Cyanido-bridged {FeIIILnIII} heterobimetallic chains assembled through the [FeIII{HB(pz)3}(CN)3]− complex as metalloligand: synthesis, crystal structure and magnetic properties
Visinescu, Diana; Alexandru, Maria-Gabriela; Dumitrescu, Dan G.; Shova, Sergiu; Moliner, Nicolás; Lloret, Francesc; Julve, Miguel; CrystEngComm 23 (2021) 4615–4626; doi:10.1039/D1CE00626F

data_7242922
_publ_section_title
;
 Cyanido-bridged {FeIIILnIII} heterobimetallic chains assembled through
 the [FeIII{HB(pz)3}(CN)3]&#x2212; complex as metalloligand: synthesis,
 crystal structure and magnetic properties
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4615
_journal_page_last               4626
_journal_paper_doi               10.1039/D1CE00626F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C22 H20 B Fe Gd N13 O9, C2 H3 N'
_chemical_formula_sum            'C24 H23 B Fe Gd N14 O9'
_chemical_formula_weight         875.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-28 deposited with the CCDC.	2021-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.244(3)
_cell_length_b                   14.193(3)
_cell_length_c                   13.216(3)
_cell_measurement_reflns_used    2563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.765
_cell_measurement_theta_min      2.513
_cell_volume                     3234.1(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5653
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.624
_diffrn_reflns_theta_max         24.624
_diffrn_reflns_theta_min         1.163
_exptl_absorpt_coefficient_mu    2.459
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.517
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5653
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0809P)^2^+36.7555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4940
_reflns_number_total             5653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00626f2.cif
_cod_data_source_block           fegdnno_c2_tw
_cod_depositor_comments
'Adding full bibliography for 7242919--7242922.cif.'
_cod_original_cell_volume        3234.1(11)
_cod_database_code               7242922
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.840(3)
 0.160(3)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 N14X-C23X = N14-C23
 1.17 with sigma of 0.01
 C24X-C23X = C24-C23
 1.54 with sigma of 0.01
 N14-C24
 2.677 with sigma of 0.01
 N14X-C24X
 2.677 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C24) = Uiso(C24X)
Uiso(C23) = Uiso(C23X)
Uiso(N14) = Uiso(N14X)
5. Others
 Sof(C23X)=Sof(C24X)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(N14X)=1-FVAR(1)
 Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(N14)=FVAR(1)
6.a Riding coordinates:
 O3(H3A,H3B), C24(H24A,H24B,H24C), C24X(H24D,H24E,H24F)
6.b Ternary CH refined with riding coordinates:
 B017(H017)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              33998
_shelx_hkl_checksum              27108
_olex2_submission_special_instructions 'No special instructions were received'