#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/94/2019447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019447
loop_
_publ_author_name
'Liang, Guang-Ming'
'Shang, Jing'
'Yang, Kun-Guo'
'Ma, Kai'
'Ni, Qing-Ling'
_publ_section_title
;
 Counter-anion role in the formation of two supramolecular complexes:
 [Ag₂(DPP)₂](ClO₄)₂·CH₃CN and [Ag₂(DPP)₂(NO₃)₂]
 {DPP is N-[(diphenylphosphanyl)methyl]pyridin-4-amine}
;
_journal_coeditor_code           FG3317
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              379
_journal_page_last               383
_journal_paper_doi               10.1107/S2053229614005725
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ag2 (C18 H17 N2 P)2] (Cl O4)2 , C2 H3 N'
_chemical_formula_moiety         'C36 H34 Ag2 N4 P2 2+, 2(Cl O4 -), C2 H3 N'
_chemical_formula_sum            'C38 H37 Ag2 Cl2 N5 O8 P2'
_chemical_formula_weight         1040.31
_chemical_name_systematic
'Bis{μ-N-[(diphenylphosphanyl)methyl]pyridin-4-amine-κ²N¹:P}disilver bis(perchlorate) acetonitrile monosolvate'
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.988(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.928(2)
_cell_length_b                   18.192(3)
_cell_length_c                   19.026(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.45
_cell_volume                     4126.0(12)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10757
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.6053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.979
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0447
_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)+(0.0727P)²+4.9016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                2995
_reflns_number_total             4447
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg3317sup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2019447
_cod_database_fobs_code          2019447
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ag Ag1 0.65542(3) 0.38326(2) 1.00024(2) 0.07792(19) Uani d . 1 1
P P1 0.81927(8) 0.36619(5) 0.93652(5) 0.0436(2) Uani d . 1 1
N N1 0.4939(3) 0.58932(18) 0.94507(18) 0.0519(8) Uani d . 1 1
N N2 0.7689(2) 0.48847(17) 0.85624(16) 0.0474(7) Uani d . 1 1
H H2B 0.7698 0.4865 0.8111 0.057 Uiso d R 1 1
C C1 0.4963(3) 0.5728(2) 0.8764(2) 0.0566(10) Uani d . 1 1
H H1A 0.4333 0.5839 0.8483 0.068 Uiso calc R 1 1
C C2 0.5848(3) 0.5409(2) 0.8454(2) 0.0505(9) Uani d . 1 1
H H2A 0.5814 0.5309 0.7975 0.061 Uiso calc R 1 1
C C3 0.6811(3) 0.52304(19) 0.88594(18) 0.0417(8) Uani d . 1 1
C C4 0.6814(3) 0.5428(2) 0.95672(19) 0.0471(8) Uani d . 1 1
H H4A 0.7444 0.5342 0.9857 0.057 Uiso calc R 1 1
C C5 0.5877(3) 0.5750(2) 0.9832(2) 0.0538(10) Uani d . 1 1
H H5A 0.5895 0.5876 1.0306 0.065 Uiso calc R 1 1
C C6 0.8610(3) 0.4551(2) 0.8964(2) 0.0483(9) Uani d . 1 1
H H6A 0.8864 0.4886 0.9333 0.058 Uiso calc R 1 1
H H6B 0.9231 0.4467 0.8658 0.058 Uiso calc R 1 1
C C7 0.8056(3) 0.3006(2) 0.86509(19) 0.0457(8) Uani d . 1 1
C C8 0.7345(4) 0.2411(2) 0.8741(2) 0.0604(10) Uani d . 1 1
H H8A 0.6939 0.2375 0.9148 0.072 Uiso calc R 1 1
C C9 0.7234(4) 0.1870(3) 0.8229(3) 0.0715(13) Uani d . 1 1
H H9A 0.6776 0.1466 0.8301 0.086 Uiso calc R 1 1
C C10 0.7799(4) 0.1933(3) 0.7619(3) 0.0737(13) Uani d . 1 1
H H10A 0.7719 0.1576 0.7272 0.088 Uiso calc R 1 1
C C11 0.8486(5) 0.2527(3) 0.7522(3) 0.0792(14) Uani d . 1 1
H H11A 0.8866 0.2571 0.7105 0.095 Uiso calc R 1 1
C C12 0.8622(4) 0.3064(3) 0.8038(2) 0.0661(12) Uani d . 1 1
H H12A 0.9096 0.3461 0.7967 0.079 Uiso calc R 1 1
C C13 0.9436(3) 0.3394(2) 0.9874(2) 0.0453(8) Uani d . 1 1
C C14 1.0117(3) 0.2812(2) 0.9685(2) 0.0570(10) Uani d . 1 1
H H14A 0.9967 0.2556 0.9269 0.068 Uiso calc R 1 1
C C15 1.1023(4) 0.2616(3) 1.0123(3) 0.0736(13) Uani d . 1 1
H H15A 1.1488 0.2232 0.9993 0.088 Uiso calc R 1 1
C C16 1.1240(4) 0.2972(3) 1.0735(3) 0.0756(14) Uani d . 1 1
H H16A 1.1840 0.2823 1.1026 0.091 Uiso calc R 1 1
C C17 1.0581(4) 0.3558(3) 1.0933(3) 0.0695(12) Uani d . 1 1
H H17A 1.0739 0.3805 1.1352 0.083 Uiso calc R 1 1
C C18 0.9684(4) 0.3770(2) 1.0499(2) 0.0586(10) Uani d . 1 1
H H18A 0.9243 0.4167 1.0625 0.070 Uiso calc R 1 1
N N3 0.5292(8) 0.3627(6) 0.8715(5) 0.083(2) Uani d P 0.50 1
C C19 0.5133(7) 0.3485(6) 0.8148(7) 0.068(2) Uani d P 0.50 1
C C20 0.5000 0.3286(7) 0.7500 0.126(4) Uani d S 1 2
H H20A 0.4356 0.3522 0.7285 0.189 Uiso d PR 0.50 1
H H20B 0.5656 0.3415 0.7249 0.189 Uiso d PR 0.50 1
H H20C 0.4898 0.2763 0.7486 0.189 Uiso d PR 0.50 1
Cl Cl1 0.79174(11) 0.45084(8) 0.65833(6) 0.0758(4) Uani d . 1 1
O O1 0.7781(10) 0.3831(4) 0.6219(3) 0.223(5) Uani d . 1 1
O O2 0.7745(4) 0.5080(3) 0.6096(2) 0.1155(16) Uani d . 1 1
O O3 0.7095(4) 0.4532(3) 0.7074(2) 0.1212(17) Uani d . 1 1
O O4 0.8910(4) 0.4521(6) 0.6947(3) 0.233(5) Uani d . 1 1
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ag1 P1 5_667 . 174.00(9) yes
C13 P1 C7 . . 105.95(17) ?
C13 P1 C6 . . 103.12(17) ?
C7 P1 C6 . . 106.42(18) ?
C13 P1 Ag1 . . 116.05(12) ?
C7 P1 Ag1 . . 114.73(12) ?
C6 P1 Ag1 . . 109.56(12) ?
C5 N1 C1 . . 116.0(3) ?
C5 N1 Ag1 . 5_667 118.3(3) ?
C1 N1 Ag1 . 5_667 124.7(3) ?
C3 N2 C6 . . 123.7(3) ?
C3 N2 H2B . . 118.1 ?
C6 N2 H2B . . 118.3 ?
N1 C1 C2 . . 124.2(4) ?
N1 C1 H1A . . 117.9 ?
C2 C1 H1A . . 117.9 ?
C1 C2 C3 . . 119.7(4) ?
C1 C2 H2A . . 120.1 ?
C3 C2 H2A . . 120.1 ?
N2 C3 C4 . . 123.0(3) ?
N2 C3 C2 . . 120.5(3) ?
C4 C3 C2 . . 116.6(3) ?
C5 C4 C3 . . 119.3(3) ?
C5 C4 H4A . . 120.3 ?
C3 C4 H4A . . 120.3 ?
N1 C5 C4 . . 124.1(4) ?
N1 C5 H5A . . 118.0 ?
C4 C5 H5A . . 118.0 ?
N2 C6 P1 . . 111.8(3) ?
N2 C6 H6A . . 109.3 ?
P1 C6 H6A . . 109.3 ?
N2 C6 H6B . . 109.3 ?
P1 C6 H6B . . 109.3 ?
H6A C6 H6B . . 107.9 ?
C12 C7 C8 . . 119.0(4) ?
C12 C7 P1 . . 123.6(3) ?
C8 C7 P1 . . 117.4(3) ?
C9 C8 C7 . . 120.7(4) ?
C9 C8 H8A . . 119.7 ?
C7 C8 H8A . . 119.7 ?
C10 C9 C8 . . 119.9(5) ?
C10 C9 H9A . . 120.0 ?
C8 C9 H9A . . 120.0 ?
C9 C10 C11 . . 119.6(5) ?
C9 C10 H10A . . 120.2 ?
C11 C10 H10A . . 120.2 ?
C10 C11 C12 . . 120.9(5) ?
C10 C11 H11A . . 119.5 ?
C12 C11 H11A . . 119.5 ?
C7 C12 C11 . . 119.9(4) ?
C7 C12 H12A . . 120.1 ?
C11 C12 H12A . . 120.1 ?
C14 C13 C18 . . 119.0(4) ?
C14 C13 P1 . . 122.9(3) ?
C18 C13 P1 . . 118.1(3) ?
C15 C14 C13 . . 119.4(4) ?
C15 C14 H14A . . 120.3 ?
C13 C14 H14A . . 120.3 ?
C16 C15 C14 . . 121.1(4) ?
C16 C15 H15A . . 119.5 ?
C14 C15 H15A . . 119.5 ?
C15 C16 C17 . . 120.7(4) ?
C15 C16 H16A . . 119.6 ?
C17 C16 H16A . . 119.6 ?
C18 C17 C16 . . 119.2(5) ?
C18 C17 H17A . . 120.4 ?
C16 C17 H17A . . 120.4 ?
C17 C18 C13 . . 120.6(4) ?
C17 C18 H18A . . 119.7 ?
C13 C18 H18A . . 119.7 ?
N3 C19 C20 . . 176.1(11) ?
C19 C20 C19 2_656 . 147.4(15) ?
C19 C20 H20A 2_656 . 52.8 ?
C19 C20 H20A . . 110.6 ?
C19 C20 H20B 2_656 . 62.1 ?
C19 C20 H20B . . 109.3 ?
H20A C20 H20B . . 109.5 ?
C19 C20 H20C 2_656 . 103.9 ?
C19 C20 H20C . . 108.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
O4 Cl1 O3 . . 106.5(3) ?
O4 Cl1 O2 . . 115.6(4) ?
O3 Cl1 O2 . . 109.4(3) ?
O4 Cl1 O1 . . 110.3(6) ?
O3 Cl1 O1 . . 106.6(5) ?
O2 Cl1 O1 . . 108.0(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 N1 5_667 2.152(3) yes
Ag1 P1 . 2.3560(10) yes
Ag1 N3 . 2.855(10) yes
Ag1 O2 6_566 3.171(5) yes
P1 C13 . 1.809(4) ?
P1 C7 . 1.811(4) ?
P1 C6 . 1.863(4) ?
N1 C5 . 1.338(5) ?
N1 C1 . 1.342(5) ?
N1 Ag1 5_667 2.152(3) ?
N2 C3 . 1.361(4) ?
N2 C6 . 1.450(5) ?
N2 H2B . 0.8600 ?
C1 C2 . 1.357(6) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.399(5) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.393(5) ?
C4 C5 . 1.373(5) ?
C4 H4A . 0.9300 ?
C5 H5A . 0.9300 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C12 . 1.372(6) ?
C7 C8 . 1.389(6) ?
C8 C9 . 1.387(6) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.367(7) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.373(7) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.389(7) ?
C11 H11A . 0.9300 ?
C12 H12A . 0.9300 ?
C13 C14 . 1.390(5) ?
C13 C18 . 1.395(6) ?
C14 C15 . 1.388(6) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.349(7) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.384(7) ?
C16 H16A . 0.9300 ?
C17 C18 . 1.383(6) ?
C17 H17A . 0.9300 ?
C18 H18A . 0.9300 ?
N3 C19 . 1.120(13) ?
C19 C20 . 1.289(13) ?
C20 C19 2_656 1.289(13) ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9600 ?
C20 H20C . 0.9599 ?
Cl1 O4 . 1.351(5) ?
Cl1 O3 . 1.377(4) ?
Cl1 O2 . 1.404(4) ?
Cl1 O1 . 1.421(7) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2B O3 . 0.86 2.16 2.966(5) 155.2
C4 H4A O2 6_566 0.93 2.49 3.213(5) 134.4
