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#$Date: 2024-07-05 19:47:52 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293122 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/61/7716121.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_7716121
loop_
_publ_author_name
'Nielsen, Hannah H.'
'Vilariño, Pol'
'Rodríguez, Gemma'
'Trepard, Florian'
'Roubeau, Olivier'
'Aromí, Guillem'
'Aguilà, David'
_publ_section_title
;
 Self-assembly of a supramolecular spin-crossover tetrahedron.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9792
_journal_page_last               9797
_journal_paper_doi               10.1039/d4dt00578c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C39 H30 Fe N12, 2(B F4)'
_chemical_formula_sum            'C39 H30 B2 F8 Fe N12'
_chemical_formula_weight         896.22
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-06 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.1758(5)
_cell_length_b                   15.1758(5)
_cell_length_c                   11.1731(5)
_cell_measurement_reflns_used    7266
_cell_measurement_temperature    300
_cell_measurement_theta_max      24.21
_cell_measurement_theta_min      2.46
_cell_volume                     2228.47(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  MD2M-Maatel
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.72931
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.478
_diffrn_reflns_theta_max         24.478
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'XALOC Beamline ALBA Cells'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1716 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.8695.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1867P)²+0.1854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2306
_refine_ls_wR_factor_ref         0.2405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2009
_reflns_number_total             2293
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00578c2.cif
_cod_data_source_block           da370_300kcooling_0m
_cod_depositor_comments
'Adding full bibliography for 7716118--7716126.cif.'
_cod_original_cell_volume        2228.47(18)
_cod_database_code               7716121
_shelx_shelxl_version_number     2018/3
_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_max   0.996
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups
2. Restrained distances
 B2-F3
 1.4 with sigma of 0.02
 B2-F4
 1.4 with sigma of 0.02
 B2-F5
 1.4 with sigma of 0.02
 B2-F6
 1.4 with sigma of 0.02
 F3-F4
 2.25 with sigma of 0.04
 F3-F5
 2.25 with sigma of 0.04
 F3-F6
 2.25 with sigma of 0.04
 F4-F5
 2.25 with sigma of 0.04
 F4-F6
 2.25 with sigma of 0.04
 F5-F6
 2.25 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(B2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Fixed Sof: F5(0.333333) B2(0.333333) F4(0.333333) F3(0.333333) F6(0.333333)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C1(H1), C11(H11), C12(H12), C4(H4), C2(H2), C3(H3A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.666667 0.333333 0.15916(7) 0.0881(4) Uani 1 3 d S T P . .
N3 N 0.8296(2) 0.4906(2) 0.3496(3) 0.0954(8) Uani 1 1 d . . . . .
H3 H 0.776(4) 0.501(4) 0.390(4) 0.143 Uiso 1 1 d . U . . .
N2 N 0.8016(2) 0.4300(2) 0.2526(3) 0.0909(7) Uani 1 1 d . . . . .
N1 N 0.7844(3) 0.3258(2) 0.0571(3) 0.1041(9) Uani 1 1 d . . . . .
F1 F 0.5958(3) 0.3569(3) 0.7104(3) 0.1785(14) Uani 1 1 d . . . . .
N4 N 1.1406(3) 0.7150(3) 0.5679(3) 0.1136(10) Uani 1 1 d . . . . .
F2 F 0.666667 0.333333 0.5476(6) 0.207(3) Uani 1 3 d S T P . .
C6 C 0.8877(3) 0.4385(3) 0.2096(3) 0.0980(10) Uani 1 1 d . . . . .
C8 C 0.9329(3) 0.5381(3) 0.3675(3) 0.0974(10) Uani 1 1 d . . . . .
C7 C 0.9710(3) 0.5054(3) 0.2768(3) 0.1041(11) Uani 1 1 d . . . . .
H7 H 1.038693 0.524316 0.263443 0.125 Uiso 1 1 calc R U . . .
C9 C 0.9822(3) 0.6060(3) 0.4654(4) 0.1017(10) Uani 1 1 d . . . . .
C5 C 0.8776(3) 0.3767(3) 0.1039(3) 0.1048(10) Uani 1 1 d . . . . .
C10 C 1.0876(3) 0.6510(3) 0.4797(4) 0.1029(10) Uani 1 1 d . . . . .
H10 H 1.123147 0.635298 0.423949 0.123 Uiso 1 1 calc R U . . .
C13 C 1.0891(3) 0.7392(3) 0.6475(4) 0.1188(13) Uani 1 1 d . . . . .
H13 H 1.125265 0.786002 0.707549 0.143 Uiso 1 1 calc R U . . .
B00F B 0.666667 0.333333 0.6671(9) 0.129(3) Uani 1 3 d S T P . .
C1 C 0.7718(4) 0.2697(4) -0.0405(4) 0.1266(14) Uani 1 1 d . . . . .
H1 H 0.707128 0.234189 -0.073890 0.152 Uiso 1 1 calc R U . . .
C11 C 0.9308(3) 0.6280(4) 0.5535(4) 0.1248(14) Uani 1 1 d . . . . .
H11 H 0.860141 0.596041 0.551952 0.150 Uiso 1 1 calc R U . . .
C12 C 0.9845(4) 0.6970(4) 0.6429(4) 0.1334(16) Uani 1 1 d . . . . .
H12 H 0.950988 0.714774 0.699203 0.160 Uiso 1 1 calc R U . . .
C4 C 0.9592(4) 0.3730(4) 0.0555(4) 0.1308(15) Uani 1 1 d . . . . .
H4 H 1.023784 0.409763 0.088994 0.157 Uiso 1 1 calc R U . . .
C2 C 0.8482(6) 0.2615(5) -0.0942(5) 0.1507(19) Uani 1 1 d . . . . .
H2 H 0.835800 0.221764 -0.162315 0.181 Uiso 1 1 calc R U . . .
C3 C 0.9418(6) 0.3122(5) -0.0460(6) 0.154(2) Uani 1 1 d . . . . .
H3A H 0.994909 0.306915 -0.079966 0.185 Uiso 1 1 calc R U . . .
F5 F 0.9798(13) 0.2098(13) -0.2973(13) 0.239(7) Uani 0.3333 1 d D U P . .
B2 B 1.0061(14) 0.1601(15) -0.2335(16) 0.137(5) Uani 0.3333 1 d D U P . .
F4 F 1.0788(14) 0.2096(18) -0.1511(17) 0.300(10) Uani 0.3333 1 d D U P . .
F3 F 0.9225(14) 0.0957(13) -0.1705(19) 0.257(7) Uani 0.3333 1 d D U P . .
F6 F 1.0519(19) 0.1197(17) -0.296(2) 0.327(11) Uani 0.3333 1 d D U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0017 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0065 0.0035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0186 0.0109 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3512 0.8902 '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
_geom_angle_publ_flag
N2 Fe1 N2 97.52(10) . 3_665 ?
N2 Fe1 N2 97.52(10) . 2_655 ?
N2 Fe1 N2 97.52(10) 3_665 2_655 ?
N2 Fe1 N1 75.97(12) 3_665 3_665 ?
N2 Fe1 N1 75.97(12) 2_655 2_655 ?
N2 Fe1 N1 92.47(11) . 2_655 ?
N2 Fe1 N1 92.48(11) 2_655 3_665 ?
N2 Fe1 N1 75.97(12) . . ?
N2 Fe1 N1 168.75(11) 3_665 2_655 ?
N2 Fe1 N1 92.47(11) 3_665 . ?
N2 Fe1 N1 168.75(11) 2_655 . ?
N2 Fe1 N1 168.75(11) . 3_665 ?
N1 Fe1 N1 94.95(12) . 2_655 ?
N1 Fe1 N1 94.95(12) 3_665 2_655 ?
N1 Fe1 N1 94.95(12) . 3_665 ?
N2 N3 H3 118(3) . . ?
N2 N3 C8 111.3(3) . . ?
C8 N3 H3 130(3) . . ?
N3 N2 Fe1 137.8(2) . . ?
C6 N2 Fe1 116.9(2) . . ?
C6 N2 N3 105.3(3) . . ?
C5 N1 Fe1 115.2(2) . . ?
C5 N1 C1 117.5(4) . . ?
C1 N1 Fe1 127.1(3) . . ?
C10 N4 C13 117.7(4) . . ?
N2 C6 C7 111.6(3) . . ?
N2 C6 C5 116.3(3) . . ?
C7 C6 C5 132.1(3) . . ?
N3 C8 C7 106.1(3) . . ?
N3 C8 C9 122.6(3) . . ?
C7 C8 C9 131.3(3) . . ?
C6 C7 H7 127.2 . . ?
C8 C7 C6 105.6(3) . . ?
C8 C7 H7 127.2 . . ?
C10 C9 C8 119.8(4) . . ?
C11 C9 C8 123.9(3) . . ?
C11 C9 C10 116.2(4) . . ?
N1 C5 C6 115.3(3) . . ?
N1 C5 C4 122.5(4) . . ?
C4 C5 C6 122.2(4) . . ?
N4 C10 C9 124.4(4) . . ?
N4 C10 H10 117.8 . . ?
C9 C10 H10 117.8 . . ?
N4 C13 H13 118.8 . . ?
N4 C13 C12 122.3(4) . . ?
C12 C13 H13 118.8 . . ?
F1 B00F F1 108.4(5) 3_665 . ?
F1 B00F F1 108.4(5) 2_655 . ?
F1 B00F F1 108.4(5) 2_655 3_665 ?
F2 B00F F1 110.5(4) . 3_665 ?
F2 B00F F1 110.5(4) . . ?
F2 B00F F1 110.5(4) . 2_655 ?
N1 C1 H1 118.0 . . ?
N1 C1 C2 124.0(5) . . ?
C2 C1 H1 118.0 . . ?
C9 C11 H11 119.9 . . ?
C12 C11 C9 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C13 C12 H12 120.5 . . ?
C11 C12 C13 119.0(4) . . ?
C11 C12 H12 120.5 . . ?
C5 C4 H4 121.1 . . ?
C5 C4 C3 117.8(5) . . ?
C3 C4 H4 121.1 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.3(5) . . ?
C3 C2 H2 120.9 . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 C4 119.9(5) . . ?
C2 C3 H3A 120.0 . . ?
F5 B2 F4 118.6(19) . . ?
F5 B2 F3 105.6(15) . . ?
F5 B2 F6 112.3(17) . . ?
F4 B2 F3 105.1(16) . . ?
F6 B2 F4 98.3(16) . . ?
F6 B2 F3 117.3(18) . . ?
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
Fe1 N2 2.105(3) . ?
Fe1 N2 2.105(3) 3_665 ?
Fe1 N2 2.105(3) 2_655 ?
Fe1 N1 2.170(3) . ?
Fe1 N1 2.170(3) 2_655 ?
Fe1 N1 2.170(3) 3_665 ?
N3 H3 1.02(5) . ?
N3 N2 1.345(4) . ?
N3 C8 1.374(4) . ?
N2 C6 1.336(4) . ?
N1 C5 1.333(5) . ?
N1 C1 1.337(5) . ?
F1 B00F 1.380(5) . ?
N4 C10 1.334(5) . ?
N4 C13 1.350(6) . ?
F2 B00F 1.335(11) . ?
C6 C7 1.381(5) . ?
C6 C5 1.468(5) . ?
C8 C7 1.377(5) . ?
C8 C9 1.431(5) . ?
C7 H7 0.9300 . ?
C9 C10 1.400(5) . ?
C9 C11 1.396(6) . ?
C5 C4 1.378(6) . ?
C10 H10 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.384(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.365(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.381(6) . ?
C12 H12 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.401(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.344(9) . ?
C3 H3A 0.9300 . ?
F5 B2 1.239(16) . ?
B2 F4 1.342(16) . ?
B2 F3 1.348(16) . ?
B2 F6 1.330(16) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C6 C7 178.7(2) . . . . ?
Fe1 N2 C6 C5 -1.9(4) . . . . ?
Fe1 N1 C5 C6 -6.3(4) . . . . ?
Fe1 N1 C5 C4 174.7(4) . . . . ?
Fe1 N1 C1 C2 -173.8(4) . . . . ?
N3 N2 C6 C7 -1.0(4) . . . . ?
N3 N2 C6 C5 178.3(3) . . . . ?
N3 C8 C7 C6 -0.7(4) . . . . ?
N3 C8 C9 C10 179.2(3) . . . . ?
N3 C8 C9 C11 2.2(6) . . . . ?
N2 N3 C8 C7 0.1(4) . . . . ?
N2 N3 C8 C9 -179.4(3) . . . . ?
N2 C6 C7 C8 1.1(4) . . . . ?
N2 C6 C5 N1 5.5(5) . . . . ?
N2 C6 C5 C4 -175.5(4) . . . . ?
N1 C5 C4 C3 -0.7(7) . . . . ?
N1 C1 C2 C3 0.3(9) . . . . ?
N4 C13 C12 C11 -0.4(8) . . . . ?
C6 C5 C4 C3 -179.6(4) . . . . ?
C8 N3 N2 Fe1 -179.1(2) . . . . ?
C8 N3 N2 C6 0.5(4) . . . . ?
C8 C9 C10 N4 -179.8(3) . . . . ?
C8 C9 C11 C12 -178.0(4) . . . . ?
C7 C6 C5 N1 -175.3(4) . . . . ?
C7 C6 C5 C4 3.7(7) . . . . ?
C7 C8 C9 C10 -0.2(7) . . . . ?
C7 C8 C9 C11 -177.2(4) . . . . ?
C9 C8 C7 C6 178.7(4) . . . . ?
C9 C11 C12 C13 -3.7(8) . . . . ?
C5 N1 C1 C2 0.3(7) . . . . ?
C5 C6 C7 C8 -178.1(4) . . . . ?
C5 C4 C3 C2 1.3(9) . . . . ?
C10 N4 C13 C12 2.7(7) . . . . ?
C10 C9 C11 C12 5.0(7) . . . . ?
C13 N4 C10 C9 -1.2(6) . . . . ?
C1 N1 C5 C6 178.9(3) . . . . ?
C1 N1 C5 C4 -0.1(6) . . . . ?
C1 C2 C3 C4 -1.1(10) . . . . ?
C11 C9 C10 N4 -2.6(6) . . . . ?
