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_7132467
_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         'C33 H10 Ag6 F30 N10'
_chemical_formula_sum            'C33 H10 Ag6 F30 N10'
_chemical_formula_weight         1763.73
_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             2023-09-22
_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                90.3820(10)
_cell_angle_beta                 106.1520(10)
_cell_angle_gamma                109.6750(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3037(6)
_cell_length_b                   15.8607(7)
_cell_length_c                   16.9640(8)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      2.52
_cell_volume                     3217.5(3)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65308
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.703
_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    1.907
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0660 before and 0.0378 after correction. The Ratio of minimum to maximum transmission is 0.8221. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       needle
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         17054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0578P)^2^+20.8027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14644
_reflns_number_total             17054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05659g2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7132466--7132467.cif.'
_cod_database_code               7132467
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C5(H5), C11(H11), C32(H32), C14(H14), C29(H29), C2(H2), C30(H30),
 C8(H8), C31(H31)
;
_shelx_res_checksum              63216
_shelx_hkl_checksum              38502
_shelx_fab_checksum              35523
_olex2_submission_special_instructions 'No special instructions were received'