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_7250143
_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
'C60 H68 Ag2 B4 F8 N24, 2(B F4), C3 H6 O, C4 H10 O'
_chemical_formula_sum            'C67 H84 Ag2 B6 F16 N24 O2'
_chemical_formula_weight         1842.18
_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             2024-04-30
_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                84.711(3)
_cell_angle_beta                 70.296(3)
_cell_angle_gamma                72.827(3)
_cell_formula_units_Z            1
_cell_length_a                   11.8538(4)
_cell_length_b                   12.0482(4)
_cell_length_c                   14.9556(5)
_cell_measurement_reflns_used    69881
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.90
_cell_measurement_theta_min      3.14
_cell_volume                     1921.14(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)'
_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 0.960
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
 3987 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  0.0481
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36830
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         70.475
_diffrn_reflns_theta_min         3.139
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.969
_exptl_absorpt_correction_T_max  0.6972
_exptl_absorpt_correction_T_min  0.4911
_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    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.030
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         7023
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0422P)^2^+6.8740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6325
_reflns_number_total             7023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00197h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7250141--7250151.cif.'
_cod_database_code               7250143
_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. Restrained distances
 C32-C31 = C32-C33
 1.48 with sigma of 0.02
 C34-C35 = C36-C37
 1.48 with sigma of 0.02
 C35-O2 = O2-C36
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32) = Uanis(C31)
Uanis(C32) = Uanis(C33)
Uanis(C34) = Uanis(C35)
Uanis(C34) = Uanis(O2)
Uanis(C34) = Uanis(C36)
Uanis(C34) = Uanis(C37)
4. Others
 Sof(F6')=Sof(F7')=Sof(F8')=1-FVAR(1)
 Sof(F6)=Sof(F7)=Sof(F8)=FVAR(1)
 Fixed Sof: O1(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5)
 H35A(0.5) H35B(0.5) O2(0.5) C36(0.5) H36A(0.5) H36B(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) H37C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C35(H35A,H35B), C36(H36A,H36B)
5.b Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C37(H37A,H37B,H37C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C19(H19), C22(H22), C30(H30)
5.d 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), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              63292
_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   17.6
_stoe_evaluation_integration_b   2.3
_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 95.3
_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 5.2
_stoe_evaluation_lana_number_refls_after_or 36846
_stoe_evaluation_lana_number_refls_outliers 1315
_stoe_evaluation_lana_number_refls_total 38161
_stoe_evaluation_lana_number_refls_unique 7027
_stoe_evaluation_lana_number_refls_written 36846
_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          12.8   28.0   43.2   58.4   73.6   88.8  104.0  119.2  134.4
<Resolution>    5.77   3.04   2.02   1.54   1.29   1.10   0.97   0.90   0.84
N(total)         166    535   1807   4178   8187   8892   5665   6066   2665
<Redundancy>     3.1    2.6    3.8    5.5    8.0    7.0    4.3    4.6    3.0
Complet. [%%]   100.0   95.0  100.0  100.0  100.0   99.6   96.0   97.3   77.6
<I/sigma>      385.0  235.1  115.2   68.7   41.5   26.5   19.4   14.2   12.3
R(int)         0.039  0.040  0.036  0.037  0.042  0.056  0.074  0.094  0.090
;
_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 '11.1 h'
_stoe_measurement_total_frame_number 3987
_stoe_measurement_total_run_number 51
_stoe_measurement_tube_power     '50.0 W'