Linkage isomerism in a homoleptic Fe(ii) complex with BODIPY-1H-tetrazole ligands
Schöbinger, Matthias; Huber, Martin; Stöger, Berthold; Weinberger, Peter; New Journal of Chemistry 50 (2026) 4271–4277; doi:10.1039/D5NJ03028E

data_7064278
_publ_section_title
;
 Linkage isomerism in a homoleptic Fe(ii) complex with BODIPY-1H-tetrazole
 ligands
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4271
_journal_page_last               4277
_journal_paper_doi               10.1039/D5NJ03028E
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety
'C90 H102 B6 F12 Fe N36, 2(Cl O4), 4(C2 H2 Cl N), 0.36(O H2)'
_chemical_formula_sum            'C98 H110.72 B6 Cl6 F12 Fe N40 O8.36'
_chemical_formula_weight         2544.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                77.116(9)
_cell_angle_beta                 70.890(10)
_cell_angle_gamma                66.469(8)
_cell_formula_units_Z            1
_cell_length_a                   13.6265(17)
_cell_length_b                   15.0163(14)
_cell_length_c                   16.2071(19)
_cell_measurement_reflns_used    1350
_cell_measurement_temperature    100
_cell_measurement_theta_max      41.16
_cell_measurement_theta_min      8.23
_cell_volume                     2856.6(6)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area X-Red 2.3.0.0 (STOE, 2021) 
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
 360 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50362
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.865
_diffrn_reflns_theta_min         2.902
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.151
_exptl_absorpt_correction_T_max  0.4211
_exptl_absorpt_correction_T_min  0.2523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00031(8)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         10614
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+2.4841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8915
_reflns_number_total             10614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03028e2.cif
_cod_data_source_block           1a_100K
_cod_depositor_comments
'Adding full bibliography for 7064278--7064283.cif.'
_cod_database_code               7064278
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C48-C49'
 1.43 with sigma of 0.002
 C48-C49
 1.43 with sigma of 0.002
 C49'-N20'
 1.1 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3') = Uanis(C49)
Uanis(Cl3') = Uanis(N20)
4. Others
 Sof(H48C)=Sof(H48D)=Sof(Cl3')=Sof(N20')=Sof(C49')=1-FVAR(1)
 Sof(H48A)=Sof(H48B)=Sof(Cl3)=Sof(N20)=Sof(C49)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C44(H44A,H44B), C46(H46A,H46B), C48(H48A,
 H48B), C48(H48C,H48D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C15(H15), C17(H17), C23(H23), C30(H30), C32(H32), C38(H38),
 C45(H45)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              76511
_olex2_submission_special_instructions 'No special instructions were received'