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_7250145
_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 Ag5 B4 F18 N24 O10 P5, H2 O'
_chemical_formula_sum            'C60 H70 Ag5 B4 F18 N24 O11 P5'
_chemical_formula_weight         2382.84
_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   mixed
_audit_creation_date             2022-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-12-11 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                95.436(6)
_cell_angle_beta                 94.643(7)
_cell_angle_gamma                92.586(7)
_cell_formula_units_Z            2
_cell_length_a                   9.1775(8)
_cell_length_b                   10.1075(8)
_cell_length_c                   43.740(4)
_cell_measurement_reflns_used    50886
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.81
_cell_measurement_theta_min      2.04
_cell_volume                     4020.2(6)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area X-Red 2.3.0.0 (STOE, 2021) 
;
_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 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_details
;
 2362 frames, detector distance = 40 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  0.0678
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            43364
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.567
_diffrn_reflns_theta_min         2.037
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.565
_exptl_absorpt_correction_T_max  0.1464
_exptl_absorpt_correction_T_min  0.0700
_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    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.955
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1161
_refine_ls_number_reflns         14791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.1189
_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^)+(0.0601P)^2^+150.4570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2599
_refine_ls_wR_factor_ref         0.2799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11382
_reflns_number_total             14791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00197h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7250141--7250151.cif.'
_cod_database_code               7250145
_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, All O(H,H) groups
2.a Rotating group:
 OW1(HW1A,HW1B)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C44(H44A,H44B), C59(H59A,H59B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C15(H15), C17(H17), C23(H23), C30(H30), C32(H32), C38(H38),
 C45(H45), C47(H47), C53(H53), C60(H60)
2.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), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              64511
_olex2_submission_special_instructions 'No special instructions were received'