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_7064282
_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         'C66 H80 B4 F8 Fe N24 O2, 2(Cl O4)'
_chemical_formula_sum            'C66 H80 B4 Cl2 F8 Fe N24 O10'
_chemical_formula_weight         1691.53
_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   geom
_audit_creation_date             2024-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.373(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2755(2)
_cell_length_b                   16.9467(2)
_cell_length_c                   24.3130(5)
_cell_measurement_reflns_used    48021
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.06
_cell_measurement_theta_min      2.61
_cell_volume                     3810.61(12)
_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
;
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 2.3, Darmstadt 2023
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
 2172 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  0.0373
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41793
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         70.533
_diffrn_reflns_theta_min         3.182
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.3088
_exptl_absorpt_correction_T_min  0.1980
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.080
_refine_diff_density_max         1.345
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0659P)^2^+4.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6345
_reflns_number_total             7094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03028e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7064278--7064283.cif.'
_cod_database_code               7064282
_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.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C19(H19), C22(H22), C30(H30)
2.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), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              56792
_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   13.2
_stoe_evaluation_integration_b   -0.9
_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 97.1
_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 5.8
_stoe_evaluation_lana_number_refls_after_or 42801
_stoe_evaluation_lana_number_refls_outliers 435
_stoe_evaluation_lana_number_refls_total 43236
_stoe_evaluation_lana_number_refls_unique 7359
_stoe_evaluation_lana_number_refls_written 42801
_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 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>    5.81   3.10   2.05   1.54   1.29   1.10   0.97   0.90   0.84
N(total)         193    797   1926   4608   9503   9444   6401   7147   3217
<Redundancy>     3.4    3.7    4.2    6.1    9.2    7.6    4.8    5.3    3.2
Complet. [%%]   100.0   96.8  100.0   99.9  100.0  100.0   98.6   98.0   85.1
<I/sigma>      309.0  162.1   74.0   39.9   25.1   18.7   15.0   10.8    9.3
R(int)         0.033  0.021  0.023  0.026  0.036  0.041  0.056  0.093  0.135
;
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '5.0 s'
_stoe_measurement_min_exposure_per_frame '5.0 s'
_stoe_measurement_total_exposure_time '3.0 h'
_stoe_measurement_total_frame_number 2172
_stoe_measurement_total_run_number 27
_stoe_measurement_tube_power     '50.0 W'