#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:16:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179369 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/66/4326637.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_4326637
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         'C18 H22 Ag N4 S 1+, P F6 1-'
_chemical_formula_sum            'C18 H22 Ag F6 N4 P S'
_chemical_formula_weight         579.30
_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                 100.521(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.672(1)
_cell_length_b                   19.400(2)
_cell_length_c                   12.301(1)
_cell_measurement_reflns_used    16170
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      1.98
_cell_volume                     2269.3(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30119
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0499P)²+0.3546P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                3723
_reflns_number_total             5297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201338w_si_001_06.cif
_cod_data_source_block           ib187ae
_cod_database_code               4326637
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 0.37962(3) 0.194525(16) 0.53563(2) 0.05391(14) Uani 1 1 d . . .
S13 S 0.29970(11) 0.22308(5) 0.15775(8) 0.0495(2) Uani 1 1 d . . .
N11 N 0.5153(3) 0.09102(15) 0.3829(2) 0.0452(7) Uani 1 1 d . . .
N21 N 0.5446(3) 0.12907(16) 0.4776(3) 0.0482(8) Uani 1 1 d . . .
C31 C 0.6036(4) 0.03597(19) 0.3871(4) 0.0513(10) Uani 1 1 d . . .
C13 C 0.4093(4) 0.11401(19) 0.2922(3) 0.0440(8) Uani 1 1 d . . .
H13 H 0.4184 0.0857 0.2279 0.053 Uiso 1 1 calc R . .
N22 N 0.2288(3) 0.13248(15) 0.4052(2) 0.0446(7) Uani 1 1 d . . .
N12 N 0.2684(3) 0.10311(15) 0.3143(2) 0.0434(7) Uani 1 1 d . . .
C22 C 0.0498(5) 0.0738(2) 0.3069(4) 0.0630(11) Uani 1 1 d . . .
H22 H -0.0394 0.0549 0.2853 0.076 Uiso 1 1 calc R . .
C12 C 0.0960(4) 0.1139(2) 0.4008(3) 0.0526(10) Uani 1 1 d . . .
C52 C 0.1704(5) 0.0325(3) 0.1468(4) 0.0784(14) Uani 1 1 d . . .
H52A H 0.0827 0.0103 0.1177 0.118 Uiso 1 1 calc R . .
H52B H 0.2439 -0.0014 0.1598 0.118 Uiso 1 1 calc R . .
H52C H 0.1913 0.0659 0.0946 0.118 Uiso 1 1 calc R . .
C51 C 0.5984(5) -0.0144(2) 0.2946(4) 0.0740(13) Uani 1 1 d . . .
H51A H 0.5039 -0.0310 0.2726 0.111 Uiso 1 1 calc R . .
H51B H 0.6599 -0.0524 0.3188 0.111 Uiso 1 1 calc R . .
H51C H 0.6279 0.0079 0.2330 0.111 Uiso 1 1 calc R . .
C32 C 0.1598(4) 0.0678(2) 0.2536(3) 0.0540(10) Uani 1 1 d . . .
C21 C 0.6898(4) 0.0390(2) 0.4879(4) 0.0605(11) Uani 1 1 d . . .
H21 H 0.7608 0.0080 0.5156 0.073 Uiso 1 1 calc R . .
C23 C 0.4390(4) 0.18878(18) 0.2633(3) 0.0440(8) Uani 1 1 d . . .
H23A H 0.5275 0.1909 0.2370 0.053 Uiso 1 1 calc R . .
H23B H 0.4477 0.2170 0.3293 0.053 Uiso 1 1 calc R . .
C33 C 0.2009(4) 0.2707(2) 0.2411(3) 0.0564(11) Uani 1 1 d . . .
C11 C 0.6518(4) 0.0969(2) 0.5411(3) 0.0540(10) Uani 1 1 d . . .
C42 C 0.0180(5) 0.1374(3) 0.4885(4) 0.0825(16) Uani 1 1 d . . .
H42A H 0.0379 0.1852 0.5045 0.124 Uiso 1 1 calc R . .
H42B H 0.0471 0.1106 0.5543 0.124 Uiso 1 1 calc R . .
H42C H -0.0812 0.1315 0.4630 0.124 Uiso 1 1 calc R . .
C41 C 0.7141(5) 0.1258(3) 0.6513(4) 0.0814(15) Uani 1 1 d . . .
H41A H 0.7337 0.1739 0.6438 0.122 Uiso 1 1 calc R . .
H41B H 0.7998 0.1018 0.6801 0.122 Uiso 1 1 calc R . .
H41C H 0.6490 0.1202 0.7009 0.122 Uiso 1 1 calc R . .
C73 C -0.0108(7) 0.2908(4) 0.3123(6) 0.106(2) Uani 1 1 d . . .
H73 H -0.1033 0.2797 0.3162 0.127 Uiso 1 1 calc R . .
C83 C 0.0637(5) 0.2522(3) 0.2412(4) 0.0804(16) Uani 1 1 d . . .
H83 H 0.0209 0.2163 0.1974 0.097 Uiso 1 1 calc R . .
C43 C 0.2641(6) 0.3250(3) 0.3056(4) 0.0721(13) Uani 1 1 d . . .
H43 H 0.3572 0.3365 0.3046 0.087 Uiso 1 1 calc R . .
C53 C 0.1887(8) 0.3616(3) 0.3708(5) 0.101(2) Uani 1 1 d . . .
H53 H 0.2299 0.3986 0.4127 0.122 Uiso 1 1 calc R . .
C63 C 0.0554(9) 0.3437(5) 0.3737(6) 0.116(3) Uani 1 1 d . . .
H63 H 0.0063 0.3683 0.4193 0.139 Uiso 1 1 calc R . .
P P 0.66938(16) 0.36697(9) 0.53020(13) 0.0875(5) Uani 1 1 d D . .
F1 F 0.6264(18) 0.3895(8) 0.4113(8) 0.142(6) Uani 0.597(17) 1 d PD A 1
F2 F 0.8012(17) 0.3322(14) 0.5093(18) 0.244(11) Uani 0.597(17) 1 d PD A 1
F4 F 0.7187(14) 0.3474(11) 0.6550(9) 0.165(8) Uani 0.597(17) 1 d PD A 1
F3 F 0.5394(15) 0.4020(7) 0.5627(10) 0.152(6) Uani 0.597(17) 1 d PD A 1
F5 F 0.5863(18) 0.3021(5) 0.5205(12) 0.156(6) Uani 0.597(17) 1 d PD A 1
F6 F 0.752(2) 0.4366(8) 0.5552(10) 0.198(9) Uani 0.597(17) 1 d PD A 1
F7 F 0.5144(14) 0.348(2) 0.5285(16) 0.222(17) Uani 0.403(17) 1 d PD A 2
F10 F 0.711(5) 0.2943(10) 0.555(3) 0.33(2) Uani 0.403(17) 1 d PD A 2
F8 F 0.8186(16) 0.3859(16) 0.5267(15) 0.159(10) Uani 0.403(17) 1 d PD A 2
F9 F 0.644(3) 0.346(2) 0.4058(14) 0.237(16) Uani 0.403(17) 1 d PD A 2
F11 F 0.620(4) 0.4374(13) 0.491(3) 0.29(2) Uani 0.403(17) 1 d PD A 2
F12 F 0.684(2) 0.3842(13) 0.6517(13) 0.162(12) Uani 0.403(17) 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'
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'
P P 0.1023 0.0942 '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 83.10(11) .
N21 Ag S13 153.50(8) 4_566
N22 Ag S13 123.07(8) 4_566
C33 S13 C23 100.61(18) .
C33 S13 Ag 106.33(14) 4_565
C23 S13 Ag 114.01(12) 4_565
C31 N11 N21 111.1(3) .
C31 N11 C13 128.7(3) .
N21 N11 C13 120.1(3) .
C11 N21 N11 105.4(3) .
C11 N21 Ag 126.7(3) .
N11 N21 Ag 121.8(2) .
N11 C31 C21 106.0(4) .
N11 C31 C51 123.3(4) .
C21 C31 C51 130.6(4) .
N11 C13 N12 111.7(3) .
N11 C13 C23 109.6(3) .
N12 C13 C23 113.7(3) .
N11 C13 H13 107.2 .
N12 C13 H13 107.2 .
C23 C13 H13 107.2 .
C12 N22 N12 105.4(3) .
C12 N22 Ag 131.1(3) .
N12 N22 Ag 123.4(2) .
C32 N12 N22 110.8(3) .
C32 N12 C13 128.9(3) .
N22 N12 C13 120.2(3) .
C32 C22 C12 106.7(4) .
C32 C22 H22 126.6 .
C12 C22 H22 126.6 .
N22 C12 C22 110.3(3) .
N22 C12 C42 120.0(4) .
C22 C12 C42 129.7(4) .
C32 C52 H52A 109.5 .
C32 C52 H52B 109.5 .
H52A C52 H52B 109.5 .
C32 C52 H52C 109.5 .
H52A C52 H52C 109.5 .
H52B C52 H52C 109.5 .
C31 C51 H51A 109.5 .
C31 C51 H51B 109.5 .
H51A C51 H51B 109.5 .
C31 C51 H51C 109.5 .
H51A C51 H51C 109.5 .
H51B C51 H51C 109.5 .
C22 C32 N12 106.7(4) .
C22 C32 C52 130.5(4) .
N12 C32 C52 122.8(4) .
C31 C21 C11 107.1(4) .
C31 C21 H21 126.4 .
C11 C21 H21 126.4 .
C13 C23 S13 111.5(3) .
C13 C23 H23A 109.3 .
S13 C23 H23A 109.3 .
C13 C23 H23B 109.3 .
S13 C23 H23B 109.3 .
H23A C23 H23B 108.0 .
C83 C33 C43 121.4(5) .
C83 C33 S13 119.0(4) .
C43 C33 S13 119.6(3) .
N21 C11 C21 110.4(4) .
N21 C11 C41 120.0(4) .
C21 C11 C41 129.6(4) .
C12 C42 H42A 109.5 .
C12 C42 H42B 109.5 .
H42A C42 H42B 109.5 .
C12 C42 H42C 109.5 .
H42A C42 H42C 109.5 .
H42B C42 H42C 109.5 .
C11 C41 H41A 109.5 .
C11 C41 H41B 109.5 .
H41A C41 H41B 109.5 .
C11 C41 H41C 109.5 .
H41A C41 H41C 109.5 .
H41B C41 H41C 109.5 .
C63 C73 C83 119.5(6) .
C63 C73 H73 120.3 .
C83 C73 H73 120.3 .
C33 C83 C73 117.1(6) .
C33 C83 H83 121.5 .
C73 C83 H83 121.5 .
C53 C43 C33 119.9(6) .
C53 C43 H43 120.0 .
C33 C43 H43 120.0 .
C63 C53 C43 119.7(7) .
C63 C53 H53 120.2 .
C43 C53 H53 120.2 .
C53 C63 C73 122.5(7) .
C53 C63 H63 118.8 .
C73 C63 H63 118.8 .
F10 P F5 48.2(13) .
F10 P F11 173.1(19) .
F5 P F11 127.5(15) .
F10 P F8 90.8(15) .
F5 P F8 135.7(11) .
F11 P F8 91.3(12) .
F10 P F2 53.5(14) .
F5 P F2 94.0(10) .
F11 P F2 125.9(12) .
F8 P F2 41.8(9) .
F10 P F1 119.6(15) .
F5 P F1 96.8(8) .
F11 P F1 53.9(14) .
F8 P F1 89.9(10) .
F2 P F1 93.2(10) .
F10 P F12 91.7(14) .
F5 P F12 102.6(10) .
F11 P F12 94.7(15) .
F8 P F12 93.2(10) .
F2 P F12 109.7(12) .
F1 P F12 148.5(11) .
F10 P F7 89.8(14) .
F5 P F7 44.1(12) .
F11 P F7 87.9(14) .
F8 P F7 177.6(9) .
F2 P F7 137.7(15) .
F1 P F7 87.8(8) .
F12 P F7 89.1(11) .
F10 P F3 124.5(16) .
F5 P F3 86.5(6) .
F11 P F3 56.8(10) .
F8 P F3 137.2(11) .
F2 P F3 174.9(9) .
F1 P F3 91.7(8) .
F12 P F3 65.3(10) .
F7 P F3 43.6(13) .
F10 P F9 86.7(17) .
F5 P F9 73.3(14) .
F11 P F9 86.7(13) .
F8 P F9 90.9(12) .
F2 P F9 72.6(15) .
F1 P F9 32.9(14) .
F12 P F9 175.6(13) .
F7 P F9 86.8(13) .
F3 P F9 112.3(14) .
F10 P F4 62.8(14) .
F5 P F4 86.4(8) .
F11 P F4 123.8(16) .
F8 P F4 88.0(9) .
F2 P F4 86.8(9) .
F1 P F4 176.8(8) .
F12 P F4 29.4(9) .
F7 P F4 94.3(7) .
F3 P F4 88.3(7) .
F9 P F4 149.5(15) .
F10 P F6 132.0(15) .
F5 P F6 172.7(7) .
F11 P F6 53.1(13) .
F8 P F6 48.5(8) .
F2 P F6 90.3(9) .
F1 P F6 88.9(6) .
F12 P F6 70.3(9) .
F7 P F6 132.0(15) .
F3 P F6 88.7(9) .
F9 P F6 113.8(13) .
F4 P F6 87.9(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag N21 2.255(3) .
Ag N22 2.301(3) .
Ag S13 2.4152(10) 4_566
S13 C33 1.782(4) .
S13 C23 1.817(4) .
S13 Ag 2.4152(10) 4_565
N11 C31 1.362(5) .
N11 N21 1.365(4) .
N11 C13 1.441(4) .
N21 C11 1.333(5) .
C31 C21 1.363(6) .
C31 C51 1.494(6) .
C13 N12 1.454(4) .
C13 C23 1.533(5) .
C13 H13 0.9800 .
N22 C12 1.326(5) .
N22 N12 1.370(4) .
N12 C32 1.358(5) .
C22 C32 1.353(6) .
C22 C12 1.397(6) .
C22 H22 0.9300 .
C12 C42 1.496(6) .
C52 C32 1.501(6) .
C52 H52A 0.9600 .
C52 H52B 0.9600 .
C52 H52C 0.9600 .
C51 H51A 0.9600 .
C51 H51B 0.9600 .
C51 H51C 0.9600 .
C21 C11 1.383(6) .
C21 H21 0.9300 .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C33 C83 1.375(6) .
C33 C43 1.391(7) .
C11 C41 1.488(6) .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C73 C63 1.362(10) .
C73 C83 1.440(9) .
C73 H73 0.9300 .
C83 H83 0.9300 .
C43 C53 1.377(7) .
C43 H43 0.9300 .
C53 C63 1.342(9) .
C53 H53 0.9300 .
C63 H63 0.9300 .
P F10 1.483(14) .
P F5 1.487(8) .
P F11 1.497(13) .
P F8 1.498(12) .
P F2 1.506(12) .
P F1 1.510(9) .
P F12 1.513(12) .
P F7 1.542(11) .
P F3 1.544(9) .
P F9 1.560(15) .
P F4 1.569(9) .
P F6 1.569(9) .
