.17    --   -5.03  28.00-126.00   52
 16  \w     39.00  65.00   0.50    0.17    --   -5.03  28.00-126.00   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      -0.0017497000
_diffrn_orient_matrix_UB_12      -0.0190071000
_diffrn_orient_matrix_UB_13      -0.0529859000
_diffrn_orient_matrix_UB_21      0.0675837000
_diffrn_orient_matrix_UB_22      0.0100648000
_diffrn_orient_matrix_UB_23      0.0186456000
_diffrn_orient_matrix_UB_31      0.0040710000
_diffrn_orient_matrix_UB_32      -0.0538257000
_diffrn_orient_matrix_UB_33      0.0182058000
_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  0.0481
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.071
_diffrn_reflns_theta_min         2.074
_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    1.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64798
_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    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8848
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0389
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             8848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           93k-f-2
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242457
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNONiSBr
_reflns_odcompleteness_completeness 99.97
_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. Restrained distances
 O4-C12 \\sim O4A-C11
 with sigma of 0.04
 C7-C6 \\sim C6A-C5A
 with sigma of 0.04
 O3-C9 \\sim O3A-C8A
 with sigma of 0.02
 O1-C6 \\sim O1A-C5A
 with sigma of 0.04
 O5-C14 \\sim O5A-C13A
 with sigma of 0.04
 O6-C14 \\sim O6A-C13A
 with sigma of 0.02
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 C13-C12 \\sim C12A-C11
 with sigma of 0.04
 O6-C13 \\sim O6A-C12A
 with sigma of 0.04
 O5-C13 \\sim O5A-C12A
 with sigma of 0.02
 C5-C7 \\sim C4A-C6A
 with sigma of 0.04
 O5-C12 \\sim O5A-C11
 with sigma of 0.02
 O4-C9 \\sim O4A-C8A
 with sigma of 0.04
 O2-C5 \\sim O2A-C4A
 with sigma of 0.02
 O1-C5 \\sim O1A-C4A
 with sigma of 0.04
 O2-C6 \\sim O2A-C5A
 with sigma of 0.04
 O3-C10 \\sim O3A-C9A
 with sigma of 0.04
 C9-C10 \\sim C8A-C9A
 with sigma of 0.02
 O2-C7 \\sim O2A-C6A
 with sigma of 0.02
 C5-C6 \\sim C4A-C5A
 with sigma of 0.02
 O3-C7 \\sim O3A-C6A
 with sigma of 0.04
 C13-C14 \\sim C12A-C13A
 with sigma of 0.02
 O4-C10 \\sim O4A-C9A
 with sigma of 0.02
 C3-C14 \\sim C14A-C13A
 with sigma of 0.04
 O1-C3 \\sim O1A-C14A
 with sigma of 0.04
 C3-C5 \\sim C14A-C4A
 with sigma of 0.04
 O6-C3 \\sim O6A-C14A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6A \\sim C7A \\sim O3A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Others
 Sof(H1d)=Sof(H1e)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(1)
 Sof(H00Z)=Sof(H)=Sof(C2)=Sof(H01E)=Sof(H01F)=FVAR(1)
 Sof(H3c)=Sof(H3d)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C9A)=
 Sof(H9Aa)=Sof(H9Ab)=Sof(H11a)=Sof(H11b)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(O3A)=
 Sof(C12A)=Sof(H12a)=Sof(H12b)=Sof(C13A)=Sof(H13a)=Sof(H13b)=Sof(C6A)=Sof(H6Aa)=
 Sof(H6Ab)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14a)=Sof(H14b)=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(H00A)=Sof(H00B)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H00E)=Sof(H00F)=Sof(C5)=Sof(H00G)=Sof(H00H)=Sof(C13)=Sof(H00I)=Sof(H00J)=
 Sof(C14)=Sof(H00K)=Sof(H00L)=Sof(C4)=Sof(H00M)=Sof(H00N)=Sof(C7)=Sof(H00O)=
 Sof(H00P)=Sof(C12)=Sof(H01A)=Sof(H01B)=Sof(C6)=Sof(H01C)=Sof(H01D)=Sof(C8)=
 Sof(H3A)=Sof(H3B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H0AA)=Sof(H0AB)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H00Z,H), C1(H1d,H1e), C3(H00A,H00B), C3(H3c,H3d), C9(H00E,H00F), C5(H00G,
 H00H), C13(H00I,H00J), C14(H00K,H00L), C4(H00M,H00N), C7(H00O,H00P), C2(H01E,
 H01F), C12(H01A,H01B), C6(H01C,H01D), C2A(H2Aa,H2Ab), C8(H3A,H3B), C10(H10A,
 H10B), C10A(H10c,H10d), C9A(H9Aa,H9Ab), C11(H0AA,H0AB), C11(H11a,H11b),
 C8A(H8Aa,H8Ab), C12A(H12a,H12b), C13A(H13a,H13b), C6A(H6Aa,H6Ab), C14A(H14a,
 H14b), C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,H7Ab)
5.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_shelx_res_checksum              94317
_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 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.635