Self-assembly of a supramolecular spin-crossover tetrahedron.
Nielsen, Hannah H.; Vilariño, Pol; Rodríguez, Gemma; Trepard, Florian; Roubeau, Olivier; Aromí, Guillem; Aguilà, David; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9792–9797; doi:10.1039/d4dt00578c

data_7716118
_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       '\w 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/[\s^2^(Fo^2^)+(0.1917P)^2^+0.3016P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              83330
_olex2_submission_special_instructions 'No special instructions were received'