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_7242472
_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
_audit_creation_date             2020-11-25
_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.	2021-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                70.113(3)
_cell_angle_beta                 79.966(2)
_cell_angle_gamma                80.068(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3884(3)
_cell_length_b                   12.6271(4)
_cell_length_c                   12.9344(4)
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.5280
_cell_measurement_theta_min      2.4400
_cell_volume                     1559.30(9)
_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 2018/2 (Sheldrick, 2018)'
_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 0.777
_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    -17.00  27.00   0.50    0.16    --   -5.03 -99.00  90.00   88
  2  \w    -67.00  14.00   0.50    0.16    --    5.18 -37.00  90.00  162
  3  \w    -76.00   9.00   0.50    0.16    --   -5.03 -57.00-180.00  170
  4  \w    -18.00   9.00   0.50    0.16    --   -5.03 -99.00-180.00   54
  5  \w    -78.00  -1.00   0.50    0.16    --   -5.03 -37.00 -60.00  154
  6  \w     40.00  81.00   0.50    0.16    --    5.18  19.00 -90.00   82
;
_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      -0.0014574000
_diffrn_orient_matrix_UB_12      0.0559315000
_diffrn_orient_matrix_UB_13      0.0012232000
_diffrn_orient_matrix_UB_21      -0.0114746000
_diffrn_orient_matrix_UB_22      -0.0200396000
_diffrn_orient_matrix_UB_23      0.0587146000
_diffrn_orient_matrix_UB_31      0.0688986000
_diffrn_orient_matrix_UB_32      -0.0096162000
_diffrn_orient_matrix_UB_33      0.0023694000
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.777
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19502
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.958
_diffrn_reflns_theta_min         2.455
_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    1.335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55431
_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    1.661
_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         0.586
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7689
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6046
_reflns_number_total             7689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00253h2.cif
_cod_data_source_block           133k
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242472
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.551
_reflns_odcompleteness_completeness 99.92
_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
 C2A-F1A \\sim F1A-C2
 with sigma of 0.02
 C2-C1 \\sim C1-C2A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C2A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
5.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)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              86892
_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 3.105
_oxdiff_exptl_absorpt_empirical_full_min 0.357