#------------------------------------------------------------------------------
#$Date: 2025-08-22 23:12:46 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301866 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/68/7236894.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_7236894
loop_
_publ_author_name
'Iasco, O.'
'Boillot, M.-L.'
'Bellec, A.'
'Guillot, R.'
'Rivière, E.'
'Mazerat, S.'
'Nowak, S.'
'Morineau, D.'
'Brosseau, A.'
'Miserque, F.'
'Repain, V.'
'Mallah, T.'
_publ_section_title
;
 The disentangling of hysteretic spin transition, polymorphism and
 metastability in bistable thin films formed by sublimation of
 bis(scorpionate) Fe(ii) molecules
;
_journal_issue                   42
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              11067
_journal_paper_doi               10.1039/C7TC03276E
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C30 H44 B2 Fe N12'
_chemical_formula_sum            'C30 H44 B2 Fe N12'
_chemical_formula_weight         650.24
_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_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                115.322(2)
_cell_angle_beta                 98.499(3)
_cell_angle_gamma                109.477(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7244(5)
_cell_length_b                   10.4918(6)
_cell_length_c                   10.8211(6)
_cell_measurement_temperature    100(1)
_cell_volume                     793.58(9)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26912
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.647
_diffrn_reflns_theta_min         2.215
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_correction_T_min  0.9712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0554
_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/[σ²(Fo²)+(0.0677P)²+0.5073P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3749
_reflns_number_total             4888
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7tc03276e2.cif
_cod_data_source_block           Fe_T100K
_cod_original_cell_volume        793.58(8)
_cod_database_code               7236894
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.4525(3) 0.1020(3) 0.2979(2) 0.0175(5) Uani 1 1 d . . .
H1A H 0.3810 0.1449 0.2711 0.026 Uiso 1 1 calc R U .
H1B H 0.3807 0.0026 0.2859 0.026 Uiso 1 1 calc R U .
H1C H 0.5222 0.0873 0.2370 0.026 Uiso 1 1 calc R U .
C2 C 0.5675(3) 0.2132(2) 0.4537(2) 0.0126(4) Uani 1 1 d . . .
C3 C 0.6690(3) 0.1807(3) 0.5384(2) 0.0146(4) Uani 1 1 d . . .
H3 H 0.6770 0.0867 0.5095 0.017 Uiso 1 1 calc R U .
C4 C 0.7544(3) 0.3163(3) 0.6732(2) 0.0120(4) Uani 1 1 d . . .
C5 C 0.8794(3) 0.3483(3) 0.8055(3) 0.0171(5) Uani 1 1 d . . .
H5A H 0.9906 0.4286 0.8278 0.026 Uiso 1 1 calc R U .
H5B H 0.8887 0.2538 0.7875 0.026 Uiso 1 1 calc R U .
H5C H 0.8390 0.3831 0.8860 0.026 Uiso 1 1 calc R U .
C6 C 0.1716(3) 0.5681(3) 0.6457(2) 0.0163(4) Uani 1 1 d . . .
H6A H 0.1782 0.6665 0.6590 0.024 Uiso 1 1 calc R U .
H6B H 0.0771 0.5205 0.6716 0.024 Uiso 1 1 calc R U .
H6C H 0.1534 0.4992 0.5457 0.024 Uiso 1 1 calc R U .
C7 C 0.3365(3) 0.5959(3) 0.7400(2) 0.0123(4) Uani 1 1 d . . .
C8 C 0.3868(3) 0.6523(3) 0.8897(2) 0.0130(4) Uani 1 1 d . . .
H8 H 0.3240 0.6801 0.9504 0.016 Uiso 1 1 calc R U .
C9 C 0.5482(3) 0.6584(2) 0.9294(2) 0.0111(4) Uani 1 1 d . . .
C10 C 0.6614(3) 0.7054(3) 1.0738(2) 0.0168(5) Uani 1 1 d . . .
H10A H 0.6650 0.6141 1.0719 0.025 Uiso 1 1 calc R U .
H10B H 0.6160 0.7524 1.1474 0.025 Uiso 1 1 calc R U .
H10C H 0.7761 0.7799 1.0951 0.025 Uiso 1 1 calc R U .
C11 C 0.7847(3) 0.7911(3) 0.4389(2) 0.0156(4) Uani 1 1 d . . .
H11A H 0.8379 0.7455 0.3719 0.023 Uiso 1 1 calc R U .
H11B H 0.8205 0.8990 0.4655 0.023 Uiso 1 1 calc R U .
H11C H 0.6612 0.7341 0.3939 0.023 Uiso 1 1 calc R U .
C12 C 0.8383(3) 0.7828(2) 0.5722(2) 0.0117(4) Uani 1 1 d . . .
C13 C 0.9975(3) 0.8820(3) 0.6859(2) 0.0137(4) Uani 1 1 d . . .
H13 H 1.0888 0.9659 0.6939 0.016 Uiso 1 1 calc R U .
C14 C 0.9919(3) 0.8304(2) 0.7839(2) 0.0111(4) Uani 1 1 d . . .
C15 C 1.1258(3) 0.8933(3) 0.9254(2) 0.0158(4) Uani 1 1 d . . .
H15A H 1.0783 0.9218 1.0021 0.024 Uiso 1 1 calc R U .
H15B H 1.2242 0.9843 0.9448 0.024 Uiso 1 1 calc R U .
H15C H 1.1608 0.8140 0.9201 0.024 Uiso 1 1 calc R U .
B1 B 0.7565(3) 0.5952(3) 0.7859(3) 0.0106(4) Uani 1 1 d . . .
H1 H 0.8384 0.6250 0.8771 0.013 Uiso 1 1 calc R U .
N1 N 0.5901(2) 0.3618(2) 0.53277(18) 0.0099(3) Uani 1 1 d . . .
N2 N 0.4618(2) 0.5698(2) 0.69087(19) 0.0100(3) Uani 1 1 d . . .
N3 N 0.7394(2) 0.6756(2) 0.59901(18) 0.0103(3) Uani 1 1 d . . .
N4 N 0.7055(2) 0.4245(2) 0.66819(18) 0.0100(3) Uani 1 1 d . . .
N5 N 0.5911(2) 0.6077(2) 0.80831(18) 0.0095(3) Uani 1 1 d . . .
N6 N 0.8359(2) 0.7051(2) 0.72913(18) 0.0095(3) Uani 1 1 d . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.00753(12) Uani 1 2 d S . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0016 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8476 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C3 109.69(19) . .
N1 C2 C1 124.25(19) . .
C3 C2 C1 126.1(2) . .
C4 C3 C2 106.2(2) . .
C4 C3 H3 126.9 . .
C2 C3 H3 126.9 . .
N4 C4 C3 107.44(19) . .
N4 C4 C5 123.34(19) . .
C3 C4 C5 129.2(2) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 C8 109.31(19) . .
N2 C7 C6 123.59(19) . .
C8 C7 C6 127.1(2) . .
C9 C8 C7 106.43(19) . .
C9 C8 H8 126.8 . .
C7 C8 H8 126.8 . .
N5 C9 C8 107.31(18) . .
N5 C9 C10 122.8(2) . .
C8 C9 C10 129.9(2) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 H11A 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C12 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N3 C12 C13 109.63(19) . .
N3 C12 C11 124.29(19) . .
C13 C12 C11 126.1(2) . .
C14 C13 C12 106.39(19) . .
C14 C13 H13 126.8 . .
C12 C13 H13 126.8 . .
N6 C14 C13 107.10(18) . .
N6 C14 C15 123.38(19) . .
C13 C14 C15 129.5(2) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N5 B1 N4 108.27(17) . .
N5 B1 N6 107.50(17) . .
N4 B1 N6 108.55(17) . .
N5 B1 H1 110.8 . .
N4 B1 H1 110.8 . .
N6 B1 H1 110.8 . .
C2 N1 N4 106.44(17) . .
C2 N1 Fe1 136.21(15) . .
N4 N1 Fe1 117.36(13) . .
C7 N2 N5 106.68(16) . .
C7 N2 Fe1 135.58(15) . .
N5 N2 Fe1 117.71(13) . .
C12 N3 N6 106.42(17) . .
C12 N3 Fe1 135.67(15) . .
N6 N3 Fe1 117.90(13) . .
C4 N4 N1 110.25(17) . .
C4 N4 B1 130.79(18) . .
N1 N4 B1 118.96(16) . .
C9 N5 N2 110.27(17) . .
C9 N5 B1 131.14(18) . .
N2 N5 B1 118.51(16) . .
C14 N6 N3 110.46(17) . .
C14 N6 B1 131.41(17) . .
N3 N6 B1 118.12(16) . .
N1 Fe1 N1 180.0 . 2_666
N1 Fe1 N2 89.97(7) . .
N1 Fe1 N2 90.03(7) 2_666 .
N1 Fe1 N2 90.03(7) . 2_666
N1 Fe1 N2 89.97(7) 2_666 2_666
N2 Fe1 N2 180.00(12) . 2_666
N1 Fe1 N3 89.60(7) . .
N1 Fe1 N3 90.40(7) 2_666 .
N2 Fe1 N3 89.82(7) . .
N2 Fe1 N3 90.17(7) 2_666 .
N1 Fe1 N3 90.40(7) . 2_666
N1 Fe1 N3 89.60(7) 2_666 2_666
N2 Fe1 N3 90.17(7) . 2_666
N2 Fe1 N3 89.83(7) 2_666 2_666
N3 Fe1 N3 180.0 . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.498(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 N1 1.344(3) .
C2 C3 1.403(3) .
C3 C4 1.380(3) .
C3 H3 0.9300 .
C4 N4 1.357(3) .
C4 C5 1.494(3) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.492(3) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 N2 1.342(3) .
C7 C8 1.401(3) .
C8 C9 1.381(3) .
C8 H8 0.9300 .
C9 N5 1.350(3) .
C9 C10 1.490(3) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.497(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 N3 1.341(3) .
C12 C13 1.401(3) .
C13 C14 1.381(3) .
C13 H13 0.9300 .
C14 N6 1.354(3) .
C14 C15 1.496(3) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
B1 N5 1.536(3) .
B1 N4 1.542(3) .
B1 N6 1.545(3) .
B1 H1 0.9800 .
N1 N4 1.375(2) .
N1 Fe1 1.9908(17) .
N2 N5 1.375(2) .
N2 Fe1 1.9966(17) .
N3 N6 1.375(2) .
N3 Fe1 1.9975(17) .
Fe1 N1 1.9909(17) 2_666
Fe1 N2 1.9967(17) 2_666
Fe1 N3 1.9975(18) 2_666
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168339839
