Rationalization of the structural, electronic and photophysical properties of silver(I) halide <i>n</i>-picolylamine hybrid coordination polymers.
Zuffa, Caterina; Veclani, Daniele; Marchini, Marianna; Monti, Filippo; Cappuccino, Chiara; Maini, Lucia; Ventura, Barbara; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2799–2811; doi:10.1039/d4dt03003f

data_7718266
_publ_section_title
;
 Rationalization of the structural, electronic and photophysical
 properties of silver(I) halide <i>n</i>-picolylamine hybrid coordination
 polymers.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2799
_journal_page_last               2811
_journal_paper_doi               10.1039/d4dt03003f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C6 H8 Ag Cl N2'
_chemical_formula_sum            'C6 H8 Ag Cl N2'
_chemical_formula_weight         251.46
_chemical_name_systematic        '[(AgCl)(3-pica)]n'
_chemical_properties_physical    Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.918(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2824(5)
_cell_length_b                   6.0256(3)
_cell_length_c                   7.3134(6)
_cell_measurement_reflns_used    1209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5190
_cell_measurement_theta_min      4.0850
_cell_volume                     386.96(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.898
_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    -34.00  44.00   1.00   51.83    --  -16.52  57.00  60.00   78
  2  \w    -53.00  56.00   1.00   51.83    --  -16.52  19.00   0.00  109
  3  \w    -25.00  20.00   1.00   51.83    --  -16.52 -99.00  90.00   45
  4  \w    -20.00  19.00   1.00   51.83    --  -16.52 -99.00 -60.00   39
  5  \w    -77.00   0.00   1.00   51.83    --  -16.52 -57.00-180.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0930657000
_diffrn_orient_matrix_UB_12      -0.0205361000
_diffrn_orient_matrix_UB_13      0.0527827000
_diffrn_orient_matrix_UB_21      -0.0368828000
_diffrn_orient_matrix_UB_22      0.0164773000
_diffrn_orient_matrix_UB_23      0.0611047000
_diffrn_orient_matrix_UB_31      -0.0219522000
_diffrn_orient_matrix_UB_32      -0.1147703000
_diffrn_orient_matrix_UB_33      -0.0006832000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2965
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.898
_diffrn_reflns_theta_min         4.102
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             244
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Contact reaction'
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1647
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.707
_reflns_number_gt                1397
_reflns_number_total             1647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03003f2.cif
_cod_data_source_block           agcl_3pica_sol-liq_a
_cod_database_code               7718266
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C6 N2 H8 Ag1 Cl1'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.81(8)
 0.19(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C2(H2), C6(H6)
;
_shelx_res_checksum              70212
_shelx_hkl_checksum              98369
_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 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.688