Pyrazolate <i>vs.</i> phenylethynide: direct exchange of the anionic bridging ligand in a cyclic trinuclear silver complex.
Titov, Aleksei A.; Smol'yakov, Alexander F.; Chernyadyev, Andrey Yu; Godovikov, Ivan A.; Filippov, Oleg A.; Shubina, Elena S.; Chemical communications (Cambridge, England) 60 (2024) 847–850; doi:10.1039/d3cc05659g

data_7132466
_publ_section_title
;
 Pyrazolate <i>vs.</i> phenylethynide: direct exchange of the anionic
 bridging ligand in a cyclic trinuclear silver complex.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              847
_journal_page_last               850
_journal_paper_doi               10.1039/d3cc05659g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C18 H7 Ag3 F12 N4'
_chemical_formula_sum            'C18 H7 Ag3 F12 N4'
_chemical_formula_weight         830.89
_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             2023-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-22 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                116.4550(10)
_cell_angle_beta                 95.181(2)
_cell_angle_gamma                102.301(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2213(5)
_cell_length_b                   12.3633(8)
_cell_length_c                   12.5168(8)
_cell_measurement_reflns_used    6408
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      2.59
_cell_volume                     1087.63(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11538
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.859
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.793
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0427 before and 0.0299 after correction.
The Ratio of minimum to maximum transmission is 0.8951.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5780
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+2.5106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5048
_reflns_number_total             5780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05659g2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7132466--7132467.cif.'
_cod_database_code               7132466
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.519
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F11R) \\sim Ueq, Uanis(F10R) \\sim Ueq, Uanis(F12R) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F12) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: F10(0.25) F10R(0.75) F11(0.25) F11R(0.75) F12(0.25) F12R(0.75)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13)
;
_shelx_res_checksum              37250
_shelx_hkl_checksum              23170
_olex2_submission_special_instructions 'No special instructions were received'