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_7719567
_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         'C44 H50 Ag2 N6, 2(B F4)'
_chemical_formula_sum            'C44 H50 Ag2 B2 F8 N6'
_chemical_formula_weight         1052.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-05-10
_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                 106.7410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.83440(10)
_cell_length_b                   15.83940(10)
_cell_length_c                   14.61290(10)
_cell_measurement_reflns_used    24117
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.3770
_cell_measurement_theta_min      4.2340
_cell_volume                     2179.79(3)
_computing_cell_refinement       'CrysAlisPro 1.171.44.92a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.92a 64-bit (release 31-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.92a (Rigaku OD, 2025)'
_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 0.988
_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   -116.00 -14.00   0.50    0.10    --  -84.76  77.00-120.00  204
  2  \w    -78.00  24.00   0.50    0.10    --  -47.12  77.00  60.00  204
  3  \w   -116.00 -14.00   0.50    0.10    --  -84.76  77.00 120.00  204
  4  \w   -110.00  -8.00   0.50    0.10    --  -84.76  61.00  30.00  204
  5  \w   -165.00 -63.00   0.50    0.10    --  -88.00 -60.00 167.96  204
  6  \w   -118.00 -16.00   0.50    0.10    --  -47.12 -77.00 -60.00  204
  7  \w   -158.00 -83.00   0.50    0.10    --  -84.76 -95.00  90.00  150
  8  \w   -148.00 -46.00   0.50    0.10    --  -72.00 -63.00  35.04  204
  9  \w   -148.00 -46.00   0.50    0.10    --  -72.00 -63.00  35.04  204
 10  \w     92.00 178.00   0.50    0.10    --  111.42  45.00 120.00  172
 11  \w     87.00 178.00   0.50    0.10    --  111.42  61.00 150.00  182
 12  \w     92.00 178.00   0.50    0.10    --  111.42  45.00 -90.00  172
 13  \w     92.00 178.00   0.50    0.10    --  111.42  45.00-120.00  172
 14  \w     92.00 178.00   0.50    0.10    --  111.42  45.00-150.00  172
 15  \w     41.00 143.00   0.50    0.10    --   72.00  77.00-105.79  204
 16  \w     95.00 178.00   0.50    0.10    --  111.42 125.00 -30.00  166
 17  \w     17.00  43.00   0.50    0.10    --   56.00  90.00 122.69   52
 18  \w     31.00 131.00   0.50    0.10    --  111.42 -45.00 120.00  200
 19  \w     31.00 131.00   0.50    0.10    --  111.42 -45.00 120.00  200
 20  \w     41.00 143.00   0.50    0.10    --  111.42 -77.00-180.00  204
 21  \w     31.00 131.00   0.50    0.10    --  111.42 -45.00 -90.00  200
 22  \w     31.00 131.00   0.50    0.10    --  111.42 -45.00 -90.00  200
 23  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00-180.00  134
 24  \w     39.00 106.00   0.50    0.10    --  113.75-101.00 -96.61  134
 25  \w     42.00 110.00   0.50    0.10    --  113.75-122.00 -45.70  136
 26  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00 -30.00  134
 27  \w     36.00 112.00   0.50    0.10    --  111.42-125.00  90.00  152
 28  \w     36.00 112.00   0.50    0.10    --  111.42-125.00 150.00  152
 29  \w     36.00 112.00   0.50    0.10    --  111.42-125.00 150.00  152
 30  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00 150.00  134
 31  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00  90.00  134
 32  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00  30.00  134
 33  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00 -30.00  134
 34  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00 -60.00  134
 35  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00   0.00  134
 36  \w     38.00 105.00   0.50    0.10    --  111.42 -95.00   0.00  134
;
_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      0.1185207000
_diffrn_orient_matrix_UB_12      -0.0147283000
_diffrn_orient_matrix_UB_13      -0.0478636000
_diffrn_orient_matrix_UB_21      0.0751353000
_diffrn_orient_matrix_UB_22      -0.0603333000
_diffrn_orient_matrix_UB_23      0.0815969000
_diffrn_orient_matrix_UB_31      -0.0839498000
_diffrn_orient_matrix_UB_32      -0.0748594000
_diffrn_orient_matrix_UB_33      -0.0563953000
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45129
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.418
_diffrn_reflns_theta_min         4.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.92a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_refine_diff_density_max         0.596
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4690
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0384P)^2^+2.1835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4435
_reflns_number_total             4690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01626f2.cif
_cod_data_source_block           Cmpd_4
_cod_database_code               7719567
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Ag2C30N4B2F8
_diffrn_oxdiff_digest_od_ed
;

;
_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. 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)
3. 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}
4. Others
 Sof(B1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              99674
_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 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.773