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_7064281
_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
'C62 H76 B4 F8 Fe N24 O2, 2(Cl O4), 2(C4 H10 O), 0.627(C H4 O)'
_chemical_formula_sum            'C70.62 H98.5 B4 Cl2 F8 Fe N24 O12.62'
_chemical_formula_weight         1807.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.455(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.0397(9)
_cell_length_b                   14.6823(3)
_cell_length_c                   17.0224(5)
_cell_measurement_reflns_used    52065
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.78
_cell_measurement_theta_min      2.69
_cell_volume                     8220.1(4)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
 2267 frames, detector distance = 45 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  0.0255
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35949
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         70.535
_diffrn_reflns_theta_min         3.296
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.873
_exptl_absorpt_correction_T_max  0.7111
_exptl_absorpt_correction_T_min  0.4154
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3773
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7676
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0715P)^2^+30.9196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6676
_reflns_number_total             7676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03028e2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7064278--7064283.cif.'
_cod_original_formula_sum        'C70.62 H98.50 B4 Cl2 F8 Fe N24 O12.62'
_cod_database_code               7064281
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C36, C36'}
3. Restrained distances
 O1-C31 = O1-C31'
 1.42 with sigma of 0.02
 O8-C36 = O8'-C36'
 1.42 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C31')
Uanis(O8) = Uanis(O8') = Uanis(C36) = Uanis(C36')
5. Others
 1*[Sof(C31)+Sof(H31A)+Sof(H31B)+Sof(H31C)+Sof(C31')+Sof(H31D)+Sof(H31E)+
 Sof(H31F)]+1*[Sof(C36)+Sof(O8)]+1*[Sof(C36')+Sof(O8')]=1 with esd of 0.000001
 Sof(C31')=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(C36)=Sof(O8)=FVAR(2)
 Sof(C36')=Sof(O8')=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C33(H33A,H33B), C34(H34A,H34B)
6.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C19(H19), C22(H22), C30(H30)
6.d 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), C31(H31A,H31B,H31C), C31'(H31D,H31E,H31F)
;
_shelx_res_checksum              43864
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '45.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   15.4
_stoe_evaluation_integration_b   0.4
_stoe_evaluation_integration_ems 0.037
_stoe_evaluation_lana_bis_l_even_max 4
_stoe_evaluation_lana_bis_l_odd_max 1
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 97.5
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 141.1
_stoe_evaluation_lana_max_2theta_desired 141.1
_stoe_evaluation_lana_mean_redundancy 4.7
_stoe_evaluation_lana_number_refls_after_or 35960
_stoe_evaluation_lana_number_refls_outliers 9936
_stoe_evaluation_lana_number_refls_total 45896
_stoe_evaluation_lana_number_refls_unique 7681
_stoe_evaluation_lana_number_refls_written 35960
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta          12.4   27.6   42.8   58.0   73.2   88.4  103.6  118.8  134.0
<Resolution>    5.84   3.09   2.04   1.56   1.29   1.10   0.97   0.90   0.84
N(total)         177    822   2533   5415  10273  10191   6570   6715   3200
<Redundancy>     2.8    3.0    4.1    5.5    7.4    6.2    3.8    3.8    2.5
Complet. [%%]    97.9   97.2  100.0  100.0  100.0  100.0   96.6   99.8   88.7
<I/sigma>      351.0  230.3   88.2   42.9   25.5   16.6   12.2    8.4    7.1
R(int)         0.026  0.016  0.016  0.019  0.026  0.032  0.043  0.060  0.083
;
_stoe_measurement_max_exposure_per_frame '15.0 s'
_stoe_measurement_mean_exposure_per_frame '15.0 s'
_stoe_measurement_min_exposure_per_frame '15.0 s'
_stoe_measurement_total_exposure_time '9.4 h'
_stoe_measurement_total_frame_number 2267
_stoe_measurement_total_run_number 29
_stoe_measurement_tube_power     '50.0 W'