#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/30/4303044.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4303044
loop_
_publ_author_name
'Brendan J. Liddle'
'Daniel Hall'
'Sergey V. Lindeman'
'Mark D. Smith'
'James R. Gardinier'
_publ_section_title
;
Manipulating Self-Assembly in Silver(I) Complexes of
1,3-Di-N-pyrazolylorganyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8404
_journal_page_last               8414
_journal_paper_doi               10.1021/ic900982m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C22 H30 Ag2 B2 F8 N10'
_chemical_formula_weight         823.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5138(11)
_cell_length_b                   7.1001(8)
_cell_length_c                   20.081(2)
_cell_measurement_reflns_used    6357
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      3
_cell_volume                     1498.7(3)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v1.0-27 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24017
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.96
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS. Program for empirical absorption correction of
 area-detector data. University of Goetingen. Germany. 
 Sheldrick, G. M. 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0298P)²+0.8778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                4390
_reflns_number_total             4885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900982m_si_001_2.cif
_cod_data_source_block           1_CH3CN
_cod_database_code               4303044
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag -0.012524(12) 0.834784(19) -0.070495(6) 0.02703(5) Uani 1 1 d . . .
N11 N -0.14836(12) 0.95012(19) -0.14527(7) 0.0224(2) Uani 1 1 d . . .
N12 N -0.27043(12) 1.0083(2) -0.13834(7) 0.0243(3) Uani 1 1 d . . .
N22 N -0.15561(13) 1.32155(18) -0.04968(7) 0.0220(2) Uani 1 1 d . . .
N21 N -0.03652(13) 1.27328(19) -0.02845(6) 0.0221(2) Uani 1 1 d . . .
C11 C -0.11453(16) 1.0130(2) -0.20519(8) 0.0242(3) Uani 1 1 d . . .
H11 H -0.0333 0.9935 -0.2238 0.029 Uiso 1 1 calc R . .
C12 C -0.21378(18) 1.1107(2) -0.23663(8) 0.0277(3) Uani 1 1 d . . .
H12 H -0.2139 1.1686 -0.2793 0.033 Uiso 1 1 calc R . .
C13 C -0.31146(17) 1.1048(3) -0.19244(9) 0.0290(3) Uani 1 1 d . . .
H13 H -0.3934 1.1592 -0.1989 0.035 Uiso 1 1 calc R . .
C1 C -0.34202(17) 0.9644(3) -0.07866(9) 0.0311(4) Uani 1 1 d . . .
H1B H -0.3465 0.8258 -0.0738 0.037 Uiso 1 1 calc R . .
H1A H -0.4301 1.0115 -0.0850 0.037 Uiso 1 1 calc R . .
C2 C -0.28640(16) 1.0471(2) -0.01460(8) 0.0269(3) Uani 1 1 d . . .
H2A H -0.2029 0.9869 -0.0054 0.032 Uiso 1 1 calc R . .
H2B H -0.3428 1.0130 0.0223 0.032 Uiso 1 1 calc R . .
C3 C -0.26786(15) 1.2598(2) -0.01384(8) 0.0252(3) Uani 1 1 d . . .
H3A H -0.3442 1.3204 -0.0341 0.030 Uiso 1 1 calc R . .
H3B H -0.2601 1.3029 0.0330 0.030 Uiso 1 1 calc R . .
C23 C -0.15185(19) 1.4257(2) -0.10542(8) 0.0290(3) Uani 1 1 d . . .
H23 H -0.2232 1.4755 -0.1294 0.035 Uiso 1 1 calc R . .
C22 C -0.0263(2) 1.4474(2) -0.12165(8) 0.0312(4) Uani 1 1 d . . .
H22 H 0.0065 1.5144 -0.1584 0.037 Uiso 1 1 calc R . .
C21 C 0.04264(18) 1.3498(2) -0.07245(8) 0.0271(3) Uani 1 1 d . . .
H21 H 0.1327 1.3391 -0.0704 0.032 Uiso 1 1 calc R . .
F1 F 0.30353(11) 0.50108(18) -0.12974(7) 0.0443(3) Uani 1 1 d . . .
F2 F 0.52031(12) 0.5097(2) -0.13056(7) 0.0468(3) Uani 1 1 d . . .
F3 F 0.41197(14) 0.2832(3) -0.18458(10) 0.0772(6) Uani 1 1 d . . .
F4 F 0.42053(19) 0.2897(3) -0.07186(11) 0.0889(7) Uani 1 1 d . . .
B1 B 0.4135(2) 0.3964(3) -0.12801(11) 0.0312(4) Uani 1 1 d . . .
N1S N 0.16281(15) 0.8943(3) -0.14153(8) 0.0368(4) Uani 1 1 d . . .
C1S C 0.24399(17) 0.8769(3) -0.17737(9) 0.0297(3) Uani 1 1 d . . .
C2S C 0.34792(19) 0.8547(3) -0.22340(10) 0.0364(4) Uani 1 1 d . . .
H2S1 H 0.4153 0.7782 -0.2025 0.055 Uiso 1 1 calc R . .
H2S2 H 0.3820 0.9789 -0.2347 0.055 Uiso 1 1 calc R . .
H2S3 H 0.3165 0.7922 -0.2640 0.055 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 Ag1 N11 152.48(5) 3_575 . ?
N21 Ag1 N1S 115.80(5) 3_575 . ?
N11 Ag1 N1S 91.40(5) . . ?
C11 N11 N12 105.12(13) . . ?
C11 N11 Ag1 123.68(10) . . ?
N12 N11 Ag1 129.93(10) . . ?
C13 N12 N11 111.01(13) . . ?
C13 N12 C1 127.42(15) . . ?
N11 N12 C1 121.57(14) . . ?
C23 N22 N21 110.91(14) . . ?
C23 N22 C3 127.87(15) . . ?
N21 N22 C3 121.22(13) . . ?
C21 N21 N22 105.79(13) . . ?
C21 N21 Ag1 127.19(12) . 3_575 ?
N22 N21 Ag1 124.95(10) . 3_575 ?
N11 C11 C12 111.24(15) . . ?
C13 C12 C11 104.81(15) . . ?
N12 C13 C12 107.81(15) . . ?
N12 C1 C2 114.56(14) . . ?
C1 C2 C3 116.03(15) . . ?
N22 C3 C2 113.36(13) . . ?
N22 C23 C22 107.75(16) . . ?
C23 C22 C21 105.24(15) . . ?
N21 C21 C22 110.30(16) . . ?
F4 B1 F1 110.67(18) . . ?
F4 B1 F2 108.99(18) . . ?
F1 B1 F2 111.61(17) . . ?
F4 B1 F3 110.7(2) . . ?
F1 B1 F3 107.30(17) . . ?
F2 B1 F3 107.48(17) . . ?
C1S N1S Ag1 163.44(18) . . ?
N1S C1S C2S 179.9(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N21 2.1811(13) 3_575 ?
Ag1 N11 2.2070(13) . ?
Ag1 N1S 2.3930(16) . ?
N11 C11 1.339(2) . ?
N11 N12 1.3584(18) . ?
N12 C13 1.347(2) . ?
N12 C1 1.463(2) . ?
N22 C23 1.343(2) . ?
N22 N21 1.3577(19) . ?
N22 C3 1.463(2) . ?
N21 C21 1.342(2) . ?
N21 Ag1 2.1812(13) 3_575 ?
C11 C12 1.393(2) . ?
C12 C13 1.373(3) . ?
C1 C2 1.519(2) . ?
C2 C3 1.523(2) . ?
C23 C22 1.375(3) . ?
C22 C21 1.396(3) . ?
F1 B1 1.374(2) . ?
F2 B1 1.383(2) . ?
F3 B1 1.392(3) . ?
F4 B1 1.359(3) . ?
N1S C1S 1.135(2) . ?
C1S C2S 1.455(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139127012
