Structural tuning of tetrazole-BODIPY Ag(i) coordination compounds <i>via</i> co-ligand addition and counterion variation.
Schöbinger, Matthias; Huber, Martin; Stöger, Berthold; Hametner, Christian; Weinberger, Peter; CrystEngComm 27 (2025) 2689–2697; doi:10.1039/d5ce00197h

data_7250141
_publ_section_title
;
 Structural tuning of tetrazole-BODIPY Ag(i) coordination compounds
 <i>via</i> co-ligand addition and counterion variation.
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2689
_journal_page_last               2697
_journal_paper_doi               10.1039/d5ce00197h
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C68 H80 Ag2 B4 F8 N28, 2(B F4)'
_chemical_formula_sum            'C68 H80 Ag2 B6 F16 N28'
_chemical_formula_weight         1874.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-11 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.810(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7076(3)
_cell_length_b                   15.1774(7)
_cell_length_c                   24.6897(8)
_cell_measurement_reflns_used    14925
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.47
_cell_measurement_theta_min      14.10
_cell_volume                     3927.5(2)
_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)'
_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 0.967
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
 2053 frames, detector distance = 50 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  0.0449
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32631
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        69.500
_diffrn_reflns_theta_max         69.636
_diffrn_reflns_theta_min         3.439
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.870
_exptl_absorpt_correction_T_max  0.2308
_exptl_absorpt_correction_T_min  0.1605
_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    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.14
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00032(5)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0613P)^2^+2.8548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6578
_reflns_number_total             7125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00197h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7250141--7250151.cif.'
_cod_database_code               7250141
_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. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F6')
Uanis(F7) = Uanis(F7')
Uanis(F8) = Uanis(F8')
3. Others
 Sof(F6')=Sof(F7')=Sof(F8')=1-FVAR(1)
 Sof(F6)=Sof(F7)=Sof(F8)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C19(H19), C22(H22), C30(H30)
4.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), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              90666
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '50.0 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 96.2
_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 139.3
_stoe_evaluation_lana_max_2theta_desired 139.3
_stoe_evaluation_lana_mean_redundancy 4.5
_stoe_evaluation_lana_number_refls_after_or 33372
_stoe_evaluation_lana_number_refls_outliers 1081
_stoe_evaluation_lana_number_refls_total 34453
_stoe_evaluation_lana_number_refls_unique 7407
_stoe_evaluation_lana_number_refls_written 33372
_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          12.5   27.5   42.5   57.5   72.5   87.5  102.5  117.5  132.5
<Resolution>    5.72   3.12   2.08   1.59   1.30   1.11   0.99   0.91   0.85
N(total)         217    665   1363   2761   7411   7614   5655   5991   2776
<Redundancy>     3.5    2.9    2.8    3.5    7.0    5.9    4.2    4.3    2.8
Complet. [%%]    98.3   99.1   98.7   99.3  100.0   99.6   95.6   97.5   84.6
<I/sigma>      239.3  180.1   87.8   53.7   35.2   27.1   21.6   18.9   18.3
R(int)         0.060  0.057  0.054  0.036  0.040  0.041  0.042  0.052  0.069
;
_stoe_measurement_max_exposure_per_frame '1.0 s'
_stoe_measurement_mean_exposure_per_frame '1.0 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '34 min'
_stoe_measurement_total_frame_number 2053
_stoe_measurement_total_run_number 25
_stoe_measurement_tube_power     '50.0 W'