Chemical Control of Magnetic Ordering in Hybrid Fe–Cl Layered Double Perovskites
Xue, Jie; Wang, Ziyu; Comstock, Andrew; Wang, Zhiyu; Sung, Herman H. Y.; Williams, Ian D.; Sun, Dali; Liu, Junwei; Lu, Haipeng; Chemistry of Materials 34 (2022) 2813–2823; doi:10.1021/acs.chemmater.2c00163

data_4004077
_publ_section_title
;
 Chemical Control of Magnetic Ordering in Hybrid Fe--Cl Layered Double
 Perovskites
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2813
_journal_page_last               2823
_journal_paper_doi               10.1021/acs.chemmater.2c00163
_journal_volume                  34
_journal_year                    2022
_chemical_formula_moiety         'Ag Cl8 In, 2(C4 H14 N2)'
_chemical_formula_sum            'C8 H28 Ag Cl8 In N4'
_chemical_formula_weight         686.63
_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             2021-09-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_cell_angle_alpha                102.735(7)
_cell_angle_beta                 91.155(6)
_cell_angle_gamma                90.898(6)
_cell_formula_units_Z            1
_cell_length_a                   7.7161(5)
_cell_length_b                   7.8117(7)
_cell_length_c                   9.3428(7)
_cell_measurement_reflns_used    2396
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1980
_cell_measurement_theta_min      4.8290
_cell_volume                     549.06(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.956
_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     82.00 108.00   1.00   16.00    --  113.00-111.00   0.00   26
  2  \w    -73.00  35.00   1.00    8.00    --  -40.20  77.00 120.00  108
  3  \w    -62.00  34.00   1.00    8.00    --  -40.20  57.00   0.00   96
  4  \w     52.00  87.00   1.00    8.00    --   40.20-125.00   0.00   35
  5  \w     13.00 111.00   1.00    8.00    --   40.20  57.00-120.00   98
  6  \w     50.00 138.00   1.00   16.00    --  113.00 -61.00 -30.00   88
  7  \w     43.00  78.00   1.00   16.00    --  113.00-111.00   0.00   35
  8  \w    105.00 177.00   1.00   16.00    --  113.00  77.00 -30.00   72
  9  \w    111.00 161.00   1.00   16.00    --  113.00  77.00-180.00   50
 10  \w    104.00 178.00   1.00   16.00    --  113.00  77.00  60.00   74
 11  \w     35.00 108.00   1.00   16.00    --  113.00-111.00 -90.00   73
 12  \w     35.00 107.00   1.00   16.00    --  113.00-111.00-180.00   72
 13  \w     87.00 178.00   1.00   16.00    --  113.00  61.00 120.00   91
 14  \w    105.00 145.00   1.00   16.00    --  113.00  77.00  30.00   40
 15  \w    148.00 174.00   1.00   16.00    --  113.00  77.00  30.00   26
 16  \w     79.00 112.00   1.00   16.00    --  113.00-126.00 119.00   33
;
_diffrn_measurement_device       'kappa 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      -0.0702436000
_diffrn_orient_matrix_UB_12      0.0490213000
_diffrn_orient_matrix_UB_13      0.1566353000
_diffrn_orient_matrix_UB_21      -0.1867098000
_diffrn_orient_matrix_UB_22      -0.0332652000
_diffrn_orient_matrix_UB_23      -0.0626955000
_diffrn_orient_matrix_UB_31      0.0100124000
_diffrn_orient_matrix_UB_32      -0.1933667000
_diffrn_orient_matrix_UB_33      0.0114192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3286
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.182
_diffrn_reflns_theta_min         4.854
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    24.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0710P)^2^+0.9200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2083
_reflns_number_total             2200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm2c00163_si_003.cif
_cod_data_source_block           xuejie25cu_173k_auto
_cod_database_code               4004077
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'In Fe Cl4 C4N2H14'
_shelx_estimated_absorpt_t_max   0.527
_shelx_estimated_absorpt_t_min   0.441
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C1(H1D,H1E), C2(H2D,H2E)
2.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              83625
_shelx_hkl_checksum              1563
_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 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.799