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_4004076
_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         'Cl8 Fe Na, 4(C8 H12 N)'
_chemical_formula_sum            'C32 H48 Cl8 Fe N4 Na'
_chemical_formula_weight         851.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-12
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6398(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.25334(10)
_cell_length_b                   39.2496(6)
_cell_length_c                   7.18736(10)
_cell_measurement_reflns_used    6511
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.7210
_cell_measurement_theta_min      6.2560
_cell_volume                     2046.05(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (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
'olex2.solve 1.5-alpha (Bourhis et al., 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 0.998
_diffrn_measured_fraction_theta_max 0.976
_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     41.00 107.00   0.50    4.00    --  113.00-111.00 -30.00  132
  2  \w     11.00 107.00   0.50    2.00    --   39.95  57.00 -90.00  192
  3  \w    -20.00  74.00   0.50    2.00    --   39.95 -77.00 120.00  188
  4  \w     16.00 116.00   0.50    2.00    --   39.95  37.00  30.00  200
  5  \w     48.00  98.00   0.50    2.00    --   39.95-126.00  53.00  100
  6  \w     61.00 146.00   0.50    4.00    --  113.00 178.00 -30.00  170
  7  \w     35.00 144.00   0.50    4.00    --  113.00 -30.00  60.00  218
  8  \w    143.00 178.00   0.50    4.00    --  113.00 111.00 -60.00   70
  9  \w     86.00 172.00   0.50    4.00    --  113.00  45.00  90.00  172
 10  \w     37.00 139.00   0.50    4.00    --  113.00 -30.00 -90.00  204
 11  \w    106.00 132.00   0.50    4.00    --  113.00 111.00 -60.00   52
 12  \w     66.00 145.00   0.50    4.00    --  113.00 178.00   0.00  158
 13  \w     38.00 104.00   0.50    4.00    --  113.00-111.00 120.00  132
 14  \w     70.00 138.00   0.50    4.00    --  113.00 -77.00 -60.00  136
;
_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      0.0274564000
_diffrn_orient_matrix_UB_12      -0.0018225000
_diffrn_orient_matrix_UB_13      0.2126408000
_diffrn_orient_matrix_UB_21      -0.0129753000
_diffrn_orient_matrix_UB_22      0.0391234000
_diffrn_orient_matrix_UB_23      0.0115026000
_diffrn_orient_matrix_UB_31      -0.2101772000
_diffrn_orient_matrix_UB_32      -0.0026330000
_diffrn_orient_matrix_UB_33      0.0247135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            12363
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.806
_diffrn_reflns_theta_min         6.102
_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    8.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       plate
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0628P)^2^+2.8842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3891
_reflns_number_total             4208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm2c00163_si_005.cif
_cod_data_source_block           xuejie15c_173k
_cod_database_code               4004076
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe Na Cl8 N4 C32 H48 '
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.237
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_shelx_res_checksum              37396
_shelx_hkl_checksum              94235
_olex2_date_sample_data_collection 2021-07-07
_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 1.892
_oxdiff_exptl_absorpt_empirical_full_min 0.648