A Supramolecular Helicate with Two Independent Fe(II) Switchable Centres and a [Fe(anilate)3]3− Guest
BARRIOS MORENO, LEONI ALEJANDRA ALEJANDRA; Teat, Simon; Roubeau, Olivier; Aromi, Guillem; Chemical Communications  (2023) –; doi:10.1039/D3CC02278A

data_7131973
_publ_section_title
;
 A Supramolecular Helicate with Two Independent Fe(II) Switchable Centres
 and a [Fe(anilate)3]3&#x2212; Guest
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02278A
_journal_year                    2023
_chemical_formula_moiety
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21
_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   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.828(3)
_cell_length_b                   21.828(3)
_cell_length_c                   21.828(3)
_cell_measurement_reflns_used    6437
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      33.76
_cell_measurement_theta_min      1.36
_cell_volume                     10400(2)
_computing_cell_refinement       XDS
_computing_data_collection       'autoPROC package'
_computing_data_reduction
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       '\w rotation'
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            168719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.522
_diffrn_reflns_theta_max         29.522
_diffrn_reflns_theta_min         1.354
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             4292
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 3817 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.092(4)
_refine_ls_extinction_coef       0.0257(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8999
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0503
_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^)+(0.1206P)^2^+0.0608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8624
_reflns_number_total             8999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02278a3.cif
_cod_data_source_block           lb2205_fresh2_300K
_cod_original_cell_volume        10400(4)
_cod_database_code               7131973
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              51236
_shelx_hkl_checksum              7599