#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:47:52 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293122 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/61/7716122.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_7716122
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                   15.0044(8)
_cell_length_b                   15.0044(8)
_cell_length_c                   10.9173(9)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.50
_cell_volume                     2128.5(2)
_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      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            19085
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.071
_diffrn_reflns_theta_max         25.071
_diffrn_reflns_theta_min         1.914
_diffrn_source                   'XALOC Beamline ALBA Cells'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1818 before and 0.0635 after correction.
The Ratio of minimum to maximum transmission is 0.7484.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.398
_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         0.556
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2337
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0629
_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)+(0.1647P)²+0.2697P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2143
_refine_ls_wR_factor_ref         0.2240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2037
_reflns_number_total             2337
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00578c2.cif
_cod_data_source_block           da370_100kcool_0m
_cod_depositor_comments
'Adding full bibliography for 7716118--7716126.cif.'
_cod_original_cell_volume        2128.5(3)
_cod_database_code               7716122
_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   0.995
_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) F6(0.333333) F3(0.333333) B2(0.333333) F4(0.333333)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C1(H1), C4(H4), C11(H11), C12(H12), 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 0.34521(7) 0.0603(4) Uani 1 3 d S T P . .
F1 F 0.63934(19) 0.23530(17) -0.2070(2) 0.0942(7) Uani 1 1 d . . . . .
N2 N 0.57727(19) 0.37060(19) 0.2528(2) 0.0608(7) Uani 1 1 d . . . . .
N3 N 0.5156(2) 0.3365(2) 0.1553(3) 0.0633(7) Uani 1 1 d . . . . .
H3 H 0.503(3) 0.281(4) 0.111(4) 0.095 Uiso 1 1 d . U . . .
N1 N 0.6860(2) 0.4548(2) 0.4444(2) 0.0668(7) Uani 1 1 d . . . . .
F2 F 0.666667 0.333333 -0.0373(4) 0.1091(14) Uani 1 3 d S T P . .
N4 N 0.2890(2) 0.4273(2) -0.0665(3) 0.0735(8) Uani 1 1 d . . . . .
C6 C 0.5693(3) 0.4505(3) 0.2982(3) 0.0668(8) Uani 1 1 d . . . . .
C5 C 0.6331(3) 0.5003(3) 0.4046(3) 0.0703(9) Uani 1 1 d . . . . .
C8 C 0.4671(3) 0.3930(3) 0.1371(3) 0.0673(8) Uani 1 1 d . . . . .
C7 C 0.4998(3) 0.4652(3) 0.2288(3) 0.0715(9) Uani 1 1 d . . . . .
H7 H 0.479223 0.514866 0.242248 0.086 Uiso 1 1 calc R U . . .
C9 C 0.3976(3) 0.3749(3) 0.0356(3) 0.0690(9) Uani 1 1 d . . . . .
C10 C 0.3545(3) 0.4386(3) 0.0229(3) 0.0689(8) Uani 1 1 d . . . . .
H10 H 0.372858 0.492386 0.080736 0.083 Uiso 1 1 calc R U . . .
C13 C 0.2614(3) 0.3505(3) -0.1466(3) 0.0767(9) Uani 1 1 d . . . . .
H13 H 0.213004 0.340792 -0.208589 0.092 Uiso 1 1 calc R U . . .
C1 C 0.7456(3) 0.4945(3) 0.5436(3) 0.0761(9) Uani 1 1 d . . . . .
H1 H 0.783113 0.463240 0.572932 0.091 Uiso 1 1 calc R U . . .
C4 C 0.6397(3) 0.5858(3) 0.4606(4) 0.0826(10) Uani 1 1 d . . . . .
H4 H 0.601970 0.616380 0.429993 0.099 Uiso 1 1 calc R U . . .
C11 C 0.3710(3) 0.2992(3) -0.0519(4) 0.0807(10) Uani 1 1 d . . . . .
H11 H 0.401374 0.256799 -0.049553 0.097 Uiso 1 1 calc R U . . .
C12 C 0.3009(3) 0.2843(3) -0.1426(4) 0.0871(11) Uani 1 1 d . . . . .
H12 H 0.280159 0.230298 -0.200594 0.105 Uiso 1 1 calc R U . . .
C2 C 0.7547(3) 0.5799(3) 0.6054(4) 0.0864(11) Uani 1 1 d . . . . .
H2 H 0.796609 0.605184 0.676438 0.104 Uiso 1 1 calc R U . . .
C3 C 0.7033(3) 0.6268(3) 0.5636(4) 0.0886(11) Uani 1 1 d . . . . .
H3A H 0.710164 0.686219 0.603427 0.106 Uiso 1 1 calc R U . . .
B1 B 0.666667 0.333333 -0.1636(7) 0.086(2) Uani 1 3 d S T P . .
F5 F 0.8063(7) 0.7843(10) 0.8058(10) 0.138(3) Uani 0.3333 1 d D U P . .
F6 F 0.7833(9) 0.8650(9) 0.6437(11) 0.148(4) Uani 0.3333 1 d D U P . .
F3 F 0.9131(9) 0.8303(9) 0.6627(13) 0.168(5) Uani 0.3333 1 d D U P . .
B2 B 0.8456(12) 0.8525(12) 0.7260(14) 0.104(5) Uani 0.3333 1 d D U P . .
F4 F 0.8982(17) 0.9439(16) 0.787(2) 0.304(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 96.12(10) 2_655 3_665 ?
N2 Fe1 N2 96.12(10) 2_655 . ?
N2 Fe1 N2 96.12(10) 3_665 . ?
N2 Fe1 N1 80.13(11) 2_655 2_655 ?
N2 Fe1 N1 80.13(11) . . ?
N2 Fe1 N1 172.87(10) 2_655 . ?
N2 Fe1 N1 172.87(10) 3_665 2_655 ?
N2 Fe1 N1 90.33(11) 2_655 3_665 ?
N2 Fe1 N1 90.33(11) 3_665 . ?
N2 Fe1 N1 80.13(11) 3_665 3_665 ?
N2 Fe1 N1 172.87(11) . 3_665 ?
N2 Fe1 N1 90.33(11) . 2_655 ?
N1 Fe1 N1 93.78(11) 3_665 . ?
N1 Fe1 N1 93.78(11) 3_665 2_655 ?
N1 Fe1 N1 93.78(11) 2_655 . ?
N3 N2 Fe1 137.8(2) . . ?
N3 N2 C6 106.2(3) . . ?
C6 N2 Fe1 115.9(2) . . ?
N2 N3 H3 125(3) . . ?
N2 N3 C8 110.9(3) . . ?
C8 N3 H3 124(3) . . ?
C5 N1 Fe1 115.5(2) . . ?
C1 N1 Fe1 126.8(3) . . ?
C1 N1 C5 117.7(3) . . ?
C10 N4 C13 118.6(3) . . ?
N2 C6 C5 114.8(3) . . ?
N2 C6 C7 110.2(3) . . ?
C7 C6 C5 135.0(3) . . ?
N1 C5 C6 113.5(3) . . ?
N1 C5 C4 122.7(3) . . ?
C4 C5 C6 123.7(3) . . ?
N3 C8 C9 123.1(3) . . ?
C7 C8 N3 106.8(3) . . ?
C7 C8 C9 130.1(3) . . ?
C6 C7 H7 127.1 . . ?
C8 C7 C6 105.8(3) . . ?
C8 C7 H7 127.1 . . ?
C10 C9 C8 118.8(3) . . ?
C11 C9 C8 124.5(3) . . ?
C11 C9 C10 116.7(3) . . ?
N4 C10 C9 123.1(3) . . ?
N4 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
N4 C13 H13 118.7 . . ?
N4 C13 C12 122.5(4) . . ?
C12 C13 H13 118.7 . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.4(4) . . ?
C2 C1 H1 118.8 . . ?
C5 C4 H4 120.7 . . ?
C5 C4 C3 118.7(4) . . ?
C3 C4 H4 120.7 . . ?
C9 C11 H11 119.6 . . ?
C12 C11 C9 120.8(3) . . ?
C12 C11 H11 119.6 . . ?
C13 C12 H12 121.0 . . ?
C11 C12 C13 118.1(4) . . ?
C11 C12 H12 121.0 . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.2 . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 H3A 120.6 . . ?
F1 B1 F1 109.1(3) 2_655 3_665 ?
F1 B1 F1 109.1(3) . 3_665 ?
F1 B1 F1 109.1(3) . 2_655 ?
F2 B1 F1 109.8(3) . . ?
F2 B1 F1 109.8(3) . 3_665 ?
F2 B1 F1 109.8(3) . 2_655 ?
F5 B2 F6 119.6(14) . . ?
F5 B2 F3 104.5(13) . . ?
F5 B2 F4 106.4(16) . . ?
F6 B2 F3 109.5(12) . . ?
F4 B2 F6 105.8(15) . . ?
F4 B2 F3 110.9(15) . . ?
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 1.970(3) 2_655 ?
Fe1 N2 1.970(3) 3_665 ?
Fe1 N2 1.970(3) . ?
Fe1 N1 2.012(3) 3_665 ?
Fe1 N1 2.012(3) . ?
Fe1 N1 2.012(3) 2_655 ?
F1 B1 1.398(4) . ?
N2 N3 1.334(4) . ?
N2 C6 1.357(4) . ?
N3 H3 0.90(5) . ?
N3 C8 1.379(4) . ?
N1 C5 1.351(5) . ?
N1 C1 1.341(4) . ?
F2 B1 1.379(9) . ?
N4 C10 1.335(4) . ?
N4 C13 1.336(5) . ?
C6 C5 1.453(5) . ?
C6 C7 1.392(5) . ?
C5 C4 1.379(5) . ?
C8 C7 1.373(5) . ?
C8 C9 1.451(5) . ?
C7 H7 0.9500 . ?
C9 C10 1.403(5) . ?
C9 C11 1.382(5) . ?
C10 H10 0.9500 . ?
C13 H13 0.9500 . ?
C13 C12 1.387(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.394(5) . ?
C4 H4 0.9500 . ?
C4 C3 1.402(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(6) . ?
C12 H12 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.356(6) . ?
C3 H3A 0.9500 . ?
F5 B2 1.246(15) . ?
F6 B2 1.376(14) . ?
F3 B2 1.397(15) . ?
B2 F4 1.365(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 N3 C8 176.7(2) . . . . ?
Fe1 N2 C6 C5 3.4(4) . . . . ?
Fe1 N2 C6 C7 -176.7(2) . . . . ?
Fe1 N1 C5 C6 1.6(4) . . . . ?
Fe1 N1 C5 C4 -178.5(3) . . . . ?
Fe1 N1 C1 C2 179.3(3) . . . . ?
N2 N3 C8 C7 -0.6(4) . . . . ?
N2 N3 C8 C9 178.2(3) . . . . ?
N2 C6 C5 N1 -3.3(4) . . . . ?
N2 C6 C5 C4 176.8(3) . . . . ?
N2 C6 C7 C8 -1.5(4) . . . . ?
N3 N2 C6 C5 -178.8(3) . . . . ?
N3 N2 C6 C7 1.1(4) . . . . ?
N3 C8 C7 C6 1.3(4) . . . . ?
N3 C8 C9 C10 -178.1(3) . . . . ?
N3 C8 C9 C11 1.1(6) . . . . ?
N1 C5 C4 C3 -0.5(6) . . . . ?
N1 C1 C2 C3 -1.2(6) . . . . ?
N4 C13 C12 C11 0.1(6) . . . . ?
C6 N2 N3 C8 -0.3(3) . . . . ?
C6 C5 C4 C3 179.4(4) . . . . ?
C5 N1 C1 C2 -0.2(5) . . . . ?
C5 C6 C7 C8 178.4(4) . . . . ?
C5 C4 C3 C2 -0.9(6) . . . . ?
C8 C9 C10 N4 -179.2(3) . . . . ?
C8 C9 C11 C12 177.2(4) . . . . ?
C7 C6 C5 N1 176.9(4) . . . . ?
C7 C6 C5 C4 -3.0(6) . . . . ?
C7 C8 C9 C10 0.5(6) . . . . ?
C7 C8 C9 C11 179.7(4) . . . . ?
C9 C8 C7 C6 -177.5(3) . . . . ?
C9 C11 C12 C13 2.8(6) . . . . ?
C10 N4 C13 C12 -2.1(6) . . . . ?
C10 C9 C11 C12 -3.5(6) . . . . ?
C13 N4 C10 C9 1.3(5) . . . . ?
C1 N1 C5 C6 -178.9(3) . . . . ?
C1 N1 C5 C4 1.1(5) . . . . ?
C1 C2 C3 C4 1.8(7) . . . . ?
C11 C9 C10 N4 1.5(5) . . . . ?
