Synthesis, structural analysis, electrochemical and magnetic properties of tetrachloroferrate ionic liquids
Zafar, Anham; Imtiaz-ud-Din.,; Ahmed, Safeer; Bučar, Dejan-Krešimir; Tahir, Muhammad Nawaz; Palgrave, Robert G.; New Journal of Chemistry 45 (2021) 13429–13440; doi:10.1039/D1NJ01400E

data_7060759
_publ_section_title
;
 Synthesis, structural analysis, electrochemical and magnetic properties
 of tetrachloroferrate ionic liquids
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13429
_journal_page_last               13440
_journal_paper_doi               10.1039/D1NJ01400E
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C21 H19 N2, Cl4 Fe'
_chemical_formula_sum            'C21 H19 Cl4 Fe N2'
_chemical_formula_weight         497.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-23 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.80890(10)
_cell_length_b                   14.1846(2)
_cell_length_c                   13.2623(2)
_cell_measurement_reflns_used    19411
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      72.2420
_cell_measurement_theta_min      4.5330
_cell_volume                     2208.28(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -4.00  21.00   1.00    2.80    --   34.00  92.00  54.48   25
  2  \w      9.00  39.00   1.00    2.80    --   42.00  78.00 169.25   30
  3  \w      8.00  33.00   1.00    2.80    --   42.00  82.00-104.77   25
  4  \w   -111.00 -28.00   1.00    2.80    --  -42.62 -38.00-120.00   83
  5  \w   -117.00 -18.00   1.00    2.80    --  -42.62 -38.00  90.00   99
  6  \w   -113.00 -20.00   1.00    2.80    --  -42.62 -38.00 -30.00   93
  7  \w    -66.00  24.00   1.00    2.80    --  -42.62  38.00  60.00   90
  8  \w     28.00  99.00   1.00    2.80    --   42.62-125.00-180.00   71
  9  \w     30.00  73.00   1.00    2.80    --   42.62 -77.00   0.00   43
 10  \w     13.00  39.00   1.00    2.80    --   46.00  79.00 -58.56   26
 11  \w     13.00  38.00   1.00    2.80    --   46.00  79.00  77.10   25
 12  \w     22.00  49.00   1.00    2.80    --   54.00  74.00  14.94   27
 13  \w    103.00 136.00   1.00    2.80    --   62.00  74.00 -43.33   33
 14  \w     31.00  56.00   1.00    2.80    --   62.00  73.00-147.08   25
 15  \w     31.00  56.00   1.00    2.80    --   62.00  73.00 104.01   25
 16  \w     31.00  58.00   1.00    2.80    --   62.00  74.00 -43.33   27
 17  \w     31.00  56.00   1.00    2.80    --   62.00  74.00 134.82   25
 18  \w    113.00 139.00   1.00    2.80    --   66.00  69.00-102.08   26
 19  \w     35.00  61.00   1.00    2.80    --   66.00  73.00  61.63   26
 20  \w     35.00  62.00   1.00    2.80    --   66.00  69.00-102.08   27
 21  \w     38.00  65.00   1.00    2.80    --   66.00  73.00 173.15   27
 22  \w    110.00 140.00   1.00    2.80    --   66.00  74.00 -19.07   30
 23  \w    113.00 141.00   1.00    2.80    --   66.00  73.00  61.63   28
 24  \w     35.00  62.00   1.00    2.80    --   66.00  74.00 -19.07   27
 25  \w     44.00  71.00   1.00   11.20    --   74.00  70.00 126.75   27
 26  \w     46.00  74.00   1.00   11.20    --   74.00  61.00 -38.60   28
 27  \w    113.00 146.00   1.00   11.20    --   78.00  72.00   9.55   33
 28  \w     47.00  76.00   1.00   11.20    --   78.00  72.00   9.55   29
 29  \w     49.00  75.00   1.00   11.20    --   78.00  63.00 103.62   26
 30  \w     49.00  76.00   1.00   11.20    --   78.00  63.00 160.51   27
 31  \w     47.00  84.00   1.00   11.20    --   78.00  69.00-140.15   37
 32  \w     51.00  83.00   1.00   11.20    --   82.00  72.00 -95.13   32
 33  \w    133.00 159.00   1.00   11.20    --   86.00  64.00  50.21   26
 34  \w     56.00  82.00   1.00   11.20    --   86.00  64.00  50.21   26
 35  \w     60.00  86.00   1.00   11.20    --   90.00  67.00 107.28   26
 36  \w     63.00  90.00   1.00   11.20    --   90.00  66.00 174.41   27
 37  \w    131.00 169.00   1.00   11.20    --   94.00  73.00  43.93   38
 38  \w     65.00  92.00   1.00   11.20    --   94.00  69.00 -38.31   27
 39  \w     62.00 100.00   1.00   11.20    --   94.00  73.00  43.93   38
 40  \w     23.00 104.00   1.00   11.20    --  104.49 -94.00-180.00   81
 41  \w     82.00 176.00   1.00   11.20    --  104.49  61.00 -30.00   94
 42  \w     34.00 106.00   1.00   11.20    --  104.49 -94.00 -60.00   72
 43  \w     77.00 166.00   1.00   11.20    --  104.49  61.00-150.00   89
 44  \w     74.00 172.00   1.00   11.20    --  104.49  66.00  16.49   98
 45  \w     52.00 116.00   1.00   11.20    --  104.49 -61.00  30.00   64
 46  \w     76.00 152.00   1.00   11.20    --  104.49  61.00 150.00   76
 47  \w    117.00 177.00   1.00   11.20    --  104.49  61.00 -90.00   60
 48  \w     75.00 110.00   1.00   11.20    --  104.49  61.00 -90.00   35
 49  \w    127.00 170.00   1.00   11.20    --  104.49  61.00-120.00   43
 50  \w     75.00 101.00   1.00   11.20    --  104.49  61.00-120.00   26
 51  \w     75.00 101.00   1.00   11.20    --  104.49  61.00   0.00   26
 52  \w    118.00 164.00   1.00   11.20    --  104.49 125.00 120.00   46
 53  \w    125.00 151.00   1.00   11.20    --  104.49  61.00 -60.00   26
 54  \w     75.00 102.00   1.00   11.20    --  104.49  61.00 -60.00   27
 55  \w     82.00 144.00   1.00   11.20    --  104.49  45.00  90.00   62
 56  \w     76.00 155.00   1.00   11.20    --  104.49  61.00-180.00   79
 57  \w    144.00 170.00   1.00   11.20    --  104.49  61.00 120.00   26
 58  \w     75.00 103.00   1.00   11.20    --  104.49  61.00 120.00   28
 59  \w     30.00 103.00   1.00   11.20    --  104.49 -94.00-120.00   73
 60  \w     35.00 109.00   1.00   11.20    --  104.49-114.00  78.00   74
 61  \w     86.00 111.00   1.00   11.20    --  104.49-125.00-180.00   25
 62  \w    113.00 175.00   1.00   11.20    --  104.49  77.00  90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0930482000
_diffrn_orient_matrix_UB_12      -0.0600481000
_diffrn_orient_matrix_UB_13      0.0599382000
_diffrn_orient_matrix_UB_21      0.0455893000
_diffrn_orient_matrix_UB_22      0.0884596000
_diffrn_orient_matrix_UB_23      0.0584709000
_diffrn_orient_matrix_UB_31      -0.0805949000
_diffrn_orient_matrix_UB_32      -0.0192809000
_diffrn_orient_matrix_UB_33      0.0814328000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36222
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.563
_diffrn_reflns_theta_max         66.563
_diffrn_reflns_theta_min         4.579
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.000
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       prism
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0301P)^2^+0.8713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3673
_reflns_number_total             3889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01400e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060759--7060760.cif.'
_cod_database_code               7060759
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.645
_shelx_estimated_absorpt_t_min   0.269
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C21(H21), C10(H10), C17(H17), C13(H13), C20(H20), C19(H19), C18(H18),
 C12(H12), C7(H7), C3(H3), C11(H11), C4(H4), C5(H5), C6(H6)
;
_shelx_res_checksum              15892
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.808