#------------------------------------------------------------------------------
#$Date: 2021-11-17 00:59:48 +0200 (Wed, 17 Nov 2021) $
#$Revision: 270695 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/92/7129255.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7129255
loop_
_publ_author_name
'Srinivasan, Anandi'
'Musgrave, Rebecca A.'
'Rouzieres, Mathieu'
'Clerac, Rodolphe'
'McGrady, John E.'
'Hillard, Elizabeth A.'
_publ_section_title
;
 A Linear Metal-Metal Bonded Tri-Iron Single-Molecule Magnet
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05043E
_journal_year                    2021
_chemical_compound_source        no
_chemical_formula_moiety         'C44 H36 Fe3 N16'
_chemical_formula_sum            'C44 H36 Fe3 N16'
_chemical_formula_weight         956.42
_chemical_melting_point          ?
_chemical_name_systematic
'tetrakis(dipyridylformamidinato)triiron(II) bis(tetrafluoroborate) acetonitrile solvate''
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_Int_Tables_number      87
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-08-28 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7015(10)
_cell_length_b                   12.7015(10)
_cell_length_c                   32.268(3)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.52
_cell_volume                     5205.7(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9949
_diffrn_measured_fraction_theta_max 0.9949
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            40554
_diffrn_reflns_theta_full        26.4762
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.2202
_exptl_crystal_description       plate
_exptl_crystal_F_000             1964.7475
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile and diethyl ether'
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.1661
_refine_diff_density_min         -0.5110
_refine_diff_density_rms         0.0850
_refine_ls_d_res_high            0.7971
_refine_ls_d_res_low             11.8189
_refine_ls_goodness_of_fit_ref   1.0663
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0663
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0643P)²+5.6404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                1899
_reflns_number_total             2750
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1cc05043e2.cif
_cod_data_source_block           mm286_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        5205.8(7)
_cod_database_code               7129255
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1), C4(H4), C2(H2), C3(H3), C8(H8), C11(H11), C10(H10), C9(H9)
;
_olex2_date_sample_data_collection 2017-01-25
_olex2_date_sample_submission    2017-01-25
_olex2_submission_original_sample_id MM286
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x,z
3 y,-x,z
4 -x,-y,z
5 -x,-y,-z
6 y,-x,-z
7 -y,x,-z
8 x,y,-z
9 x+1/2,y+1/2,z+1/2
10 -y+1/2,x+1/2,z+1/2
11 y+1/2,-x+1/2,z+1/2
12 -x+1/2,-y+1/2,z+1/2
13 -x+1/2,-y+1/2,-z+1/2
14 y+1/2,-x+1/2,-z+1/2
15 -y+1/2,x+1/2,-z+1/2
16 x+1/2,y+1/2,-z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe2 Fe 0.5 0.0 0.25 0.0317(2) Uani 1.000000 4 S T P
Fe1 Fe 0.5 0.0 0.164026(16) 0.03186(18) Uani 1.000000 2 S T P
N2 N 0.43006(14) -0.15061(14) 0.23823(7) 0.0245(4) Uani 1.000000 1 . . .
N1 N 0.42895(15) -0.15336(15) 0.16620(6) 0.0288(5) Uani 1.000000 1 . . .
N3 N 0.35274(16) 0.06417(15) 0.19112(7) 0.0305(5) Uani 1.000000 1 . . .
C5 C 0.40571(17) -0.20430(17) 0.20181(7) 0.0230(5) Uani 1.000000 1 . . .
N4 N 0.3753(2) 0.05732(18) 0.12213(7) 0.0477(7) Uani 1.000000 1 . . .
C6 C 0.41191(18) -0.19653(19) 0.27461(8) 0.0305(6) Uani 1.000000 1 . . .
H6 H 0.38166(18) -0.26488(19) 0.27565(8) 0.0366(7) Uiso 1.000000 1 R . .
C1 C 0.41014(18) -0.20029(19) 0.12951(9) 0.0319(6) Uani 1.000000 1 . . .
H1 H 0.42642(18) -0.16284(19) 0.10484(9) 0.0383(7) Uiso 1.000000 1 R . .
C4 C 0.3616(2) -0.3064(2) 0.19986(9) 0.0398(7) Uani 1.000000 1 . . .
H4 H 0.3438(2) -0.3431(2) 0.22453(9) 0.0477(8) Uiso 1.000000 1 R . .
C7 C 0.3055(2) 0.0805(2) 0.15252(9) 0.0419(7) Uani 1.000000 1 . . .
C2 C 0.3685(2) -0.2998(2) 0.12606(10) 0.0407(7) Uani 1.000000 1 . . .
H2 H 0.3568(2) -0.3311(2) 0.09971(10) 0.0488(8) Uiso 1.000000 1 R . .
C3 C 0.3446(2) -0.3519(2) 0.16157(10) 0.0495(8) Uani 1.000000 1 . . .
H3 H 0.3157(2) -0.4207(2) 0.16006(10) 0.0594(10) Uiso 1.000000 1 R . .
C8 C 0.2026(2) 0.1138(3) 0.14339(10) 0.0564(9) Uani 1.000000 1 . . .
H8 H 0.1533(2) 0.1284(3) 0.16474(10) 0.0677(11) Uiso 1.000000 1 R . .
C11 C 0.3456(3) 0.0690(3) 0.08255(10) 0.0702(12) Uani 1.000000 1 . . .
H11 H 0.3946(3) 0.0525(3) 0.06128(10) 0.0843(14) Uiso 1.000000 1 R . .
C10 C 0.2469(3) 0.1040(4) 0.07144(13) 0.0924(16) Uani 1.000000 1 . . .
H10 H 0.2288(3) 0.1137(4) 0.04312(13) 0.1108(19) Uiso 1.000000 1 R . .
C9 C 0.1761(3) 0.1245(4) 0.10190(13) 0.0859(15) Uani 1.000000 1 . . .
H9 H 0.1071(3) 0.1465(4) 0.09467(13) 0.1031(18) Uiso 1.000000 1 R . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Fe 0.35822 0.84933 11.76950 7.35730 3.52220 2.30450 4.76110 0.30720 15.35350
76.88050 1.03690004349
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Fe1 Fe2 Fe1 180.0 14 . ?
N2 Fe2 Fe1 100.21(6) 4_655 14 ?
N2 Fe2 Fe1 79.79(6) 14 14 ?
N2 Fe2 Fe1 79.79(6) . . ?
N2 Fe2 Fe1 100.21(6) 14 . ?
N2 Fe2 Fe1 100.21(6) . 14 ?
N2 Fe2 Fe1 100.21(6) 15_545 . ?
N2 Fe2 Fe1 79.79(6) 4_655 . ?
N2 Fe2 Fe1 79.79(6) 15_545 14 ?
N2 Fe2 N2 91.80(2) 14 4_655 ?
N2 Fe2 N2 91.80(2) 14 . ?
N2 Fe2 N2 159.58(11) 15_545 14 ?
N2 Fe2 N2 159.58(11) 4_655 . ?
N2 Fe2 N2 91.80(2) 15_545 . ?
N2 Fe2 N2 91.80(2) 15_545 4_655 ?
N1 Fe1 Fe2 88.13(6) 4_655 . ?
N1 Fe1 Fe2 88.13(6) . . ?
N1 Fe1 N1 176.26(11) 4_655 . ?
N3 Fe1 Fe2 66.80(6) . . ?
N3 Fe1 Fe2 66.80(6) 4_655 . ?
N3 Fe1 N1 90.47(7) 4_655 . ?
N3 Fe1 N1 88.06(7) 4_655 4_655 ?
N3 Fe1 N1 90.47(7) . 4_655 ?
N3 Fe1 N1 88.06(7) . . ?
N3 Fe1 N3 133.61(11) 4_655 . ?
N4 Fe1 Fe2 127.80(7) 4_655 . ?
N4 Fe1 Fe2 127.80(7) . . ?
N4 Fe1 N1 91.28(8) . 4_655 ?
N4 Fe1 N1 91.01(8) 4_655 4_655 ?
N4 Fe1 N1 91.01(8) . . ?
N4 Fe1 N1 91.28(8) 4_655 . ?
N4 Fe1 N3 165.36(9) . 4_655 ?
N4 Fe1 N3 61.01(9) 4_655 4_655 ?
N4 Fe1 N3 61.01(9) . . ?
N4 Fe1 N3 165.36(9) 4_655 . ?
N4 Fe1 N4 104.39(14) 4_655 . ?
C5 N2 Fe2 132.72(15) . . ?
C6 N2 Fe2 107.85(17) . . ?
C6 N2 C5 119.4(2) . . ?
C5 N1 Fe1 123.62(15) . . ?
C1 N1 Fe1 116.56(17) . . ?
C1 N1 C5 119.8(2) . . ?
C6 N3 Fe1 145.32(17) 14 . ?
C7 N3 Fe1 93.75(18) . . ?
C7 N3 C6 120.9(2) . 14 ?
N1 C5 N2 115.7(2) . . ?
C4 C5 N2 125.1(2) . . ?
C4 C5 N1 119.2(2) . . ?
C7 N4 Fe1 95.63(16) . . ?
C11 N4 Fe1 145.4(3) . . ?
C11 N4 C7 118.8(3) . . ?
N3 C6 N2 119.8(2) 15_545 . ?
H6 C6 N2 120.12(14) . . ?
H6 C6 N3 120.12(14) . 15_545 ?
H1 C1 N1 118.44(14) . . ?
C2 C1 N1 123.1(3) . . ?
C2 C1 H1 118.44(18) . . ?
H4 C4 C5 120.47(15) . . ?
C3 C4 C5 119.1(2) . . ?
C3 C4 H4 120.47(16) . . ?
N4 C7 N3 109.4(3) . . ?
C8 C7 N3 129.1(3) . . ?
C8 C7 N4 121.5(3) . . ?
H2 C2 C1 121.12(18) . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 H2 121.12(15) . . ?
C2 C3 C4 121.1(2) . . ?
H3 C3 C4 119.45(16) . . ?
H3 C3 C2 119.45(15) . . ?
H8 C8 C7 121.37(19) . . ?
C9 C8 C7 117.3(4) . . ?
C9 C8 H8 121.4(3) . . ?
H11 C11 N4 118.7(2) . . ?
C10 C11 N4 122.7(4) . . ?
C10 C11 H11 118.7(2) . . ?
H10 C10 C11 120.8(2) . . ?
C9 C10 C11 118.4(3) . . ?
C9 C10 H10 120.8(2) . . ?
C10 C9 C8 121.3(4) . . ?
H9 C9 C8 119.3(3) . . ?
H9 C9 C10 119.3(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe2 Fe1 2.7742(6) . ?
Fe2 Fe1 2.7742(6) 14 ?
Fe2 N2 2.1431(18) 14 ?
Fe2 N2 2.1431(18) 4_655 ?
Fe2 N2 2.1431(18) 15_545 ?
Fe2 N2 2.1431(18) . ?
Fe1 N1 2.1479(19) 4_655 ?
Fe1 N1 2.1479(19) . ?
Fe1 N3 2.220(2) 4_655 ?
Fe1 N3 2.220(2) . ?
Fe1 N4 2.206(2) 4_655 ?
Fe1 N4 2.206(2) . ?
N2 C5 1.393(3) . ?
N2 C6 1.331(3) . ?
N1 C5 1.352(3) . ?
N1 C1 1.347(3) . ?
N3 C6 1.306(3) 14 ?
N3 C7 1.398(3) . ?
C5 C4 1.414(3) . ?
N4 C7 1.355(4) . ?
N4 C11 1.340(4) . ?
C6 H6 0.9500 . ?
C1 H1 0.9500 . ?
C1 C2 1.375(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.381(4) . ?
C7 C8 1.404(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.358(4) . ?
C3 H3 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.387(5) . ?
C11 H11 0.9500 . ?
C11 C10 1.378(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.357(6) . ?
C9 H9 0.9500 . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.584 -0.192 -0.819 1591.1 528.6 ?
