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_7242479
_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, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_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             2020-11-11
_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.	2021-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                72.091(3)
_cell_angle_beta                 79.842(3)
_cell_angle_gamma                81.154(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5475(3)
_cell_length_b                   12.6632(3)
_cell_length_c                   13.0124(4)
_cell_measurement_reflns_used    9333
_cell_measurement_temperature    333
_cell_measurement_theta_max      28.0200
_cell_measurement_theta_min      1.9690
_cell_volume                     1618.65(8)
_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      333
_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 0.857
_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    -22.00  81.00   0.50    0.73    --   21.69  70.00-138.00  206
  2  \w     49.00  92.00   0.50    0.73    --   21.69 178.00  90.00   86
  3  \w     60.00 102.00   0.50    0.73    --   21.69 178.00 120.00   84
  4  \w    -51.00  51.00   0.50    0.73    --   21.69 -70.00  89.00  204
  5  \w    -71.00  -3.00   0.50    0.73    --  -21.62 -70.00  89.00  136
  6  \w      6.00  35.00   0.50    0.73    --  -21.62 -99.00  90.00   58
  7  \w      9.00  35.00   0.50    0.73    --  -21.62 -99.00-150.00   52
  8  \w     15.00  61.00   0.50    0.73    --  -21.62  57.00 -30.00   92
  9  \w    -35.00  59.00   0.50    0.73    --  -21.62  37.00   0.00  188
 10  \w    -46.00 -10.00   0.50    0.73    --  -21.62  57.00 -30.00   72
 11  \w    -36.00  61.00   0.50    0.73    --  -21.62  70.00-138.00  194
;
_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      -0.0353241000
_diffrn_orient_matrix_UB_12      0.0004338000
_diffrn_orient_matrix_UB_13      -0.0417621000
_diffrn_orient_matrix_UB_21      -0.0503409000
_diffrn_orient_matrix_UB_22      0.0366016000
_diffrn_orient_matrix_UB_23      0.0185733000
_diffrn_orient_matrix_UB_31      0.0306400000
_diffrn_orient_matrix_UB_32      0.0465272000
_diffrn_orient_matrix_UB_33      -0.0354341000
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19117
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.906
_diffrn_reflns_theta_min         1.973
_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    1.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47995
_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    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.059
_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     372
_refine_ls_number_reflns         7320
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.1865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5151
_reflns_number_total             7320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h2.cif
_cod_data_source_block           333k
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242479
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.562
_reflns_odcompleteness_completeness 99.89
_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. Rigid body (RIGU) restrains
 C13, O6, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C14, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              54970
_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 3.207
_oxdiff_exptl_absorpt_empirical_full_min 0.589