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_7250146
_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         '2(C45 H51 Ag B3 F6 N18), 2(F6 P)'
_chemical_formula_sum            'C90 H102 Ag2 B6 F24 N36 P2'
_chemical_formula_weight         2486.61
_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             2024-07-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-12-11 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                61.779(2)
_cell_angle_beta                 85.708(3)
_cell_angle_gamma                74.541(2)
_cell_formula_units_Z            1
_cell_length_a                   11.3667(4)
_cell_length_b                   16.8858(5)
_cell_length_c                   16.9432(6)
_cell_measurement_reflns_used    45983
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.85
_cell_measurement_theta_min      2.97
_cell_volume                     2756.75(17)
_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  'SHELXL 2014/7 (Sheldrick, 2015)'
_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 0.965
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
 2634 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  0.0309
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30111
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.464
_diffrn_reflns_theta_min         2.965
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.017
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.4930
_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.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         9961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0828P)^2^+4.4344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8439
_reflns_number_total             9961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00197h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7250141--7250151.cif.'
_cod_database_code               7250146
_shelx_shelxl_version_number     2014/7
_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), C44(H44A,H44B)
2.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)
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), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94203
_shelx_fab_checksum              860
_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 94.4
_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 141.0
_stoe_evaluation_lana_max_2theta_desired 141.0
_stoe_evaluation_lana_mean_redundancy 3.0
_stoe_evaluation_lana_number_refls_after_or 30111
_stoe_evaluation_lana_number_refls_outliers 7346
_stoe_evaluation_lana_number_refls_total 37457
_stoe_evaluation_lana_number_refls_unique 9961
_stoe_evaluation_lana_number_refls_written 30111
_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 -1
_stoe_evaluation_lana_table
;
2Theta          12.7   27.9   43.1   58.3   73.5   88.7  103.9  119.1  134.3
<Resolution>    5.88   3.03   2.03   1.54   1.29   1.10   0.97   0.90   0.84
N(total)         187    508   1440   3585   8004   8515   5743   6525   2950
<Redundancy>     2.3    1.7    2.0    2.8    4.3    3.9    2.6    2.8    2.1
Complet. [%%]    97.1   90.1   97.5   99.4  100.0   99.8   93.0   97.8   76.9
<I/sigma>      256.9  171.1   72.9   39.4   23.4   14.5   11.1    7.4    6.1
R(int)         0.025  0.027  0.023  0.024  0.023  0.033  0.049  0.070  0.098
;
_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 '14.6 h'
_stoe_measurement_total_frame_number 2634
_stoe_measurement_total_run_number 32
_stoe_measurement_tube_power     '50.0 W'