Fluorinated tris(pyridyl)borate ligand support on coinage metals.
Vanga, Mukundam; Muñoz-Castro, Alvaro; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1308–1312; doi:10.1039/d1dt04136c

data_7709184
_publ_section_title
;
 Fluorinated tris(pyridyl)borate ligand support on coinage metals.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1308
_journal_page_last               1312
_journal_paper_doi               10.1039/d1dt04136c
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C30 H26 Ag B F9 N3'
_chemical_formula_sum            'C30 H26 Ag B F9 N3'
_chemical_formula_weight         718.22
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-03 deposited with the CCDC.	2021-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                72.0740(10)
_cell_angle_beta                 89.2980(10)
_cell_angle_gamma                73.7390(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2339(4)
_cell_length_b                   12.0369(4)
_cell_length_c                   12.9756(4)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      38.32
_cell_measurement_theta_min      2.62
_cell_volume                     1455.17(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Photon II 7 CPAD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II 7'
_diffrn_measurement_method       '0.3\% \w and \f scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'Photon II 7 CPAD'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27189
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.551
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.5688
_exptl_absorpt_correction_T_min  0.5203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.278
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         10786
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0076P)^2^+4.0286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9796
_reflns_number_total             10786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04136c2.cif
_cod_data_source_block           hrd53_0m_a
_cod_depositor_comments
'Adding full bibliography for 7709183--7709187.cif.'
_cod_database_code               7709184
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Restrained distances
 C28A-C25 \\sim C26-C25 \\sim C26A-C25 \\sim C27-C25 \\sim C27A-C25 \\sim
C28-C25
 with sigma of 0.008
 F8-C18 \\sim F9-C18 \\sim F9A-C18A \\sim F7-C18 \\sim F7A-C18A \\sim F8A-C18A
 with sigma of 0.009
 C18-C13 \\sim C18A-C13
 with sigma of 0.008
2. Rigid bond restraints
 F7, F8, F9, F7A, F8A, F9A
 with sigma for 1-2 distances of 0.009 and sigma for 1-3 distances of 0.009
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.004 within 1.7A
4. Others
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C18A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C18)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C20(H20), C21(H21), C23(H23), C24(H24)
5.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C26A(H26D,H26E,
 H26F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F)
;
_shelx_res_checksum              73298
_shelx_hkl_checksum              78577
_olex2_submission_special_instructions 'No special instructions were received'