#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:47:52 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293122 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/61/7716118.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_7716118
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             2024-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-22 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                   15.005(2)
_cell_length_b                   15.005(2)
_cell_length_c                   10.863(2)
_cell_measurement_reflns_used    41647
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.8
_cell_measurement_theta_min      3.22
_cell_volume                     2118.1(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  MD2M-Maatel
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41793
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         34.196
_diffrn_reflns_theta_min         1.608
_diffrn_source                   'XALOC Beamline ALBA Cells'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.916
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4790
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0826
_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)+(0.1917P)²+0.3016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2507
_refine_ls_wR_factor_ref         0.2629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4492
_reflns_number_total             4790
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00578c2.cif
_cod_data_source_block           gr5
_cod_depositor_comments
'Adding full bibliography for 7716118--7716126.cif.'
_cod_original_cell_volume        2118.1(7)
_cod_database_code               7716118
_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   0.973
_shelx_estimated_absorpt_t_min   0.973
_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
 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
 B2-F5 \\sim B2-F4 \\sim B2-F3 \\sim B2-F6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F3) \\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) F4(0.333333) F3(0.333333) F6(0.333333) B2(0.333333)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C11(H11), C10(H10), C1(H1), C4(H4), 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 0.333333 0.666667 0.65418(4) 0.04376(18) Uani 1 3 d S T P . .
F1 F 0.36103(15) 0.59615(14) 1.20492(17) 0.0758(5) Uani 1 1 d . . . . .
N3 N 0.33702(12) 0.51564(12) 0.84480(15) 0.0468(3) Uani 1 1 d . . . . .
H3 H 0.283(3) 0.508(3) 0.883(3) 0.070 Uiso 1 1 d . U . . .
N2 N 0.37106(12) 0.57781(12) 0.74699(15) 0.0454(3) Uani 1 1 d . . . . .
F2 F 0.333333 0.666667 1.0336(3) 0.0876(9) Uani 1 3 d S T P . .
N1 N 0.45427(13) 0.68629(13) 0.55466(16) 0.0499(3) Uani 1 1 d . . . . .
N4 N 0.42696(14) 0.28825(14) 1.06657(18) 0.0547(4) Uani 1 1 d . . . . .
C6 C 0.45041(15) 0.57006(15) 0.70123(18) 0.0503(4) Uani 1 1 d . . . . .
C5 C 0.50024(16) 0.63348(16) 0.59397(19) 0.0529(4) Uani 1 1 d . . . . .
C7 C 0.46634(17) 0.50046(17) 0.76989(19) 0.0545(4) Uani 1 1 d . . . . .
H7 H 0.516250 0.480208 0.756327 0.065 Uiso 1 1 calc R U . . .
C8 C 0.39293(15) 0.46770(15) 0.86215(19) 0.0499(4) Uani 1 1 d . . . . .
C9 C 0.37489(16) 0.39720(16) 0.96368(19) 0.0518(4) Uani 1 1 d . . . . .
C13 C 0.29880(18) 0.3714(2) 1.0530(2) 0.0615(5) Uani 1 1 d . . . . .
H13 H 0.256632 0.401984 1.051185 0.074 Uiso 1 1 calc R U . . .
C11 C 0.35045(18) 0.26059(18) 1.1465(2) 0.0588(5) Uani 1 1 d . . . . .
H11 H 0.340120 0.211086 1.207683 0.071 Uiso 1 1 calc R U . . .
C10 C 0.43829(15) 0.35400(15) 0.9759(2) 0.0523(4) Uani 1 1 d . . . . .
H10 H 0.491725 0.371979 0.917436 0.063 Uiso 1 1 calc R U . . .
C1 C 0.49365(18) 0.74600(18) 0.4536(2) 0.0578(4) Uani 1 1 d . . . . .
H1 H 0.461807 0.782792 0.423658 0.069 Uiso 1 1 calc R U . . .
C4 C 0.58592(19) 0.6404(2) 0.5370(2) 0.0634(5) Uani 1 1 d . . . . .
H4 H 0.616526 0.602600 0.567508 0.076 Uiso 1 1 calc R U . . .
C12 C 0.2849(2) 0.3011(2) 1.1443(2) 0.0654(5) Uani 1 1 d . . . . .
H12 H 0.231930 0.280989 1.203870 0.078 Uiso 1 1 calc R U . . .
C2 C 0.5790(2) 0.7554(2) 0.3920(2) 0.0659(5) Uani 1 1 d . . . . .
H2 H 0.604409 0.797610 0.320813 0.079 Uiso 1 1 calc R U . . .
C3 C 0.6266(2) 0.7035(2) 0.4342(3) 0.0701(6) Uani 1 1 d . . . . .
H3A H 0.686063 0.710476 0.394204 0.084 Uiso 1 1 calc R U . . .
B1 B 0.333333 0.666667 1.1608(5) 0.0641(10) Uani 1 3 d S T P . .
F5 F 0.8690(7) 0.7923(7) 0.3544(9) 0.120(3) Uani 0.3333 1 d D U P . .
F4 F 0.7788(9) 0.8040(7) 0.1949(8) 0.130(3) Uani 0.3333 1 d D U P . .
F3 F 0.8270(7) 0.9125(8) 0.3484(11) 0.143(4) Uani 0.3333 1 d D U P . .
F6 F 0.9495(13) 0.9106(16) 0.2415(19) 0.270(10) Uani 0.3333 1 d D U P . .
B2 B 0.8511(9) 0.8494(10) 0.2790(12) 0.101(4) 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'
F F 0.0186 0.0109 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3512 0.8903 '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'
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 96.08(6) 3_565 2_665 ?
N2 Fe1 N2 96.08(6) 3_565 . ?
N2 Fe1 N2 96.08(6) 2_665 . ?
N2 Fe1 N1 172.81(6) 2_665 3_565 ?
N2 Fe1 N1 80.20(7) . . ?
N2 Fe1 N1 172.81(6) 3_565 . ?
N2 Fe1 N1 90.45(7) . 3_565 ?
N2 Fe1 N1 90.45(7) 3_565 2_665 ?
N2 Fe1 N1 90.45(7) 2_665 . ?
N2 Fe1 N1 80.20(7) 2_665 2_665 ?
N2 Fe1 N1 172.81(7) . 2_665 ?
N2 Fe1 N1 80.20(7) 3_565 3_565 ?
N1 Fe1 N1 93.62(7) 2_665 . ?
N1 Fe1 N1 93.63(7) 3_565 . ?
N1 Fe1 N1 93.62(7) 2_665 3_565 ?
N2 N3 H3 119(2) . . ?
N2 N3 C8 110.92(15) . . ?
C8 N3 H3 130(2) . . ?
N3 N2 Fe1 137.91(12) . . ?
N3 N2 C6 106.20(15) . . ?
C6 N2 Fe1 115.81(13) . . ?
C5 N1 Fe1 115.65(13) . . ?
C1 N1 Fe1 126.82(15) . . ?
C1 N1 C5 117.53(18) . . ?
C11 N4 C10 118.72(18) . . ?
N2 C6 C5 115.27(17) . . ?
N2 C6 C7 110.86(17) . . ?
C7 C6 C5 133.87(18) . . ?
N1 C5 C6 112.97(17) . . ?
N1 C5 C4 122.8(2) . . ?
C4 C5 C6 124.2(2) . . ?
C6 C7 H7 127.8 . . ?
C8 C7 C6 104.39(16) . . ?
C8 C7 H7 127.8 . . ?
N3 C8 C7 107.62(17) . . ?
N3 C8 C9 123.20(17) . . ?
C7 C8 C9 129.17(17) . . ?
C13 C9 C8 123.82(17) . . ?
C13 C9 C10 117.12(19) . . ?
C10 C9 C8 119.04(18) . . ?
C9 C13 H13 120.0 . . ?
C12 C13 C9 119.9(2) . . ?
C12 C13 H13 120.0 . . ?
N4 C11 H11 118.6 . . ?
N4 C11 C12 122.8(2) . . ?
C12 C11 H11 118.6 . . ?
N4 C10 C9 122.94(19) . . ?
N4 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.3(2) . . ?
C2 C1 H1 118.9 . . ?
C5 C4 H4 120.5 . . ?
C5 C4 C3 119.0(2) . . ?
C3 C4 H4 120.5 . . ?
C13 C12 C11 118.4(2) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.8(2) . . ?
C3 C2 H2 120.1 . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 C4 118.6(2) . . ?
C2 C3 H3A 120.7 . . ?
F1 B1 F1 108.9(2) 2_665 . ?
F1 B1 F1 108.9(2) 3_565 . ?
F1 B1 F1 108.9(2) 3_565 2_665 ?
F2 B1 F1 110.0(2) . . ?
F2 B1 F1 110.0(2) . 3_565 ?
F2 B1 F1 110.0(2) . 2_665 ?
F5 B2 F4 118.7(12) . . ?
F5 B2 F3 108.4(10) . . ?
F5 B2 F6 97.0(13) . . ?
F4 B2 F3 107.5(10) . . ?
F4 B2 F6 118.6(14) . . ?
F6 B2 F3 105.5(13) . . ?
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 1.9671(15) 3_565 ?
Fe1 N2 1.9671(16) 2_665 ?
Fe1 N2 1.9671(15) . ?
Fe1 N1 2.0035(17) 3_565 ?
Fe1 N1 2.0035(17) . ?
Fe1 N1 2.0035(17) 2_665 ?
F1 B1 1.401(2) . ?
N3 H3 0.86(4) . ?
N3 N2 1.335(2) . ?
N3 C8 1.364(2) . ?
N2 C6 1.348(2) . ?
F2 B1 1.381(6) . ?
N1 C5 1.354(3) . ?
N1 C1 1.352(3) . ?
N4 C11 1.329(3) . ?
N4 C10 1.344(3) . ?
C6 C5 1.453(3) . ?
C6 C7 1.398(3) . ?
C5 C4 1.383(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.385(3) . ?
C8 C9 1.457(3) . ?
C9 C13 1.398(3) . ?
C9 C10 1.400(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(3) . ?
C10 H10 0.9500 . ?
C1 H1 0.9500 . ?
C1 C2 1.389(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.392(4) . ?
C12 H12 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.372(4) . ?
C3 H3A 0.9500 . ?
F5 B2 1.308(11) . ?
F4 B2 1.317(12) . ?
F3 B2 1.393(12) . ?
F6 B2 1.353(13) . ?
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 C5 3.5(2) . . . . ?
Fe1 N2 C6 C7 -176.40(14) . . . . ?
Fe1 N1 C5 C6 1.2(2) . . . . ?
Fe1 N1 C5 C4 -178.58(19) . . . . ?
Fe1 N1 C1 C2 179.10(19) . . . . ?
N3 N2 C6 C5 -179.17(17) . . . . ?
N3 N2 C6 C7 0.9(2) . . . . ?
N3 C8 C9 C13 0.2(3) . . . . ?
N3 C8 C9 C10 -178.15(19) . . . . ?
N2 N3 C8 C7 -0.4(2) . . . . ?
N2 N3 C8 C9 178.46(18) . . . . ?
N2 C6 C5 N1 -3.1(3) . . . . ?
N2 C6 C5 C4 176.8(2) . . . . ?
N2 C6 C7 C8 -1.2(2) . . . . ?
N1 C5 C4 C3 -0.5(4) . . . . ?
N1 C1 C2 C3 -0.5(4) . . . . ?
N4 C11 C12 C13 1.5(4) . . . . ?
C6 C5 C4 C3 179.7(2) . . . . ?
C6 C7 C8 N3 0.9(2) . . . . ?
C6 C7 C8 C9 -177.8(2) . . . . ?
C5 N1 C1 C2 -1.0(3) . . . . ?
C5 C6 C7 C8 179.0(2) . . . . ?
C5 C4 C3 C2 -1.0(4) . . . . ?
C7 C6 C5 N1 176.8(2) . . . . ?
C7 C6 C5 C4 -3.4(4) . . . . ?
C7 C8 C9 C13 178.8(2) . . . . ?
C7 C8 C9 C10 0.5(3) . . . . ?
C8 N3 N2 Fe1 176.11(15) . . . . ?
C8 N3 N2 C6 -0.3(2) . . . . ?
C8 C9 C13 C12 178.0(2) . . . . ?
C8 C9 C10 N4 -179.90(19) . . . . ?
C9 C13 C12 C11 2.2(4) . . . . ?
C13 C9 C10 N4 1.7(3) . . . . ?
C11 N4 C10 C9 1.9(3) . . . . ?
C10 N4 C11 C12 -3.6(4) . . . . ?
C10 C9 C13 C12 -3.7(4) . . . . ?
C1 N1 C5 C6 -178.63(19) . . . . ?
C1 N1 C5 C4 1.5(3) . . . . ?
C1 C2 C3 C4 1.5(4) . . . . ?
