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_7242451
_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             2020-11-10
_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                92.2792(18)
_cell_angle_beta                 112.126(2)
_cell_angle_gamma                96.0601(18)
_cell_formula_units_Z            2
_cell_length_a                   11.2107(3)
_cell_length_b                   12.3150(2)
_cell_length_c                   12.7451(3)
_cell_measurement_reflns_used    29610
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.9190
_cell_measurement_theta_min      2.1280
_cell_volume                     1614.84(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      93
_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 0.837
_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    -42.00  18.00   0.50    0.24    --    5.18 -30.00 -11.44  120
  2  \w    -67.00  18.00   0.50    0.24    --    5.18 -32.00 -57.00  170
  3  \w    -63.00  18.00   0.50    0.24    --    5.18 -29.00  28.00  162
  4  \w    -64.00  19.00   0.50    0.24    --    5.18 -33.00 132.51  166
  5  \w    -40.00  18.00   0.50    0.24    --    5.18 -31.00 173.49  116
  6  \w    -69.00  18.00   0.50    0.24    --    5.18 -19.00  60.00  174
  7  \w    -10.00  78.00   0.50    0.24    --    5.18  57.00 -30.00  176
  8  \w     43.00  80.00   0.50    0.24    --    5.18  29.00-170.00   74
  9  \w    -63.00  19.00   0.50    0.24    --    5.18 -28.00-113.26  164
 10  \w    -17.00  28.00   0.50    0.24    --   -4.95 -99.00 150.00   90
 11  \w    -80.00 -25.00   0.50    0.24    --   -4.95 -29.00  28.00  110
 12  \w     37.00  66.00   0.50    0.24    --   -4.95  29.00-170.00   58
 13  \w    -17.00  12.00   0.50    0.24    --   -4.95  29.00-170.00   58
;
_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      0.0061888000
_diffrn_orient_matrix_UB_12      -0.0073309000
_diffrn_orient_matrix_UB_13      -0.0531169000
_diffrn_orient_matrix_UB_21      0.0668493000
_diffrn_orient_matrix_UB_22      0.0208920000
_diffrn_orient_matrix_UB_23      0.0260276000
_diffrn_orient_matrix_UB_31      0.0154338000
_diffrn_orient_matrix_UB_32      -0.0537563000
_diffrn_orient_matrix_UB_33      0.0117284000
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45358
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.014
_diffrn_reflns_theta_min         1.978
_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    1.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41902
_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    1.638
_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         1.083
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0915P)^2^+0.2292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6983
_reflns_number_total             8651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           93k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_original_cell_volume        1614.83(7)
_cod_database_code               7242451
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         ClCNNiSHO
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.452
_reflns_odcompleteness_completeness 99.94
_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(H7BC)=Sof(H7BD)=Sof(O4A)=Sof(O1A)=Sof(O6A)=Sof(H9BC)=Sof(H9BD)=Sof(O2A)=
 Sof(H3BC)=Sof(H3BD)=Sof(O3A)=Sof(O5A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C7A)=
 Sof(H7AC)=Sof(H7AD)=Sof(C9A)=Sof(H9AC)=Sof(H9AD)=Sof(C12A)=Sof(H12C)=Sof(H12D)=
 Sof(C3A)=Sof(H3AC)=Sof(H3AD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(O3)=Sof(O6)=Sof(O1)=Sof(H9AA)=Sof(H9AB)=Sof(O2)=
 Sof(H3AA)=Sof(H3AB)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(O5)=
 Sof(O4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C11)=Sof(H11C)=Sof(H11D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C7(H7BC,H7BD), C7(H7AA,H7AB), C9(H9BC,H9BD), C9(H9AA,H9AB),
 C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C13(H13A,H13B), C11A(H11A,H11B),
 C5(H5A,H5B), C7A(H7AC,H7AD), C12(H12A,H12B), C10(H10A,H10B), C9A(H9AC,H9AD),
 C12A(H12C,H12D), C4(H4A,H4B), C14(H14A,H14B), C8(H8A,H8B), C6(H6A,H6B),
 C3A(H3AC,H3AD), C5A(H5AA,H5AB), C13A(H13C,H13D), C11(H11C,H11D), C6A(H6AA,
 H6AB), C14A(H14C,H14D)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              99851
_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 4.420
_oxdiff_exptl_absorpt_empirical_full_min 0.405