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_4004078
_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 Fe, 2(C4 H14 N2)'
_chemical_formula_sum            'C8 H28 Ag Cl8 Fe N4'
_chemical_formula_weight         627.66
_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             2021-10-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_cell_angle_alpha                76.162(5)
_cell_angle_beta                 89.632(5)
_cell_angle_gamma                89.618(5)
_cell_formula_units_Z            2
_cell_length_a                   7.5923(5)
_cell_length_b                   10.8224(7)
_cell_length_c                   13.3237(7)
_cell_measurement_reflns_used    3707
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.2250
_cell_measurement_theta_min      4.1920
_cell_volume                     1062.96(12)
_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)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.953
_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     37.00 137.00   1.00   12.00    --  113.00 -30.00 -60.00  100
  2  \w   -111.00 -24.00   1.00    3.00    --  -39.95 -37.00-180.00   87
  3  \w    -64.00  42.00   1.00    3.00    --  -39.95  19.00   0.00  106
  4  \w     47.00  81.00   1.00    3.00    --   39.95-125.00 -60.00   34
  5  \w     16.00  70.00   1.00    3.00    --   39.95 -99.00  30.00   54
  6  \w    -19.00  74.00   1.00    3.00    --   39.95 -77.00  90.00   93
  7  \w     45.00 141.00   1.00   12.00    --  113.00 -45.00  30.00   96
  8  \w     50.00 109.00   1.00   12.00    --  113.00-111.00  60.00   59
  9  \w     82.00 115.00   1.00   12.00    --  113.00-133.00 147.00   33
 10  \w     43.00 142.00   1.00   12.00    --  113.00 -61.00 150.00   99
 11  \w     35.00 107.00   1.00   12.00    --  113.00-111.00 -30.00   72
 12  \w    108.00 178.00   1.00   12.00    --  113.00  77.00 120.00   70
 13  \w     47.00 107.00   1.00   12.00    --  113.00 -94.00 150.00   60
 14  \w     30.00 169.00   1.00   12.00    --  113.00 -15.00 120.00  139
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081077000
_diffrn_orient_matrix_UB_12      0.0381078000
_diffrn_orient_matrix_UB_13      -0.1189819000
_diffrn_orient_matrix_UB_21      -0.1262617000
_diffrn_orient_matrix_UB_22      -0.1093221000
_diffrn_orient_matrix_UB_23      -0.0046315000
_diffrn_orient_matrix_UB_31      -0.1586430000
_diffrn_orient_matrix_UB_32      0.0899435000
_diffrn_orient_matrix_UB_33      -0.0016362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6809
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.175
_diffrn_reflns_theta_min         3.416
_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    22.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31870
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_description       block
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4299
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0625P)^2^+0.3806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3639
_reflns_number_total             4299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm2c00163_si_002.cif
_cod_data_source_block           xuejie20_173k_auto
_cod_original_cell_volume        1062.96(11)
_cod_database_code               4004078
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.404
_shelx_estimated_absorpt_t_min   0.177
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 Ag1, Ag2, Fe1, Cl1, Cl2, Cl3, Cl4, Cl5, Cl6, Cl7, Cl8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3C,H3D,H3E), N4(H4C,H4D,H4E)
;
_shelx_res_checksum              29400
_shelx_hkl_checksum              23966
_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 2.157
_oxdiff_exptl_absorpt_empirical_full_min 0.643