Rare “Janus”-Faced {FeII7} Single-Molecule Magnet Exhibiting Intramolecular Ferromagnetic Interactions
Alexandropoulos, Dimitris I.; Vignesh, Kuduva R.; Stamatatos, Theocharis; Dunbar, Kim R.; Chemical Science  (2019) –; doi:10.1039/C8SC04384A

data_1550196
_publ_section_title
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 Rare &#x201C;Janus&#x201D;-Faced {FeII7} Single-Molecule Magnet
 Exhibiting Intramolecular Ferromagnetic Interactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04384A
_journal_year                    2019
_chemical_formula_moiety         'C24 H36 Fe7 N48, 4(C2 H3 N), 2(Cl O4)'
_chemical_formula_sum            'C32 H48 Cl2 Fe7 N52 O8'
_chemical_formula_weight         1751.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                93.108(2)
_cell_angle_beta                 94.573(2)
_cell_angle_gamma                98.460(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4046(7)
_cell_length_b                   12.5476(8)
_cell_length_c                   13.4127(9)
_cell_measurement_reflns_used    8206
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.741
_cell_measurement_theta_min      2.471
_cell_volume                     1888.2(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15101
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.773
_diffrn_reflns_theta_min         2.627
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.6956.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.733
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.255
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6891
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0227P)^2^+3.5724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5294
_reflns_number_total             6891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04384a2.cif
_cod_data_source_block           da429_2_0m_a
_cod_database_code               1550196
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-O1 \\sim Cl1-O2 \\sim Cl1-O3 \\sim Cl1-O4 \\sim Cl1A-O1A \\sim Cl1A-O2A
\\sim Cl1A-O3A \\sim Cl1A-O4A
 with sigma of 0.02
 O1-O2 \\sim O2-O3 \\sim O3-O4 \\sim O4-O1 \\sim O1A-O2A \\sim O2A-O3A \\sim
O3A-O4A \\sim O4A-O1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim O1 \\sim O2 \\sim O3 \\sim O3 \\sim O4 \\sim Cl1A \\sim O1A \\sim O2A
\\sim O3A \\sim O4A: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
Uanis(Cl1) = Uanis(Cl1A)
4. Rigid body (RIGU) restrains
 Cl1, O1, O2, O3, O3, O4, Cl1A, O1A, O2A, O3A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=1-FVAR(1)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(1)
6.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              8757
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'