#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:54:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179459 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/56/4335657.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_4335657
loop_
_publ_author_name
'Ting Hu'
'Thomas C. W. Mak'
_publ_section_title
;
 Silver(I) Multiple Salts Assembled with Phosphonate,
 Perfluorocarboxylate, and the Multinuclear Silver-Ethynediide
 Supramolecular Synthon
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9066
_journal_page_last               9076
_journal_paper_doi               10.1021/ic401259r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C12 H18 Ag7 F3 O8 P2'
_chemical_formula_weight         1164.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.1940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6770(4)
_cell_length_b                   28.777(2)
_cell_length_c                   14.4277(11)
_cell_measurement_reflns_used    20159
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.843
_cell_measurement_theta_min      2.839
_cell_volume                     2326.7(3)
_computing_cell_refinement       SAINT(Bruker,2001)
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        APEX2(Bruker,2003)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18645
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    5.966
_exptl_absorpt_correction_T_max  0.5868
_exptl_absorpt_correction_T_min  0.4486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.324
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.379
_refine_diff_density_min         -1.821
_refine_diff_density_rms         0.255
_refine_ls_extinction_coef       0.00204(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0488
_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)+(0.0674P)²+37.0124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                2386
_reflns_number_total             2759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401259r_si_002_5.cif
_cod_data_source_block           5
_cod_database_code               4335657
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ag4 Ag 0.63892(12) 0.02409(3) 0.88856(5) 0.0460(2) Uani 1 1 d .
Ag1 Ag 0.77360(11) -0.08566(2) 0.79293(4) 0.0379(2) Uani 1 1 d .
Ag2 Ag 0.73033(11) -0.04493(2) 0.60515(4) 0.0374(2) Uani 1 1 d .
Ag3 Ag 1.0000 0.00906(3) 0.7500 0.0351(2) Uani 1 2 d S
C1 C 0.5968(14) -0.0204(3) 0.7352(5) 0.0290(14) Uani 1 1 d .
C2 C 1.0000 -0.1766(4) 0.7500 0.058(4) Uani 1 2 d SD
C3 C 1.0000 -0.2311(8) 0.7500 0.109(7) Uani 1 2 d SDU
C4 C 0.7482(12) 0.1343(2) 0.5609(5) 0.0251(13) Uani 1 1 d .
C5 C 0.6395(18) 0.1315(3) 0.6515(6) 0.0424(19) Uani 1 1 d .
H5A H 0.7548 0.1187 0.7009 0.064 Uiso 1 1 calc R
H5B H 0.5008 0.1119 0.6414 0.064 Uiso 1 1 calc R
H5C H 0.5950 0.1620 0.6690 0.064 Uiso 1 1 calc R
C6 C 0.5562(16) 0.1518(3) 0.4794(6) 0.043(2) Uani 1 1 d .
H6A H 0.4859 0.1799 0.4981 0.065 Uiso 1 1 calc R
H6B H 0.4348 0.1285 0.4648 0.065 Uiso 1 1 calc R
H6C H 0.6294 0.1577 0.4250 0.065 Uiso 1 1 calc R
C7 C 0.9589(17) 0.1677(3) 0.5748(9) 0.053(3) Uani 1 1 d .
H7A H 0.9097 0.1970 0.5972 0.080 Uiso 1 1 calc R
H7B H 1.0149 0.1722 0.5161 0.080 Uiso 1 1 calc R
H7C H 1.0850 0.1549 0.6199 0.080 Uiso 1 1 calc R
F1 F 0.800(3) -0.2494(5) 0.7499(14) 0.182(6) Uani 1 1 d DU
F2 F 1.003(5) -0.2442(8) 0.6554(15) 0.137(7) Uani 0.50 1 d PDU
O1 O 0.8228(18) -0.1593(2) 0.7707(8) 0.079(3) Uani 1 1 d .
O2 O 1.0171(9) 0.0591(2) 0.6203(3) 0.0303(11) Uani 1 1 d .
O3 O 0.6277(9) 0.04428(17) 0.5130(4) 0.0272(10) Uani 1 1 d .
O4 O 0.9753(9) 0.07975(18) 0.4483(3) 0.0285(10) Uani 1 1 d .
P1 P 0.8477(3) 0.07626(6) 0.53419(11) 0.0193(3) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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'
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
O2 Ag4 O3 126.19(19) 2_756 2_656
O2 Ag4 C1 125.9(2) 2_756 2_656
O3 Ag4 C1 104.3(2) 2_656 2_656
O2 Ag4 C1 98.1(2) 2_756 .
O3 Ag4 C1 133.2(2) 2_656 .
C1 Ag4 C1 28.9(3) 2_656 .
O2 Ag4 Ag2 163.73(15) 2_756 2_656
O3 Ag4 Ag2 66.73(13) 2_656 2_656
C1 Ag4 Ag2 48.94(17) 2_656 2_656
C1 Ag4 Ag2 73.33(18) . 2_656
O2 Ag4 Ag3 49.50(13) 2_756 .
O3 Ag4 Ag3 173.35(12) 2_656 .
C1 Ag4 Ag3 78.22(18) 2_656 .
C1 Ag4 Ag3 49.41(18) . .
Ag2 Ag4 Ag3 118.57(3) 2_656 .
O2 Ag4 Ag2 87.91(13) 2_756 6_556
O3 Ag4 Ag2 50.26(13) 2_656 6_556
C1 Ag4 Ag2 144.95(17) 2_656 6_556
C1 Ag4 Ag2 160.39(16) . 6_556
Ag2 Ag4 Ag2 96.02(2) 2_656 6_556
Ag3 Ag4 Ag2 130.08(3) . 6_556
O1 Ag1 C1 146.1(4) . .
O1 Ag1 O4 99.0(3) . 6_556
C1 Ag1 O4 114.6(2) . 6_556
O1 Ag1 Ag2 104.4(3) . .
C1 Ag1 Ag2 49.44(18) . .
O4 Ag1 Ag2 143.95(12) 6_556 .
O1 Ag1 Ag1 78.6(2) . 2_756
C1 Ag1 Ag1 102.03(19) . 2_756
O4 Ag1 Ag1 94.24(12) 6_556 2_756
Ag2 Ag1 Ag1 64.67(2) . 2_756
O1 Ag1 Ag3 139.3(2) . .
C1 Ag1 Ag3 50.5(2) . .
O4 Ag1 Ag3 88.43(12) 6_556 .
Ag2 Ag1 Ag3 56.088(18) . .
Ag1 Ag1 Ag3 60.962(14) 2_756 .
O1 Ag1 Ag1 94.8(3) . 2_656
C1 Ag1 Ag1 59.8(2) . 2_656
O4 Ag1 Ag1 132.25(12) 6_556 2_656
Ag2 Ag1 Ag1 72.83(3) . 2_656
Ag1 Ag1 Ag1 133.36(4) 2_756 2_656
Ag3 Ag1 Ag1 109.468(16) . 2_656
O1 Ag1 Ag2 107.6(3) . 2_756
C1 Ag1 Ag2 100.1(2) . 2_756
O4 Ag1 Ag2 43.47(11) 6_556 2_756
Ag2 Ag1 Ag2 102.55(3) . 2_756
Ag1 Ag1 Ag2 56.14(2) 2_756 2_756
Ag3 Ag1 Ag2 53.684(17) . 2_756
Ag1 Ag1 Ag2 157.480(19) 2_656 2_756
O4 Ag2 C1 144.6(2) 5_756 .
O4 Ag2 O3 110.81(18) 5_756 5_656
C1 Ag2 O3 103.1(2) . 5_656
O4 Ag2 Ag3 99.03(14) 5_756 .
C1 Ag2 Ag3 55.2(2) . .
O3 Ag2 Ag3 143.19(12) 5_656 .
O4 Ag2 Ag4 156.91(14) 5_756 2_656
C1 Ag2 Ag4 54.32(18) . 2_656
O3 Ag2 Ag4 59.34(12) 5_656 2_656
Ag3 Ag2 Ag4 84.83(3) . 2_656
O4 Ag2 Ag1 100.76(13) 5_756 .
C1 Ag2 Ag1 48.85(18) . .
O3 Ag2 Ag1 126.04(12) 5_656 .
Ag3 Ag2 Ag1 65.36(2) . .
Ag4 Ag2 Ag1 101.51(2) 2_656 .
O4 Ag2 Ag4 75.61(13) 5_756 6
C1 Ag2 Ag4 138.29(18) . 6
O3 Ag2 Ag4 46.82(12) 5_656 6
Ag3 Ag2 Ag4 127.59(3) . 6
Ag4 Ag2 Ag4 83.98(2) 2_656 6
Ag1 Ag2 Ag4 166.71(3) . 6
O4 Ag2 Ag1 47.66(14) 5_756 2_756
C1 Ag2 Ag1 96.98(19) . 2_756
O3 Ag2 Ag1 154.63(12) 5_656 2_756
Ag3 Ag2 Ag1 61.95(2) . 2_756
Ag4 Ag2 Ag1 145.89(3) 2_656 2_756
Ag1 Ag2 Ag1 59.19(2) . 2_756
Ag4 Ag2 Ag1 121.51(2) 6 2_756
O2 Ag3 O2 105.4(3) 2_756 .
O2 Ag3 C1 97.2(2) 2_756 .
O2 Ag3 C1 107.5(2) . .
O2 Ag3 C1 107.5(2) 2_756 2_756
O2 Ag3 C1 97.2(2) . 2_756
C1 Ag3 C1 138.9(3) . 2_756
O2 Ag3 Ag2 145.52(12) 2_756 .
O2 Ag3 Ag2 80.63(14) . .
C1 Ag3 Ag2 49.70(17) . .
C1 Ag3 Ag2 105.30(17) 2_756 .
O2 Ag3 Ag2 80.63(13) 2_756 2_756
O2 Ag3 Ag2 145.52(12) . 2_756
C1 Ag3 Ag2 105.30(17) . 2_756
C1 Ag3 Ag2 49.70(17) 2_756 2_756
Ag2 Ag3 Ag2 113.84(4) . 2_756
O2 Ag3 Ag4 45.25(12) 2_756 .
O2 Ag3 Ag4 122.38(12) . .
C1 Ag3 Ag4 52.74(17) . .
C1 Ag3 Ag4 134.66(17) 2_756 .
Ag2 Ag3 Ag4 102.427(19) . .
Ag2 Ag3 Ag4 86.36(2) 2_756 .
O2 Ag3 Ag4 122.38(12) 2_756 2_756
O2 Ag3 Ag4 45.25(12) . 2_756
C1 Ag3 Ag4 134.66(17) . 2_756
C1 Ag3 Ag4 52.74(17) 2_756 2_756
Ag2 Ag3 Ag4 86.36(2) . 2_756
Ag2 Ag3 Ag4 102.427(19) 2_756 2_756
Ag4 Ag3 Ag4 164.02(4) . 2_756
O2 Ag3 Ag1 107.66(13) 2_756 .
O2 Ag3 Ag1 139.15(14) . .
C1 Ag3 Ag1 45.28(16) . .
C1 Ag3 Ag1 95.17(17) 2_756 .
Ag2 Ag3 Ag1 58.55(2) . .
Ag2 Ag3 Ag1 64.37(2) 2_756 .
Ag4 Ag3 Ag1 70.08(2) . .
Ag4 Ag3 Ag1 125.71(3) 2_756 .
O2 Ag3 Ag1 139.15(14) 2_756 2_756
O2 Ag3 Ag1 107.66(13) . 2_756
C1 Ag3 Ag1 95.17(17) . 2_756
C1 Ag3 Ag1 45.28(16) 2_756 2_756
Ag2 Ag3 Ag1 64.37(2) . 2_756
Ag2 Ag3 Ag1 58.55(2) 2_756 2_756
Ag4 Ag3 Ag1 125.71(3) . 2_756
Ag4 Ag3 Ag1 70.08(2) 2_756 2_756
Ag1 Ag3 Ag1 58.08(3) . 2_756
C1 C1 Ag1 104.0(4) 2_656 .
C1 C1 Ag2 136.3(8) 2_656 .
Ag1 C1 Ag2 81.7(2) . .
C1 C1 Ag4 80.7(6) 2_656 2_656
Ag1 C1 Ag4 152.3(4) . 2_656
Ag2 C1 Ag4 76.7(2) . 2_656
C1 C1 Ag3 147.9(6) 2_656 .
Ag1 C1 Ag3 84.2(2) . .
Ag2 C1 Ag3 75.1(2) . .
Ag4 C1 Ag3 106.5(3) 2_656 .
C1 C1 Ag4 70.4(5) 2_656 .
Ag1 C1 Ag4 97.2(3) . .
Ag2 C1 Ag4 152.9(4) . .
Ag4 C1 Ag4 109.9(3) 2_656 .
Ag3 C1 Ag4 77.8(2) . .
O1 C2 O1 131.1(13) 2_756 .
O1 C2 C3 114.5(6) 2_756 .
O1 C2 C3 114.5(6) . .
F1 C3 F1 130(2) . 2_756
F1 C3 F2 92.0(13) . .
F1 C3 F2 74.9(13) 2_756 .
F1 C3 F2 74.9(13) . 2_756
F1 C3 F2 92.0(13) 2_756 2_756
F2 C3 F2 149(3) . 2_756
F1 C3 C2 115.0(12) . .
F1 C3 C2 115.0(12) 2_756 .
F2 C3 C2 105.4(13) . .
F2 C3 C2 105.4(13) 2_756 .
C7 C4 C5 109.6(7) . .
C7 C4 C6 109.7(7) . .
C5 C4 C6 109.5(6) . .
C7 C4 P1 110.0(5) . .
C5 C4 P1 108.1(5) . .
C6 C4 P1 109.8(5) . .
C3 F1 F2 57.2(10) . 2_756
C3 F2 F1 47.9(10) . 2_756
C2 O1 Ag1 125.0(8) . .
P1 O2 Ag4 123.1(3) . 2_756
P1 O2 Ag3 137.5(3) . .
Ag4 O2 Ag3 85.25(17) 2_756 .
P1 O3 Ag4 128.2(3) . 2_656
P1 O3 Ag2 133.9(3) . 5_656
Ag4 O3 Ag2 82.91(15) 2_656 5_656
P1 O4 Ag2 137.6(3) . 5_756
P1 O4 Ag1 123.5(3) . 6
Ag2 O4 Ag1 88.87(17) 5_756 6
O2 P1 O3 110.7(3) . .
O2 P1 O4 111.1(3) . .
O3 P1 O4 110.5(3) . .
O2 P1 C4 107.5(3) . .
O3 P1 C4 108.7(3) . .
O4 P1 C4 108.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag4 O2 2.219(5) 2_756
Ag4 O3 2.309(5) 2_656
Ag4 C1 2.420(7) 2_656
Ag4 C1 2.535(8) .
Ag4 Ag2 2.8997(9) 2_656
Ag4 Ag3 3.1137(6) .
Ag4 Ag2 3.1425(9) 6_556
Ag1 O1 2.169(7) .
Ag1 C1 2.227(7) .
Ag1 O4 2.355(5) 6_556
Ag1 Ag2 2.9260(9) .
Ag1 Ag1 3.0265(13) 2_756
Ag1 Ag3 3.1176(10) .
Ag1 Ag1 3.1551(13) 2_656
Ag1 Ag2 3.1849(9) 2_756
Ag2 O4 2.191(5) 5_756
Ag2 C1 2.246(7) .
Ag2 O3 2.435(5) 5_656
Ag2 Ag3 2.8464(8) .
Ag2 Ag4 2.8997(9) 2_656
Ag2 Ag4 3.1425(9) 6
Ag2 Ag1 3.1849(9) 2_756
Ag3 O2 2.376(5) 2_756
Ag3 O2 2.376(5) .
Ag3 C1 2.419(8) .
Ag3 C1 2.419(8) 2_756
Ag3 Ag2 2.8464(8) 2_756
Ag3 Ag4 3.1137(6) 2_756
Ag3 Ag1 3.1176(10) 2_756
C1 C1 1.241(15) 2_656
C1 Ag4 2.420(7) 2_656
C2 O1 1.202(10) 2_756
C2 O1 1.202(10) .
C2 C3 1.57(2) .
C3 F1 1.251(15) .
C3 F1 1.251(15) 2_756
C3 F2 1.418(19) .
C3 F2 1.418(19) 2_756
C4 C7 1.522(11) .
C4 C5 1.534(10) .
C4 C6 1.553(11) .
C4 P1 1.825(7) .
F1 F2 1.63(3) 2_756
F2 F1 1.63(3) 2_756
O2 P1 1.526(5) .
O2 Ag4 2.219(5) 2_756
O3 P1 1.542(5) .
O3 Ag4 2.309(5) 2_656
O3 Ag2 2.435(5) 5_656
O4 P1 1.536(5) .
O4 Ag2 2.191(5) 5_756
O4 Ag1 2.355(5) 6
