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#$Date: 2025-08-22 23:12:46 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301866 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/68/7236895.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_7236895
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_sum            'C15 H22 B Fe0.5 N6'
_chemical_formula_weight         325.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                106.485(7)
_cell_angle_beta                 108.711(7)
_cell_angle_gamma                109.714(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7770(9)
_cell_length_b                   10.7908(10)
_cell_length_c                   10.9916(17)
_cell_measurement_reflns_used    7827
_cell_measurement_temperature    240(1)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.62
_cell_volume                     833.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      240(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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            29746
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_min         2.232
_exptl_absorpt_coefficient_mu    0.453
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_F_000             344
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0636
_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)+(0.0821P)²+0.2198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3460
_reflns_number_total             5099
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7tc03276e2.cif
_cod_data_source_block           Fe_T240K
_cod_original_cell_volume        833.71(18)
_cod_original_formula_sum        'C15 H22 B Fe0.50 N6'
_cod_database_code               7236895
_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.
;
_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 0.3235(5) 0.5638(4) 0.9460(3) 0.0546(8) Uani 1 1 d . . .
H1A H 0.4436 0.5964 1.0186 0.082 Uiso 1 1 calc R U .
H1B H 0.2342 0.5023 0.9643 0.082 Uiso 1 1 calc R U .
H1C H 0.3060 0.6471 0.9470 0.082 Uiso 1 1 calc R U .
C2 C 0.3031(4) 0.4791(3) 0.8031(3) 0.0395(6) Uani 1 1 d . . .
C3 C 0.1952(4) 0.3325(4) 0.7125(3) 0.0477(7) Uani 1 1 d . . .
H3 H 0.1142 0.2630 0.7263 0.057 Uiso 1 1 calc R U .
C4 C 0.2310(4) 0.3086(3) 0.5963(3) 0.0416(6) Uani 1 1 d . . .
C5 C 0.1495(5) 0.1659(3) 0.4668(4) 0.0589(9) Uani 1 1 d . . .
H5A H 0.0232 0.1354 0.4096 0.088 Uiso 1 1 calc R U .
H5B H 0.1597 0.0925 0.4969 0.088 Uiso 1 1 calc R U .
H5C H 0.2137 0.1789 0.4115 0.088 Uiso 1 1 calc R U .
C6 C 0.4325(5) 0.9597(3) 0.8139(3) 0.0473(7) Uani 1 1 d . . .
H6A H 0.3408 0.9040 0.8340 0.071 Uiso 1 1 calc R U .
H6B H 0.4112 1.0371 0.7992 0.071 Uiso 1 1 calc R U .
H6C H 0.5507 1.0010 0.8931 0.071 Uiso 1 1 calc R U .
C7 C 0.4244(4) 0.8617(3) 0.6821(3) 0.0328(5) Uani 1 1 d . . .
C8 C 0.3744(4) 0.8629(3) 0.5511(3) 0.0397(6) Uani 1 1 d . . .
H8 H 0.3374 0.9267 0.5248 0.048 Uiso 1 1 calc R U .
C9 C 0.3896(4) 0.7504(3) 0.4655(3) 0.0370(6) Uani 1 1 d . . .
C10 C 0.3499(5) 0.7043(4) 0.3120(3) 0.0511(8) Uani 1 1 d . . .
H10A H 0.3774 0.6254 0.2818 0.077 Uiso 1 1 calc R U .
H10B H 0.4236 0.7857 0.3019 0.077 Uiso 1 1 calc R U .
H10C H 0.2233 0.6721 0.2540 0.077 Uiso 1 1 calc R U .
C11 C 0.9057(4) 0.8764(3) 1.0773(3) 0.0495(8) Uani 1 1 d . . .
H11A H 0.8932 0.9602 1.0725 0.074 Uiso 1 1 calc R U .
H11B H 1.0251 0.9084 1.1503 0.074 Uiso 1 1 calc R U .
H11C H 0.8153 0.8226 1.0997 0.074 Uiso 1 1 calc R U .
C12 C 0.8797(4) 0.7800(3) 0.9362(3) 0.0353(6) Uani 1 1 d . . .
C13 C 1.0033(4) 0.7468(3) 0.9020(3) 0.0434(7) Uani 1 1 d . . .
H13 H 1.1242 0.7789 0.9642 0.052 Uiso 1 1 calc R U .
C14 C 0.9116(4) 0.6557(3) 0.7563(3) 0.0392(6) Uani 1 1 d . . .
C15 C 0.9827(4) 0.5900(4) 0.6632(4) 0.0529(8) Uani 1 1 d . . .
H15A H 0.9888 0.5073 0.6763 0.079 Uiso 1 1 calc R U .
H15B H 1.1024 0.6618 0.6886 0.079 Uiso 1 1 calc R U .
H15C H 0.9026 0.5588 0.5649 0.079 Uiso 1 1 calc R U .
B1 B 0.5335(4) 0.7006(3) 0.7904(3) 0.0311(6) Uani 1 1 d . . .
H1 H 0.5436 0.7633 0.8800 0.037 Uiso 1 1 calc R U .
N1 N 0.3535(3) 0.4343(2) 0.6127(2) 0.0335(5) Uani 1 1 d . . .
N2 N 0.4468(3) 0.6827(2) 0.5400(2) 0.0312(5) Uani 1 1 d . . .
N3 N 0.7394(3) 0.6327(2) 0.7027(2) 0.0321(5) Uani 1 1 d . . .
N4 N 0.3968(3) 0.5405(2) 0.7411(2) 0.0305(5) Uani 1 1 d . . .
N5 N 0.4680(3) 0.7524(2) 0.6750(2) 0.0279(4) Uani 1 1 d . . .
N6 N 0.7212(3) 0.7106(2) 0.8152(2) 0.0295(4) Uani 1 1 d . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.02396(16) 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 . .
N4 C2 C3 107.6(3) . .
N4 C2 C1 123.2(3) . .
C3 C2 C1 129.2(3) . .
C2 C3 C4 106.3(3) . .
C2 C3 H3 126.8 . .
C4 C3 H3 126.8 . .
N1 C4 C3 110.1(3) . .
N1 C4 C5 122.1(3) . .
C3 C4 C5 127.8(3) . .
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 . .
N5 C7 C8 107.8(2) . .
N5 C7 C6 123.4(2) . .
C8 C7 C6 128.8(2) . .
C7 C8 C9 106.4(2) . .
C7 C8 H8 126.8 . .
C9 C8 H8 126.8 . .
N2 C9 C8 109.8(2) . .
N2 C9 C10 122.2(2) . .
C8 C9 C10 128.0(3) . .
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 . .
N6 C12 C13 107.5(2) . .
N6 C12 C11 123.2(3) . .
C13 C12 C11 129.3(3) . .
C12 C13 C14 106.3(2) . .
C12 C13 H13 126.9 . .
C14 C13 H13 126.9 . .
N3 C14 C13 109.9(2) . .
N3 C14 C15 121.4(3) . .
C13 C14 C15 128.7(3) . .
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 . .
N4 B1 N6 108.8(2) . .
N4 B1 N5 110.1(2) . .
N6 B1 N5 109.7(2) . .
N4 B1 H1 109.4 . .
N6 B1 H1 109.4 . .
N5 B1 H1 109.4 . .
C4 N1 N4 106.3(2) . .
C4 N1 Fe1 136.34(19) . .
N4 N1 Fe1 117.18(15) . .
C9 N2 N5 106.5(2) . .
C9 N2 Fe1 136.87(17) . .
N5 N2 Fe1 116.54(15) . .
C14 N3 N6 106.3(2) . .
C14 N3 Fe1 136.20(18) . .
N6 N3 Fe1 117.35(14) . .
C2 N4 N1 109.7(2) . .
C2 N4 B1 131.0(2) . .
N1 N4 B1 119.31(19) . .
C7 N5 N2 109.5(2) . .
C7 N5 B1 130.3(2) . .
N2 N5 B1 120.20(19) . .
C12 N6 N3 110.1(2) . .
C12 N6 B1 130.5(2) . .
N3 N6 B1 119.35(19) . .
N2 Fe1 N2 180.0 . 2_666
N2 Fe1 N3 86.72(8) . .
N2 Fe1 N3 93.28(8) 2_666 .
N2 Fe1 N3 93.28(8) . 2_666
N2 Fe1 N3 86.72(8) 2_666 2_666
N3 Fe1 N3 180.00(11) . 2_666
N2 Fe1 N1 86.84(8) . .
N2 Fe1 N1 93.16(8) 2_666 .
N3 Fe1 N1 87.57(8) . .
N3 Fe1 N1 92.43(8) 2_666 .
N2 Fe1 N1 93.16(8) . 2_666
N2 Fe1 N1 86.84(8) 2_666 2_666
N3 Fe1 N1 92.44(8) . 2_666
N3 Fe1 N1 87.57(8) 2_666 2_666
N1 Fe1 N1 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 1.493(4) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 N4 1.352(3) .
C2 C3 1.372(4) .
C3 C4 1.386(4) .
C3 H3 0.9300 .
C4 N1 1.335(3) .
C4 C5 1.505(4) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.495(4) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 N5 1.347(3) .
C7 C8 1.370(4) .
C8 C9 1.385(4) .
C8 H8 0.9300 .
C9 N2 1.333(3) .
C9 C10 1.499(4) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.496(4) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 N6 1.345(3) .
C12 C13 1.376(4) .
C13 C14 1.387(4) .
C13 H13 0.9300 .
C14 N3 1.336(3) .
C14 C15 1.496(4) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
B1 N4 1.540(4) .
B1 N6 1.542(3) .
B1 N5 1.550(4) .
B1 H1 0.9800 .
N1 N4 1.377(3) .
N1 Fe1 2.144(2) .
N2 N5 1.377(3) .
N2 Fe1 2.136(2) .
N3 N6 1.375(3) .
N3 Fe1 2.141(2) .
Fe1 N2 2.136(2) 2_666
Fe1 N3 2.141(2) 2_666
Fe1 N1 2.144(2) 2_666
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168339839
