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_7250150
_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         'C32 H37 Ag B2 F4 N13 O4 Re, C2 H3 N'
_chemical_formula_sum            'C34 H40 Ag B2 F4 N14 O4 Re'
_chemical_formula_weight         1100.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-11 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2292(3)
_cell_length_b                   24.4944(10)
_cell_length_c                   17.7165(5)
_cell_measurement_reflns_used    39362
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.84
_cell_measurement_theta_min      10.11
_cell_volume                     4005.1(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 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
 1688 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  0.0854
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            31325
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         70.444
_diffrn_reflns_theta_min         3.079
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    10.406
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_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    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         1.575
_refine_diff_density_min         -1.863
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0971P)^2^+25.8301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3301
_reflns_number_total             3864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00197h2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7250141--7250151.cif.'
_cod_database_code               7250150
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H17A,H17B,H17C} of C17, All C(H,H) groups
 At 1.5 times of:
  {H10A,H10B,H10C} of C10, {H19A,H19B,H19C} of C19, {H13A,H13B,H13C} of C13,
  {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12
2. Others
 Fixed Sof: O2(0.5) O3(0.5) O4(0.5) H17A(0.5) H17B(0.5) H17C(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              36585
_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   16.4
_stoe_evaluation_integration_b   0.0
_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 98.3
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 4
_stoe_evaluation_lana_max_2theta_available 140.9
_stoe_evaluation_lana_max_2theta_desired 140.9
_stoe_evaluation_lana_mean_redundancy 8.1
_stoe_evaluation_lana_number_refls_after_or 31325
_stoe_evaluation_lana_number_refls_outliers 869
_stoe_evaluation_lana_number_refls_total 32194
_stoe_evaluation_lana_number_refls_unique 3864
_stoe_evaluation_lana_number_refls_written 31325
_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 mmm
_stoe_evaluation_lana_table
;
2Theta          12.7   27.9   43.1   58.3   73.5   88.7  103.9  119.1  134.3
<Resolution>    5.65   3.07   2.02   1.56   1.29   1.10   0.97   0.90   0.84
N(total)          63    441   1730   4017   7563   7190   4480   4710   2000
<Redundancy>     2.7    4.0    6.7   10.0   13.8   10.7    6.4    6.5    3.7
Complet. [%%]    82.1   98.1   99.6   99.2  100.0   99.8   99.1   99.7   91.8
<I/sigma>      492.5  241.1  106.9   67.9   37.7   24.1   14.9   11.7    7.8
R(int)         0.048  0.056  0.068  0.073  0.097  0.098  0.115  0.146  0.156
;
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '10.0 s'
_stoe_measurement_min_exposure_per_frame '10.0 s'
_stoe_measurement_total_exposure_time '4.7 h'
_stoe_measurement_total_frame_number 1688
_stoe_measurement_total_run_number 22
_stoe_measurement_tube_power     '50.0 W'