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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/7/71/61/7716120.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_7716120
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                   15.1790(4)
_cell_length_b                   15.1790(4)
_cell_length_c                   11.1228(5)
_cell_measurement_reflns_used    5099
_cell_measurement_temperature    300
_cell_measurement_theta_max      22.75
_cell_measurement_theta_min      2.46
_cell_volume                     2219.38(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.077
_diffrn_reflns_theta_max         22.077
_diffrn_reflns_theta_min         1.879
_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    0.442
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1801 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.7714.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_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         0.416
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         1719
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0705
_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)+(0.1952P)²+0.0700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.2376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1516
_reflns_number_total             1719
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00578c2.cif
_cod_data_source_block           da370_300heating_0m
_cod_depositor_comments
'Adding full bibliography for 7716118--7716126.cif.'
_cod_original_cell_volume        2219.38(15)
_cod_database_code               7716120
_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) F3(0.333333) F4(0.333333) F6(0.333333)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C11(H11), C10(H10), C1(H1), 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 0.333333 0.666667 0.84191(8) 0.1018(6) Uani 1 3 d S T P . .
N2 N 0.4299(2) 0.6282(2) 0.7476(3) 0.1039(10) Uani 1 1 d . . . . .
N3 N 0.4908(3) 0.6612(3) 0.6513(3) 0.1093(10) Uani 1 1 d . . . . .
H3 H 0.507(4) 0.728(5) 0.611(5) 0.164 Uiso 1 1 d . U . . .
N1 N 0.3249(3) 0.5412(3) 0.9435(3) 0.1175(11) Uani 1 1 d . . . . .
F2 F 0.4053(3) 0.6441(4) 0.2926(4) 0.1922(16) Uani 1 1 d . . . . .
F1 F 0.333333 0.666667 0.4535(6) 0.216(3) Uani 1 3 d S T P . .
C6 C 0.4377(3) 0.5505(3) 0.7905(4) 0.1130(13) Uani 1 1 d . . . . .
N4 N 0.7152(3) 0.5748(3) 0.4327(4) 0.1278(13) Uani 1 1 d . . . . .
C8 C 0.5382(3) 0.6051(3) 0.6329(4) 0.1107(12) Uani 1 1 d . . . . .
C9 C 0.6059(3) 0.6238(3) 0.5347(4) 0.1151(13) Uani 1 1 d . . . . .
C5 C 0.3757(4) 0.4991(3) 0.8970(4) 0.1182(13) Uani 1 1 d . . . . .
C7 C 0.5046(4) 0.5340(4) 0.7241(4) 0.1189(14) Uani 1 1 d . . . . .
H7 H 0.523304 0.485157 0.737794 0.143 Uiso 1 1 calc R U . . .
C13 C 0.7394(4) 0.6505(4) 0.3519(5) 0.1343(16) Uani 1 1 d . . . . .
H13 H 0.785958 0.660935 0.291457 0.161 Uiso 1 1 calc R U . . .
C11 C 0.6286(5) 0.6971(4) 0.4472(5) 0.1403(17) Uani 1 1 d . . . . .
H11 H 0.597269 0.736375 0.449634 0.168 Uiso 1 1 calc R U . . .
C10 C 0.6514(3) 0.5641(3) 0.5202(4) 0.1158(13) Uani 1 1 d . . . . .
H10 H 0.635679 0.512862 0.576338 0.139 Uiso 1 1 calc R U . . .
B1 B 0.333333 0.666667 0.3379(9) 0.139(4) Uani 1 3 d S T P . .
C1 C 0.2698(4) 0.4979(4) 1.0419(5) 0.1416(18) Uani 1 1 d . . . . .
H1 H 0.235205 0.527659 1.076484 0.170 Uiso 1 1 calc R U . . .
C12 C 0.6970(5) 0.7127(4) 0.3565(5) 0.154(2) Uani 1 1 d . . . . .
H12 H 0.714217 0.763823 0.299857 0.185 Uiso 1 1 calc R U . . .
C4 C 0.3710(5) 0.4130(4) 0.9462(5) 0.1482(18) Uani 1 1 d . . . . .
H4 H 0.407509 0.384765 0.912981 0.178 Uiso 1 1 calc R U . . .
C2 C 0.2608(6) 0.4136(6) 1.0946(6) 0.167(2) Uani 1 1 d . . . . .
H2 H 0.221166 0.386439 1.163061 0.201 Uiso 1 1 calc R U . . .
C3 C 0.3102(6) 0.3704(6) 1.0462(7) 0.174(2) Uani 1 1 d . . . . .
H3A H 0.303702 0.311334 1.079745 0.209 Uiso 1 1 calc R U . . .
F5 F 0.2095(15) 0.2266(17) 1.3010(16) 0.268(8) Uani 0.3333 1 d D U P . .
B2 B 0.1583(17) 0.1515(16) 1.2322(18) 0.156(7) Uani 0.3333 1 d D U P . .
F3 F 0.0891(17) 0.1662(18) 1.169(2) 0.305(10) Uani 0.3333 1 d D U P . .
F4 F 0.202(2) 0.122(2) 1.144(2) 0.338(12) Uani 0.3333 1 d D U P . .
F6 F 0.115(2) 0.068(2) 1.305(3) 0.379(13) 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 0.8902 '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 97.41(12) 2_665 3_565 ?
N2 Fe1 N2 97.42(12) 2_665 . ?
N2 Fe1 N2 97.42(11) 3_565 . ?
N2 Fe1 N1 169.02(13) 3_565 2_665 ?
N2 Fe1 N1 76.05(14) . . ?
N2 Fe1 N1 169.03(13) 2_665 . ?
N2 Fe1 N1 92.22(13) . 2_665 ?
N2 Fe1 N1 92.22(13) 2_665 3_565 ?
N2 Fe1 N1 92.22(13) 3_565 . ?
N2 Fe1 N1 76.05(14) 3_565 3_565 ?
N2 Fe1 N1 169.03(14) . 3_565 ?
N2 Fe1 N1 76.05(14) 2_665 2_665 ?
N1 Fe1 N1 95.19(13) 3_565 . ?
N1 Fe1 N1 95.19(13) 2_665 . ?
N1 Fe1 N1 95.19(13) 3_565 2_665 ?
N3 N2 Fe1 137.7(3) . . ?
C6 N2 Fe1 116.7(3) . . ?
C6 N2 N3 105.6(3) . . ?
N2 N3 H3 120(3) . . ?
N2 N3 C8 111.3(4) . . ?
C8 N3 H3 127(3) . . ?
C5 N1 Fe1 115.3(3) . . ?
C5 N1 C1 117.0(4) . . ?
C1 N1 Fe1 127.5(4) . . ?
N2 C6 C5 116.3(4) . . ?
N2 C6 C7 111.6(4) . . ?
C7 C6 C5 132.1(4) . . ?
C10 N4 C13 117.5(4) . . ?
N3 C8 C9 122.5(4) . . ?
N3 C8 C7 105.8(4) . . ?
C7 C8 C9 131.8(4) . . ?
C11 C9 C8 124.2(4) . . ?
C11 C9 C10 115.8(4) . . ?
C10 C9 C8 119.9(4) . . ?
N1 C5 C6 115.4(4) . . ?
N1 C5 C4 122.1(5) . . ?
C4 C5 C6 122.5(5) . . ?
C6 C7 C8 105.7(4) . . ?
C6 C7 H7 127.2 . . ?
C8 C7 H7 127.2 . . ?
N4 C13 H13 118.9 . . ?
N4 C13 C12 122.1(5) . . ?
C12 C13 H13 118.9 . . ?
C9 C11 H11 119.5 . . ?
C12 C11 C9 120.9(5) . . ?
C12 C11 H11 119.5 . . ?
N4 C10 C9 125.0(4) . . ?
N4 C10 H10 117.5 . . ?
C9 C10 H10 117.5 . . ?
F2 B1 F2 107.7(5) 2_665 . ?
F2 B1 F2 107.7(5) 2_665 3_565 ?
F2 B1 F2 107.7(5) 3_565 . ?
F1 B1 F2 111.2(4) . . ?
F1 B1 F2 111.2(4) . 2_665 ?
F1 B1 F2 111.2(4) . 3_565 ?
N1 C1 H1 117.8 . . ?
N1 C1 C2 124.3(6) . . ?
C2 C1 H1 117.8 . . ?
C13 C12 H12 120.8 . . ?
C11 C12 C13 118.5(5) . . ?
C11 C12 H12 120.8 . . ?
C5 C4 H4 121.1 . . ?
C3 C4 C5 117.8(6) . . ?
C3 C4 H4 121.1 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.5(6) . . ?
C3 C2 H2 120.8 . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 C4 120.2(6) . . ?
C2 C3 H3A 119.9 . . ?
F5 B2 F3 109.8(18) . . ?
F5 B2 F4 123(2) . . ?
F5 B2 F6 105.7(19) . . ?
F3 B2 F4 102.9(17) . . ?
F6 B2 F3 114(2) . . ?
F6 B2 F4 101.9(19) . . ?
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 2.109(3) 2_665 ?
Fe1 N2 2.109(3) 3_565 ?
Fe1 N2 2.109(3) . ?
Fe1 N1 2.163(4) 2_665 ?
Fe1 N1 2.163(4) . ?
Fe1 N1 2.163(4) 3_565 ?
N2 N3 1.338(4) . ?
N2 C6 1.330(5) . ?
N3 H3 1.02(6) . ?
N3 C8 1.377(5) . ?
N1 C5 1.329(6) . ?
N1 C1 1.334(6) . ?
F2 B1 1.393(5) . ?
F1 B1 1.286(11) . ?
C6 C5 1.470(6) . ?
C6 C7 1.377(6) . ?
N4 C13 1.357(6) . ?
N4 C10 1.325(6) . ?
C8 C9 1.429(6) . ?
C8 C7 1.379(6) . ?
C9 C11 1.385(7) . ?
C9 C10 1.397(6) . ?
C5 C4 1.385(7) . ?
C7 H7 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.384(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.381(7) . ?
C10 H10 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.350(9) . ?
C12 H12 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.382(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.331(10) . ?
C3 H3A 0.9300 . ?
F5 B2 1.267(16) . ?
B2 F3 1.370(17) . ?
B2 F4 1.375(17) . ?
B2 F6 1.360(18) . ?
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 178.8(3) . . . . ?
Fe1 N2 C6 C5 1.5(5) . . . . ?
Fe1 N2 C6 C7 -178.3(3) . . . . ?
Fe1 N1 C5 C6 5.7(5) . . . . ?
Fe1 N1 C5 C4 -174.7(4) . . . . ?
Fe1 N1 C1 C2 173.6(5) . . . . ?
N2 N3 C8 C9 178.9(4) . . . . ?
N2 N3 C8 C7 -0.4(5) . . . . ?
N2 C6 C5 N1 -4.9(6) . . . . ?
N2 C6 C5 C4 175.5(5) . . . . ?
N2 C6 C7 C8 -1.4(5) . . . . ?
N3 N2 C6 C5 -179.0(3) . . . . ?
N3 N2 C6 C7 1.1(5) . . . . ?
N3 C8 C9 C11 -1.8(7) . . . . ?
N3 C8 C9 C10 -179.7(4) . . . . ?
N3 C8 C7 C6 1.0(5) . . . . ?
N1 C5 C4 C3 0.6(9) . . . . ?
N1 C1 C2 C3 0.2(10) . . . . ?
C6 N2 N3 C8 -0.4(4) . . . . ?
C6 C5 C4 C3 -179.8(5) . . . . ?
N4 C13 C12 C11 0.5(10) . . . . ?
C8 C9 C11 C12 178.2(5) . . . . ?
C8 C9 C10 N4 -180.0(4) . . . . ?
C9 C8 C7 C6 -178.2(5) . . . . ?
C9 C11 C12 C13 2.7(10) . . . . ?
C5 N1 C1 C2 -1.6(8) . . . . ?
C5 C6 C7 C8 178.8(4) . . . . ?
C5 C4 C3 C2 -2.0(11) . . . . ?
C7 C6 C5 N1 174.9(5) . . . . ?
C7 C6 C5 C4 -4.7(8) . . . . ?
C7 C8 C9 C11 177.3(5) . . . . ?
C7 C8 C9 C10 -0.6(8) . . . . ?
C13 N4 C10 C9 1.0(7) . . . . ?
C11 C9 C10 N4 2.0(7) . . . . ?
C10 N4 C13 C12 -2.3(8) . . . . ?
C10 C9 C11 C12 -3.8(8) . . . . ?
C1 N1 C5 C6 -178.5(4) . . . . ?
C1 N1 C5 C4 1.1(7) . . . . ?
C1 C2 C3 C4 1.7(12) . . . . ?
