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_4004075
_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_absolute_configuration ad
_chemical_formula_moiety         'Ag Cl2, Cl6 Fe, 4(C9 H14 N)'
_chemical_formula_sum            'C36 H56 Ag Cl8 Fe N4'
_chemical_formula_weight         992.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.73130(10)
_cell_length_b                   35.4619(5)
_cell_length_c                   7.73470(10)
_cell_measurement_reflns_used    7987
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.4260
_cell_measurement_theta_min      4.9870
_cell_volume                     2120.39(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.980
_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     51.00 141.00   1.00    8.00    --  113.00 -61.00-150.00   90
  2  \w    -74.00  39.00   1.00    3.00    --  -39.95  77.00 120.00  113
  3  \w    -89.00 -10.00   1.00    3.00    --  -39.95 -57.00 -30.00   79
  4  \w    -39.00  79.00   1.00    3.00    --   39.95 -19.00-180.00  118
  5  \w     39.00  97.00   1.00    3.00    --   39.95-125.00 -90.00   58
  6  \w     92.00 172.00   1.00    8.00    --  113.00  45.00   0.00   80
  7  \w    152.00 178.00   1.00    8.00    --  113.00  77.00-150.00   26
  8  \w     36.00 101.00   1.00    8.00    --  113.00-111.00  90.00   65
  9  \w     35.00 109.00   1.00    8.00    --  113.00-111.00 150.00   74
 10  \w     89.00 178.00   1.00    8.00    --  113.00  61.00-120.00   89
 11  \w    119.00 178.00   1.00    8.00    --  113.00 111.00 -60.00   59
 12  \w    115.00 147.00   1.00    8.00    --  113.00  77.00-150.00   32
 13  \w     33.00 107.00   1.00    8.00    --  113.00 -94.00-120.00   74
 14  \w     62.00 146.00   1.00    8.00    --  113.00 178.00 120.00   84
 15  \w     86.00 173.00   1.00    8.00    --  113.00  45.00 -60.00   87
;
_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      -0.0730944000
_diffrn_orient_matrix_UB_12      -0.0402036000
_diffrn_orient_matrix_UB_13      0.0173268000
_diffrn_orient_matrix_UB_21      -0.1801378000
_diffrn_orient_matrix_UB_22      0.0164111000
_diffrn_orient_matrix_UB_23      0.0373744000
_diffrn_orient_matrix_UB_31      -0.0439509000
_diffrn_orient_matrix_UB_32      -0.0004263000
_diffrn_orient_matrix_UB_33      -0.1949391000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13850
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.463
_diffrn_reflns_theta_min         2.492
_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    11.327
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39028
_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    1.554
_exptl_crystal_description       plate
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.614
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 2463 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7748
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1114P)^2^+14.4840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2116
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.792
_reflns_Friedel_fraction_max     0.756
_reflns_number_gt                7060
_reflns_number_total             7748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm2c00163_si_006.cif
_cod_data_source_block           xuejie17cu_173k
_cod_database_code               4004075
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N4, C4, C40, C41, C42, C43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2, C2, C20, C21, C22, C23, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C10, C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E), C3(H3D,H3E), C4(H4D,H4E)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
3.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C10(H10A,H10B,H10C), N2(H2A,H2B,H2C), C20(H20A,H20B,H20C),
 N3(H3A,H3B,H3C), C30(H30A,H30B,H30C), N4(H4A,H4B,H4C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              89975
_shelx_hkl_checksum              74439
_olex2_date_sample_data_collection 2021-06-10
_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 2.030
_oxdiff_exptl_absorpt_empirical_full_min 0.656