#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:16:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179369 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/66/4326635.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_4326635
loop_
_publ_author_name
'Irene Bassanetti'
'Luciano Marchiò'
_publ_contact_author_address
;
Departimento di Chimica GIAF
Università di Parma
via Usberti 17/a, 43100, Parma, Italy
;
_publ_contact_author_email       marchio@unipr.it
_publ_contact_author_fax         '0039 0521 905557'
_publ_contact_author_name        'Dr. Luciano Marchiò'
_publ_contact_author_phone       '0039 0521 905419'
_publ_section_title
;
 Structural Variability in Ag(I) and Cu(I) Coordination Polymers with
 Thioether-Functionalized Bis(pyrazolyl)methane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10786
_journal_page_last               10797
_journal_paper_doi               10.1021/ic201338w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C14 H14 Ag N4 S 1+, B F4 1-'
_chemical_formula_sum            'C14 H14 Ag B F4 N4 S'
_chemical_formula_weight         465.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.979(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.901(1)
_cell_length_b                   17.268(2)
_cell_length_c                   11.510(1)
_cell_measurement_reflns_used    19445
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.17
_cell_volume                     1723.9(3)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart ApexII CCD'
_diffrn_measurement_method       'theta & 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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27694
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5272
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0682P)²+0.6793P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                4108
_reflns_number_total             5272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201338w_si_001_04.cif
_cod_data_source_block           ib114
_cod_database_code               4326635
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ag Ag 0.43022(3) 0.161212(14) 0.51295(2) 0.06531(11) Uani 1 1 d . . .
S13 S 0.32709(7) 0.22840(4) 0.09633(5) 0.04836(14) Uani 1 1 d . . .
N12 N 0.2751(2) 0.08838(11) 0.25317(18) 0.0443(4) Uani 1 1 d . . .
C33 C 0.1811(3) 0.26893(13) 0.1619(2) 0.0458(5) Uani 1 1 d . . .
N11 N 0.5475(2) 0.06196(11) 0.32176(17) 0.0428(4) Uani 1 1 d . . .
N22 N 0.2308(2) 0.12529(13) 0.34368(18) 0.0491(4) Uani 1 1 d . . .
N21 N 0.5834(2) 0.08546(12) 0.43767(18) 0.0486(4) Uani 1 1 d . . .
C23 C 0.4651(3) 0.18506(15) 0.2193(2) 0.0475(5) Uani 1 1 d . . .
H23A H 0.5682 0.1899 0.2054 0.057 Uiso 1 1 calc R . .
H23B H 0.4624 0.2121 0.2926 0.057 Uiso 1 1 calc R . .
C13 C 0.4271(3) 0.09955(13) 0.2314(2) 0.0429(4) Uani 1 1 d . . .
H13 H 0.4278 0.0748 0.1549 0.051 Uiso 1 1 calc R . .
C31 C 0.6435(3) 0.00593(15) 0.3017(2) 0.0511(5) Uani 1 1 d . . .
H31 H 0.6415 -0.0184 0.2293 0.061 Uiso 1 1 calc R . .
C32 C 0.1548(3) 0.05092(17) 0.1821(3) 0.0613(7) Uani 1 1 d . . .
H32 H 0.1574 0.0222 0.1142 0.074 Uiso 1 1 calc R . .
C21 C 0.7450(3) -0.00858(17) 0.4080(3) 0.0581(6) Uani 1 1 d . . .
H21 H 0.8246 -0.0446 0.4228 0.070 Uiso 1 1 calc R . .
C43 C 0.2156(3) 0.31718(16) 0.2600(2) 0.0557(6) Uani 1 1 d . . .
H43 H 0.3175 0.3287 0.2960 0.067 Uiso 1 1 calc R . .
C11 C 0.7034(3) 0.04189(16) 0.4887(2) 0.0543(6) Uani 1 1 d . . .
H11 H 0.7531 0.0450 0.5687 0.065 Uiso 1 1 calc R . .
C12 C 0.0814(3) 0.10978(18) 0.3287(3) 0.0594(6) Uani 1 1 d . . .
H12 H 0.0195 0.1276 0.3783 0.071 Uiso 1 1 calc R . .
C83 C 0.0300(3) 0.25245(18) 0.1065(3) 0.0617(7) Uani 1 1 d . . .
H83 H 0.0074 0.2196 0.0408 0.074 Uiso 1 1 calc R . .
C53 C 0.0954(5) 0.34815(19) 0.3038(3) 0.0727(9) Uani 1 1 d . . .
H53 H 0.1171 0.3797 0.3710 0.087 Uiso 1 1 calc R . .
C63 C -0.0542(5) 0.3329(2) 0.2495(4) 0.0837(11) Uani 1 1 d . . .
H63 H -0.1338 0.3543 0.2793 0.100 Uiso 1 1 calc R . .
C73 C -0.0872(4) 0.2860(2) 0.1510(4) 0.0827(10) Uani 1 1 d . . .
H73 H -0.1894 0.2764 0.1136 0.099 Uiso 1 1 calc R . .
C22 C 0.0302(3) 0.0634(2) 0.2290(3) 0.0709(8) Uani 1 1 d . . .
H22 H -0.0692 0.0447 0.2003 0.085 Uiso 1 1 calc R . .
B B 0.6282(6) 0.3796(3) 0.4416(5) 0.0858(12) Uani 1 1 d D . .
F2 F 0.6346(16) 0.3069(7) 0.4619(12) 0.188(5) Uani 0.655(11) 1 d P A 1
F1 F 0.4823(5) 0.4097(3) 0.4594(3) 0.0927(15) Uani 0.655(11) 1 d P A 1
F4 F 0.6066(5) 0.3866(5) 0.3161(5) 0.106(2) Uani 0.655(11) 1 d P A 1
F3 F 0.7361(13) 0.4173(8) 0.5019(12) 0.232(6) Uani 0.655(11) 1 d P A 1
F5 F 0.619(4) 0.3992(13) 0.551(2) 0.36(3) Uani 0.345(11) 1 d PD A 2
F6 F 0.613(2) 0.4188(11) 0.3515(19) 0.213(11) Uani 0.345(11) 1 d PD A 2
F8 F 0.7965(11) 0.3958(7) 0.4732(9) 0.095(3) Uani 0.345(11) 1 d PD A 2
F7 F 0.6052(15) 0.3002(6) 0.4522(10) 0.077(3) Uani 0.345(11) 1 d PD A 2
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'
S S 0.1246 0.1234 '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_3
N21 Ag N22 86.43(7) .
N21 Ag S13 162.25(6) 4_566
N22 Ag S13 104.43(5) 4_566
C33 S13 C23 105.17(11) .
C33 S13 Ag 103.72(8) 4_565
C23 S13 Ag 112.68(8) 4_565
N22 N12 C32 111.2(2) .
N22 N12 C13 121.14(19) .
C32 N12 C13 127.0(2) .
C43 C33 C83 121.1(3) .
C43 C33 S13 122.2(2) .
C83 C33 S13 116.7(2) .
C31 N11 N21 111.34(19) .
C31 N11 C13 126.0(2) .
N21 N11 C13 122.42(18) .
C12 N22 N12 105.1(2) .
C12 N22 Ag 133.80(19) .
N12 N22 Ag 117.12(15) .
C11 N21 N11 104.6(2) .
C11 N21 Ag 131.97(18) .
N11 N21 Ag 122.16(15) .
C13 C23 S13 110.17(17) .
C13 C23 H23A 109.6 .
S13 C23 H23A 109.6 .
C13 C23 H23B 109.6 .
S13 C23 H23B 109.6 .
H23A C23 H23B 108.1 .
N12 C13 N11 112.46(18) .
N12 C13 C23 112.37(18) .
N11 C13 C23 110.53(19) .
N12 C13 H13 107.0 .
N11 C13 H13 107.0 .
C23 C13 H13 107.0 .
N11 C31 C21 107.2(2) .
N11 C31 H31 126.4 .
C21 C31 H31 126.4 .
C22 C32 N12 106.9(3) .
C22 C32 H32 126.6 .
N12 C32 H32 126.6 .
C31 C21 C11 105.2(2) .
C31 C21 H21 127.4 .
C11 C21 H21 127.4 .
C33 C43 C53 118.7(3) .
C33 C43 H43 120.6 .
C53 C43 H43 120.6 .
N21 C11 C21 111.7(2) .
N21 C11 H11 124.1 .
C21 C11 H11 124.1 .
N22 C12 C22 110.8(3) .
N22 C12 H12 124.6 .
C22 C12 H12 124.6 .
C33 C83 C73 118.5(3) .
C33 C83 H83 120.7 .
C73 C83 H83 120.7 .
C63 C53 C43 120.8(3) .
C63 C53 H53 119.6 .
C43 C53 H53 119.6 .
C53 C63 C73 119.9(3) .
C53 C63 H63 120.0 .
C73 C63 H63 120.0 .
C63 C73 C83 120.9(3) .
C63 C73 H73 119.6 .
C83 C73 H73 119.6 .
C32 C22 C12 105.9(3) .
C32 C22 H22 127.0 .
C12 C22 H22 127.0 .
F6 B F3 96.1(13) .
F6 B F2 133.9(14) .
F3 B F2 114.7(9) .
F6 B F5 130.4(15) .
F3 B F5 62.5(10) .
F2 B F5 95.0(13) .
F6 B F7 129.0(13) .
F3 B F7 125.4(8) .
F2 B F7 11.1(10) .
F5 B F7 97.3(10) .
F6 B F4 28.8(12) .
F3 B F4 115.9(8) .
F2 B F4 105.1(8) .
F5 B F4 157.3(15) .
F7 B F4 100.6(7) .
F6 B F1 89.5(11) .
F3 B F1 109.8(9) .
F2 B F1 109.3(7) .
F5 B F1 61.7(16) .
F7 B F1 100.7(7) .
F4 B F1 101.1(4) .
F6 B F8 90.8(11) .
F3 B F8 31.9(9) .
F2 B F8 98.0(8) .
F5 B F8 89.7(14) .
F7 B F8 108.8(8) .
F4 B F8 97.5(5) .
F1 B F8 141.3(7) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag N21 2.203(2) .
Ag N22 2.404(2) .
Ag S13 2.4069(7) 4_566
S13 C33 1.786(2) .
S13 C23 1.814(2) .
S13 Ag 2.4069(7) 4_565
N12 N22 1.353(3) .
N12 C32 1.356(3) .
N12 C13 1.443(3) .
C33 C43 1.381(4) .
C33 C83 1.382(4) .
N11 C31 1.345(3) .
N11 N21 1.362(3) .
N11 C13 1.467(3) .
N22 C12 1.329(3) .
N21 C11 1.330(3) .
C23 C13 1.528(3) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C13 H13 0.9800 .
C31 C21 1.371(4) .
C31 H31 0.9300 .
C32 C22 1.355(4) .
C32 H32 0.9300 .
C21 C11 1.383(4) .
C21 H21 0.9300 .
C43 C53 1.389(5) .
C43 H43 0.9300 .
C11 H11 0.9300 .
C12 C22 1.391(5) .
C12 H12 0.9300 .
C83 C73 1.388(5) .
C83 H83 0.9300 .
C53 C63 1.364(6) .
C53 H53 0.9300 .
C63 C73 1.371(6) .
C63 H63 0.9300 .
C73 H73 0.9300 .
C22 H22 0.9300 .
B F6 1.221(13) .
B F3 1.236(10) .
B F2 1.276(12) .
B F5 1.325(15) .
B F7 1.395(11) .
B F4 1.419(8) .
B F1 1.456(7) .
B F8 1.487(10) .
