Strong Magnetocrystalline Anisotropy Arising from Metal–Ligand Covalency in a Metal–Organic Candidate for 2D Magnetic Order
Wang, Yiran; Ziebel, Michael E.; Sun, Lei; Gish, J. Tyler; Pearson, Tyler J.; Lu, Xue-Zeng; Thorarinsdottir, Agnes E.; Hersam, Mark C.; Long, Jeffrey R.; Freedman, Danna E.; Rondinelli, James M.; Puggioni, Danilo; Harris, T. David; Chemistry of Materials 33 (2021) 8712–8721; doi:10.1021/acs.chemmater.1c02670

data_4004050
_publ_section_title
;
 Strong Magnetocrystalline Anisotropy Arising from Metal--Ligand Covalency
 in a Metal--Organic Candidate for 2D Magnetic Order
;
_journal_issue                   22
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8712
_journal_page_last               8721
_journal_paper_doi               10.1021/acs.chemmater.1c02670
_journal_volume                  33
_journal_year                    2021
_chemical_formula_moiety         '0.33(C18 Cl6 Fe2 O12), 0.67(C4 H12 N1)'
_chemical_formula_sum            'C14 H24 Cl2 Fe2 N2 O4'
_chemical_formula_weight         466.95
_chemical_name_common            2
_space_group_crystal_system      trigonal
_space_group_IT_number           162
_space_group_name_Hall           '-P 3 2'
_space_group_name_H-M_alt        'P -3 1 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.5717(18)
_cell_length_b                   13.5717(18)
_cell_length_c                   9.9759(18)
_cell_measurement_reflns_used    939
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      50.11
_cell_measurement_theta_min      3.76
_cell_volume                     1591.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      250.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2180
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        50.358
_diffrn_reflns_theta_max         50.358
_diffrn_reflns_theta_min         3.761
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.445
_exptl_absorpt_correction_T_max  0.7499
_exptl_absorpt_correction_T_min  0.4603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1033 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.6138.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         606
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.1011
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2595
_refine_ls_wR_factor_ref         0.2916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                397
_reflns_number_total             606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c02670_si_002.cif
_cod_data_source_block           NMe4_Fe2_Cl2dhbq3
_cod_original_cell_volume        1591.3(5)
_cod_database_code               4004050
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.105
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3 \\sim N1-C4
 with sigma of 0.002
3. Rigid bond restraints
 C3, N1, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C3 \\sim N1 \\sim C4: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.002
5. Others
 Fixed Sof: C3(0.16667) H3A(0.16667) H3B(0.16667) H3C(0.16667) C4(0.5)
 H4A(0.5) H4B(0.5) H4C(0.5)
6.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              18019
_shelx_hkl_checksum              7291
_shelx_fab_checksum              55080
_olex2_submission_special_instructions 'No special instructions were received'