Engineered π⋯π interactions favour supramolecular dimers X@[FeL<sub>3</sub>]<sub>2</sub> (X = Cl, Br, I): solid state and solution structure.
Risa, Arnau; Barrios, Leoní A; Diego, Rosa; Roubeau, Olivier; Aleshin, Dmitry Y.; Nelyubina, Yulia; Novikov, Valentin; Teat, Simon J.; Ribas-Ariño, Jordi; Aromí, Guillem; Chemical science 15 (2024) 9047–9053; doi:10.1039/d4sc01365d

data_1571752
_publ_section_title
;
 Engineered &#x3c0;&#x22ef;&#x3c0; interactions favour supramolecular
 dimers X@[FeL<sub>3</sub>]<sub>2</sub> (X = Cl, Br, I): solid state and
 solution structure.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9047
_journal_page_last               9053
_journal_paper_doi               10.1039/d4sc01365d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'2(C90 H60 Fe N18), 2.611(F6 P), (I), 0.389(I3), H2 O, 5 (C3 H6 O)'
_chemical_formula_sum            'C195 H152 F15.66 Fe2 I2.17 N36 O6 P2.61'
_chemical_formula_weight         3878.72
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.532(3)
_cell_length_b                   26.532(3)
_cell_length_c                   26.532(3)
_cell_measurement_reflns_used    12011
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.18
_cell_measurement_theta_min      1.11
_cell_volume                     18677(4)
_computing_cell_refinement       'Global Phasing autoPROC package'
_computing_data_collection       'Global Phasing autoPROC package'
_computing_data_reduction
;
autoPROC (Acta Cryst. 2011, D67, 293-302)
XDS (Kabsch, W. Acta Cryst. 2010, D66, 125-132)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       '\w rotation at various \k'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            347834
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.899
_diffrn_reflns_theta_max         30.899
_diffrn_reflns_theta_min         1.114
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             7857
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 8290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(3)
_refine_ls_extinction_coef       0.0100(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         18241
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0542
_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/[\s^2^(Fo^2^)+(0.1217P)^2^+4.8088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                17922
_reflns_number_total             18241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01365d2.cif
_cod_data_source_block           ar34
_cod_depositor_comments
'Adding full bibliography for 1571750--1571752.cif.'
_cod_original_cell_volume        18677(6)
_cod_database_code               1571752
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              56813
_shelx_fab_checksum              73659