A systematic study of naphthyridine-derived ligands for well-defined silver(I) dimers.
Bavaresco, Sofia Teixeira; Marquard, Nina P.; Miura-Stempel, Emily; Mohsen, Mariana G.; Campbell, Michael G.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13651–13657; doi:10.1039/d5dt01626f

data_7719562
_publ_section_title
;
 A systematic study of naphthyridine-derived ligands for well-defined
 silver(I) dimers.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13651
_journal_page_last               13657
_journal_paper_doi               10.1039/d5dt01626f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C42 H46 Ag2 N6, 2(B F4)'
_chemical_formula_sum            'C42 H46 Ag2 B2 F8 N6'
_chemical_formula_weight         1024.21
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-12-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-02 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.96840(10)
_cell_length_b                   20.96840(10)
_cell_length_c                   9.67490(10)
_cell_measurement_reflns_used    36133
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.3080
_cell_measurement_theta_min      2.9900
_cell_volume                     4253.80(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.118a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -124.00 -79.00   0.50    0.30    --  -49.35-125.00   0.00   90
  2  \w   -114.00 -25.00   0.50    0.30    --  -49.35 -57.00-150.00  178
  3  \w    -73.00  27.00   0.50    0.30    --  -49.35  57.00   0.00  200
  4  \w    -95.00 -14.00   0.50    1.20    --  -84.79  61.00  60.00  162
  5  \w    -53.00 -12.00   0.50    1.20    --  -84.79  61.00-120.00   82
  6  \w   -150.00 -66.00   0.50    1.20    --  -84.79 -61.00  90.00  168
  7  \w   -105.00 -30.00   0.50    1.20    --  -84.79  77.00 150.00  150
  8  \w    -67.00 -16.00   0.50    1.20    --  -84.79  77.00 -60.00  102
  9  \w   -154.00 -59.00   0.50    1.20    --  -84.79 -30.00 -30.00  190
 10  \w   -141.00-105.00   0.50    1.20    --  -84.79 -95.00 150.00   72
 11  \w   -116.00 -82.00   0.50    1.20    --  -84.79  77.00 -60.00   68
 12  \w    -66.00 -26.00   0.50    1.20    --  -84.79 125.00 120.00   80
 13  \w     94.00 120.00   0.50    1.20    --  111.35  61.00-120.00   52
 14  \w    107.00 133.00   0.50    1.20    --  111.35  61.00 150.00   52
 15  \w     48.00  86.00   0.50    1.20    --  111.35 -77.00 120.00   76
 16  \w     58.00 112.00   0.50    1.20    --  111.35-125.00 150.00  108
 17  \w     81.00 152.00   0.50    1.20    --  111.35  30.00 120.00  142
 18  \w     42.00 177.00   0.50    1.20    --  111.35  15.00   0.00  270
 19  \w    150.00 176.00   0.50    1.20    --  111.35  45.00  30.00   52
 20  \w     42.00 103.00   0.50    1.20    --  111.35 -95.00 -30.00  122
 21  \w     99.00 133.00   0.50    1.20    --  111.35  45.00  30.00   68
 22  \w     47.00 105.00   0.50    1.20    --  111.35 -95.00 -60.00  116
 23  \w     74.00 102.00   0.50    1.20    --  111.35 -95.00-150.00   56
 24  \w    110.00 173.00   0.50    1.20    --  111.35  45.00-150.00  126
 25  \w     43.00 112.00   0.50    1.20    --  111.35-125.00-150.00  138
 26  \w     38.00 102.00   0.50    1.20    --  111.35 -95.00   0.00  128
 27  \w     45.00 111.00   0.50    1.20    --  111.35-125.00-120.00  132
 28  \w    106.00 132.00   0.50    1.20    --  111.35 -61.00 -30.00   52
 29  \w     48.00  86.00   0.50    1.20    --  111.35 -61.00 -30.00   76
 30  \w     75.00 103.00   0.50    1.20    --  111.35 -95.00  30.00   56
 31  \w    122.00 147.00   0.50    1.20    --  111.35  61.00-120.00   50
 32  \w    117.00 143.00   0.50    1.20    --  111.35 -77.00 120.00   52
 33  \w     37.00  71.00   0.50    1.20    --  111.35-125.00-180.00   68
 34  \w     85.00 103.00   0.50    1.20    --  111.35-125.00-180.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0106518000
_diffrn_orient_matrix_UB_12      0.0480947000
_diffrn_orient_matrix_UB_13      0.1181780000
_diffrn_orient_matrix_UB_21      0.0518787000
_diffrn_orient_matrix_UB_22      -0.0335695000
_diffrn_orient_matrix_UB_23      0.0861456000
_diffrn_orient_matrix_UB_31      0.0509063000
_diffrn_orient_matrix_UB_32      0.0442481000
_diffrn_orient_matrix_UB_33      -0.0630541000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            50885
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.654
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.118a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       needle
_exptl_crystal_F_000             2064
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+5.4814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4194
_reflns_number_total             4576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01626f2.cif
_cod_data_source_block           Cmpd_3
_cod_original_cell_volume        4253.80(6)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7719562
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Ag2C30N6B2F8
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C16, C16B}
3. Uiso/Uaniso restraints and constraints
Uanis(B1) = Uanis(B1B)
Uanis(F1) = Uanis(F1B)
Uanis(F2) = Uanis(F2B)
Uanis(F3) = Uanis(F3B)
Uanis(F4) = Uanis(F4B)
Uanis(C16) = Uanis(C16B)
Uanis(C17) = Uanis(C17B)
Uanis(C18) = Uanis(C18B)
Uanis(C17) = Uanis(C20)
Uanis(C18) = Uanis(C21)
4. Same fragment restrains
{B1B, F1B, F2B, F3B, F4B} sigma for 1-2: 0.02, 1-3: 0.04
{B1, F4, F3, F2, F1} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B1, F1, F2, F3, F4}
{C16B, C17B, C18B} sigma for 1-2: 0.02, 1-3: 0.04
{C16, C18, C17} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C16, C17, C18}
5. Others
 Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(B1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-
 FVAR(1)
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C16B(H16B), C19(H19)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              60922
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.851