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_1571751
_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), 3(F6 P), Br, 4(C3 H6 O)'
_chemical_formula_sum            'C192 H144 Br F18 Fe2 N36 O4 P3'
_chemical_formula_weight         3645.94
_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-2017/1
_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                   26.5373(7)
_cell_length_b                   26.5373(7)
_cell_length_c                   26.5373(7)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.284
_cell_measurement_theta_min      2.226
_cell_volume                     18688.3(9)
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            125109
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.376
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         1.760
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             7496
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 3648 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         10649
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1544P)^2^+20.9710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2223
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9033
_reflns_number_total             10649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01365d2.cif
_cod_data_source_block           lb2191
_cod_depositor_comments
'Adding full bibliography for 1571750--1571752.cif.'
_cod_original_cell_volume        18688.3(15)
_cod_database_code               1571751
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              23579
_shelx_fab_checksum              62680