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_7242447
_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             2020-11-24
_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                92.239(2)
_cell_angle_beta                 111.956(2)
_cell_angle_gamma                96.066(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2193(3)
_cell_length_b                   12.3191(2)
_cell_length_c                   12.7473(3)
_cell_measurement_reflns_used    28482
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.9490
_cell_measurement_theta_min      2.2900
_cell_volume                     1618.98(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 n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      113
_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 0.999
_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      9.00  77.00   0.50    0.26    --    5.18  51.00 -78.00  136
  2  \w    -21.00  19.00   0.50    0.26    --    5.18 -28.00-171.52   80
  3  \w    -51.00 -25.00   0.50    0.26    --    5.18 -28.00-171.52   52
  4  \w    -64.00  18.00   0.50    0.26    --    5.18 -23.00 -77.67  164
  5  \w    -68.00  19.00   0.50    0.26    --    5.18 -28.00  13.21  174
  6  \w    -69.00  18.00   0.50    0.26    --    5.18 -19.00  60.00  174
  7  \w    -67.00  19.00   0.50    0.26    --    5.18 -51.00 135.00  172
  8  \w    -66.00  18.00   0.50    0.26    --    5.18 -19.00 150.00  168
  9  \w    -79.00   8.00   0.50    0.26    --   -5.03 -19.00 -30.00  174
 10  \w    -18.00  55.00   0.50    0.26    --   -5.03  51.00 -78.00  146
 11  \w      5.00  39.00   0.50    0.26    --    5.18 -99.00 -90.00   68
 12  \w    -18.00  28.00   0.50    0.26    --   -5.03 -99.00 120.00   92
 13  \w    -72.00 -35.00   0.50    0.26    --   -5.03 -51.00 135.00   74
;
_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      -0.0542762000
_diffrn_orient_matrix_UB_12      -0.0318274000
_diffrn_orient_matrix_UB_13      0.0042190000
_diffrn_orient_matrix_UB_21      -0.0230247000
_diffrn_orient_matrix_UB_22      -0.0172823000
_diffrn_orient_matrix_UB_23      -0.0586853000
_diffrn_orient_matrix_UB_31      0.0353571000
_diffrn_orient_matrix_UB_32      -0.0454469000
_diffrn_orient_matrix_UB_33      0.0128022000
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            37298
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.974
_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    1.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42668
_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    1.633
_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         0.839
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0848P)^2^+0.5937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5734
_reflns_number_total             6613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           113k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242447
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.453
_reflns_odcompleteness_completeness 99.88
_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              74949
_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 0.414