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_7064279
_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
'4(C2 H2 Br N), C90 H102 B6 F12 Fe N36, 2(Cl O4)'
_chemical_formula_sum            'C98 H110 B6 Br4 Cl2 F12 Fe N40 O8'
_chemical_formula_weight         2715.50
_chemical_name_common            'Trirubidium sodium tetraplumbate'
_chemical_name_structure_type    Rb3NaTiO4
_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             2025-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-31 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.081(5)
_cell_angle_beta                 70.357(5)
_cell_angle_gamma                66.017(5)
_cell_formula_units_Z            1
_cell_length_a                   13.6961(9)
_cell_length_b                   15.0329(9)
_cell_length_c                   16.4033(11)
_cell_measurement_reflns_used    57574
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.03
_cell_measurement_theta_min      2.89
_cell_volume                     2884.9(3)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
 2659 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  0.0406
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38400
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         71.185
_diffrn_reflns_theta_min         2.881
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.887
_exptl_absorpt_correction_T_max  0.6592
_exptl_absorpt_correction_T_min  0.4539
_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    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.040
_refine_diff_density_max         2.372
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         10474
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1037P)^2^+7.4876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9196
_reflns_number_total             10474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03028e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7064278--7064283.cif.'
_cod_original_cell_volume        2884.9(4)
_cod_database_code               7064279
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_ac3_digest_hkl    41addfe6536e329ea810ed3a3a3f85ded57737
_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. Restrained distances
 Br2'-C49'
 1.9 with sigma of 0.02
 C49'-C48'
 1.5 with sigma of 0.02
 C48'-N20'
 1.1 with sigma of 0.02
 Cl1-O3' = Cl1-O2'
 1.44 with sigma of 0.02
3. Restrained planarity
 Br2', C49', C48', N20'
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Br2') = Uanis(C48')
Uanis(Br2') = Uanis(C49')
Uanis(Br2') = Uanis(N20')
Uanis(Br2) = Uanis(C48)
Uanis(Br2) = Uanis(C49)
Uanis(Br2) = Uanis(N20)
Uanis(Br1) = Uanis(Br1')
Uanis(C46) = Uanis(N19)
Uanis(O2) = Uanis(O2')
Uanis(O3) = Uanis(O3')
5. Others
 Sof(Br2')=Sof(C48')=Sof(C49')=Sof(H49C)=Sof(H49D)=Sof(N20')=1-FVAR(1)
 Sof(Br2)=Sof(N20)=Sof(C48)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
 Sof(Br1')=Sof(O2')=Sof(O3')=1-FVAR(2)
 Sof(Br1)=Sof(O2)=Sof(O3)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C44(H44A,H44B), C47(H47A,H47B), C49(H49A,
 H49B), C49'(H49C,H49D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C19(H19), C22(H22), C30(H30), C34(H34), C37(H37),
 C45(H45)
6.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              97955
_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 93.7
_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 142.4
_stoe_evaluation_lana_max_2theta_desired 142.4
_stoe_evaluation_lana_mean_redundancy 3.7
_stoe_evaluation_lana_number_refls_after_or 38400
_stoe_evaluation_lana_number_refls_outliers 1222
_stoe_evaluation_lana_number_refls_total 39622
_stoe_evaluation_lana_number_refls_unique 10474
_stoe_evaluation_lana_number_refls_written 38400
_stoe_evaluation_lana_or_c1      0.100
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      2.0
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          12.5   27.9   43.3   58.7   74.1   89.5  104.9  120.3  135.7
<Resolution>    5.78   3.06   2.03   1.52   1.28   1.09   0.96   0.89   0.84
N(total)         160    578   1692   4292   8620   9114   6210   6379   2577
<Redundancy>     2.3    2.0    2.4    3.7    5.5    4.8    3.2    3.2    2.2
Complet. [%%]    93.1   93.8   97.9   99.6  100.0   99.6   93.5   97.0   70.8
<I/sigma>      318.2  302.1  120.4   65.6   41.7   25.4   19.0   14.7   11.9
R(int)         0.041  0.025  0.031  0.034  0.040  0.045  0.061  0.082  0.117
;
_stoe_measurement_identifier     100K
_stoe_measurement_max_exposure_per_frame '20.0 s'
_stoe_measurement_mean_exposure_per_frame '20.0 s'
_stoe_measurement_min_exposure_per_frame '20.0 s'
_stoe_measurement_total_exposure_time '14.8 h'
_stoe_measurement_total_frame_number 2659
_stoe_measurement_total_run_number 33
_stoe_measurement_tube_power     '50.0 W'