#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:58:58 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179549 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/18/4501854.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_4501854
loop_
_publ_author_name
'Sun, Di'
'Zhang, Na'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
_publ_section_title
;
 Series of Ag(I) Coordination Complexes Derived from Aminopyrimidyl
 Ligands and Dicarboxylates: Syntheses, Crystal Structures, and Properties
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3699
_journal_paper_doi               10.1021/cg100554u
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         '2(C15 H20 Ag2 N6 O4), 3(H2 O) '
_chemical_formula_sum            'C30 H46 Ag4 N12 O11'
_chemical_formula_weight         1182.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.387(7)
_cell_angle_beta                 109.497(3)
_cell_angle_gamma                101.338(6)
_cell_formula_units_Z            1
_cell_length_a                   9.0313(11)
_cell_length_b                   10.0434(13)
_cell_length_c                   12.4591(16)
_cell_measurement_reflns_used    2297
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      54.99
_cell_measurement_theta_min      6.13
_cell_volume                     1021.2(2)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω 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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8053
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_correction_T_min  0.7576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3574
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0567P)²+1.1419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                3040
_reflns_number_total             3574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100554u_si_002.cif
_cod_data_source_block           p2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4501854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ag1 Ag 0.37087(6) -0.00401(4) 0.74017(3) 0.05734(16) Uani 1 1 d .
Ag2 Ag 0.74592(5) 0.07731(4) 0.79834(3) 0.05360(16) Uani 1 1 d .
C1 C 0.2771(5) -0.0155(5) 0.9651(3) 0.0355(9) Uani 1 1 d .
C2 C 0.1792(5) 0.1434(4) 1.0550(4) 0.0391(9) Uani 1 1 d .
C3 C 0.1824(6) 0.2217(5) 0.9733(4) 0.0502(11) Uani 1 1 d .
H3A H 0.1476 0.3029 0.9745 0.060 Uiso 1 1 calc R
C4 C 0.2387(6) 0.1762(5) 0.8896(4) 0.0483(11) Uani 1 1 d .
H4A H 0.2450 0.2299 0.8350 0.058 Uiso 1 1 calc R
C5 C 0.1234(6) 0.1856(6) 1.1504(4) 0.0529(12) Uani 1 1 d .
H5A H 0.0639 0.1047 1.1656 0.079 Uiso 1 1 calc R
H5B H 0.0543 0.2467 1.1278 0.079 Uiso 1 1 calc R
H5C H 0.2157 0.2328 1.2194 0.079 Uiso 1 1 calc R
C6 C 0.2284(6) -0.0510(5) 0.4527(4) 0.0435(10) Uani 1 1 d .
C7 C 0.0710(6) -0.2094(6) 0.5132(4) 0.0545(12) Uani 1 1 d .
C8 C 0.0253(7) -0.3012(7) 0.4081(5) 0.0656(14) Uani 1 1 d .
H8A H -0.0427 -0.3895 0.3931 0.079 Uiso 1 1 calc R
C9 C 0.0833(7) -0.2576(6) 0.3279(5) 0.0621(14) Uani 1 1 d .
H9A H 0.0512 -0.3174 0.2561 0.074 Uiso 1 1 calc R
C10 C 0.0081(8) -0.2458(8) 0.6062(5) 0.0775(18) Uani 1 1 d .
H10A H -0.0062 -0.1640 0.6464 0.116 Uiso 1 1 calc R
H10B H 0.0846 -0.2824 0.6605 0.116 Uiso 1 1 calc R
H10C H -0.0943 -0.3143 0.5710 0.116 Uiso 1 1 calc R
C11 C 0.5966(7) 0.3215(5) 0.7861(4) 0.0539(12) Uani 1 1 d .
C12 C 0.5929(7) 0.4625(5) 0.7561(5) 0.0560(12) Uani 1 1 d .
H12A H 0.6044 0.5271 0.8251 0.067 Uiso 1 1 calc R
H12B H 0.6861 0.4952 0.7354 0.067 Uiso 1 1 calc R
C13 C 0.4407(7) 0.4658(5) 0.6575(4) 0.0537(12) Uani 1 1 d .
H13A H 0.4184 0.3912 0.5921 0.064 Uiso 1 1 calc R
H13B H 0.3494 0.4495 0.6829 0.064 Uiso 1 1 calc R
C14 C 0.4546(7) 0.6016(5) 0.6176(4) 0.0552(13) Uani 1 1 d .
H14A H 0.3676 0.5874 0.5427 0.066 Uiso 1 1 calc R
H14B H 0.5562 0.6238 0.6050 0.066 Uiso 1 1 calc R
C15 C 0.4490(6) 0.7275(5) 0.6963(4) 0.0434(10) Uani 1 1 d .
N1 N 0.3182(5) -0.1351(4) 0.9591(3) 0.0439(9) Uani 1 1 d .
H1A H 0.3489 -0.1637 0.9039 0.053 Uiso 1 1 calc R
H1B H 0.3143 -0.1840 1.0104 0.053 Uiso 1 1 calc R
N2 N 0.2848(4) 0.0582(4) 0.8832(3) 0.0393(8) Uani 1 1 d .
N3 N 0.2282(4) 0.0259(4) 1.0529(3) 0.0372(8) Uani 1 1 d .
N4 N 0.3313(6) 0.0725(5) 0.4759(4) 0.0577(11) Uani 1 1 d .
H4B H 0.3616 0.1271 0.5427 0.069 Uiso 1 1 calc R
H4C H 0.3676 0.0980 0.4242 0.069 Uiso 1 1 calc R
N5 N 0.1834(5) -0.1342(4) 0.3464(3) 0.0489(9) Uani 1 1 d .
N6 N 0.1747(5) -0.0864(4) 0.5368(3) 0.0474(9) Uani 1 1 d .
O1 O 0.7125(6) 0.3152(4) 0.8743(4) 0.0795(12) Uani 1 1 d .
O1W O 0.0195(13) 0.5162(11) 0.9413(10) 0.104(3) Uani 0.50 1 d P
H1WA H -0.0621 0.4614 0.9454 0.125 Uiso 0.50 1 d PR
H1WB H 0.0853 0.5562 1.0098 0.125 Uiso 0.50 1 d PR
O2 O 0.4910(6) 0.2190(4) 0.7189(3) 0.0723(12) Uani 1 1 d .
O2W O 0.2700(13) 0.5056(10) 0.8774(8) 0.201(4) Uani 1 1 d U
H2WA H 0.1872 0.5144 0.8929 0.241 Uiso 1 1 d R
H2WB H 0.2962 0.5713 0.8451 0.241 Uiso 1 1 d R
O3 O 0.4951(4) 0.8434(3) 0.6729(3) 0.0503(8) Uani 1 1 d .
O4 O 0.3951(6) 0.7124(4) 0.7745(3) 0.0670(11) 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'
Ag Ag -0.8971 1.1015 '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'
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
N2 Ag1 O3 144.05(12) . 1_545 y
N2 Ag1 O2 99.90(14) . . y
O3 Ag1 O2 106.67(14) 1_545 . y
N2 Ag1 N6 120.08(13) . . y
O3 Ag1 N6 80.73(12) 1_545 . y
O2 Ag1 N6 96.70(14) . . y
N2 Ag1 Ag2 117.17(10) . . ?
O3 Ag1 Ag2 59.13(9) 1_545 . ?
O2 Ag1 Ag2 61.90(12) . . ?
N6 Ag1 Ag2 121.45(9) . . ?
N3 Ag2 N5 152.32(13) 2_657 2_656 y
N3 Ag2 O1 103.22(13) 2_657 . y
N5 Ag2 O1 97.06(15) 2_656 . y
N3 Ag2 Ag1 87.43(9) 2_657 . ?
N5 Ag2 Ag1 114.45(11) 2_656 . ?
O1 Ag2 Ag1 81.08(11) . . ?
N1 C1 N2 118.3(4) . . ?
N1 C1 N3 118.4(4) . . ?
N2 C1 N3 123.3(4) . . ?
N3 C2 C3 121.2(4) . . ?
N3 C2 C5 117.2(4) . . ?
C3 C2 C5 121.6(4) . . ?
C4 C3 C2 117.6(4) . . ?
C4 C3 H3A 121.2 . . ?
C2 C3 H3A 121.2 . . ?
N2 C4 C3 122.8(4) . . ?
N2 C4 H4A 118.6 . . ?
C3 C4 H4A 118.6 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 N6 117.8(4) . . ?
N4 C6 N5 118.4(4) . . ?
N6 C6 N5 123.8(5) . . ?
N6 C7 C8 121.1(5) . . ?
N6 C7 C10 117.3(5) . . ?
C8 C7 C10 121.6(6) . . ?
C9 C8 C7 117.5(6) . . ?
C9 C8 H8A 121.2 . . ?
C7 C8 H8A 121.2 . . ?
N5 C9 C8 123.4(5) . . ?
N5 C9 H9A 118.3 . . ?
C8 C9 H9A 118.3 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C11 O1 124.1(5) . . ?
O2 C11 C12 118.1(5) . . ?
O1 C11 C12 117.8(5) . . ?
C13 C12 C11 115.1(5) . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C14 C13 C12 113.0(5) . . ?
C14 C13 H13A 109.0 . . ?
C12 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 C15 118.0(4) . . ?
C13 C14 H14A 107.8 . . ?
C15 C14 H14A 107.8 . . ?
C13 C14 H14B 107.8 . . ?
C15 C14 H14B 107.8 . . ?
H14A C14 H14B 107.2 . . ?
O4 C15 O3 124.0(4) . . ?
O4 C15 C14 120.2(4) . . ?
O3 C15 C14 115.8(4) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C4 N2 C1 117.0(4) . . ?
C4 N2 Ag1 118.7(3) . . ?
C1 N2 Ag1 124.3(3) . . ?
C2 N3 C1 118.0(4) . . ?
C2 N3 Ag2 118.9(3) . 2_657 ?
C1 N3 Ag2 122.7(3) . 2_657 ?
C6 N4 H4B 120.0 . . ?
C6 N4 H4C 120.0 . . ?
H4B N4 H4C 120.0 . . ?
C9 N5 C6 116.3(4) . . ?
C9 N5 Ag2 118.1(3) . 2_656 ?
C6 N5 Ag2 125.5(3) . 2_656 ?
C7 N6 C6 117.8(4) . . ?
C7 N6 Ag1 116.1(3) . . ?
C6 N6 Ag1 116.6(3) . . ?
C11 O1 Ag2 98.4(3) . . ?
O1W O1W H1WA 50.6 2_567 . ?
O1W O1W H1WB 58.3 2_567 . ?
H1WA O1W H1WB 109.0 . . ?
C11 O2 Ag1 134.3(3) . . ?
H2WA O2W H2WB 108.6 . . ?
C15 O3 Ag1 108.3(3) . 1_565 ?
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 N2 2.236(3) . y
Ag1 O3 2.298(3) 1_545 y
Ag1 O2 2.378(4) . y
Ag1 N6 2.477(4) . y
Ag1 Ag2 3.1284(7) . y
Ag2 N3 2.206(4) 2_657 y
Ag2 N5 2.208(4) 2_656 y
Ag2 O1 2.566(4) . y
C1 N1 1.325(5) . ?
C1 N2 1.347(5) . ?
C1 N3 1.357(5) . ?
C2 N3 1.339(5) . ?
C2 C3 1.369(7) . ?
C2 C5 1.484(6) . ?
C3 C4 1.369(7) . ?
C3 H3A 0.9300 . ?
C4 N2 1.333(6) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N4 1.327(7) . ?
C6 N6 1.352(6) . ?
C6 N5 1.356(6) . ?
C7 N6 1.326(7) . ?
C7 C8 1.383(8) . ?
C7 C10 1.505(7) . ?
C8 C9 1.356(8) . ?
C8 H8A 0.9300 . ?
C9 N5 1.323(7) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 O2 1.236(7) . ?
C11 O1 1.259(7) . ?
C11 C12 1.514(7) . ?
C12 C13 1.518(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.507(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.517(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O4 1.238(6) . ?
C15 O3 1.262(6) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N3 Ag2 2.206(3) 2_657 ?
N4 H4B 0.8600 . ?
N4 H4C 0.8600 . ?
N5 Ag2 2.208(4) 2_656 ?
O1W O1W 1.67(2) 2_567 ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O3 Ag1 2.298(3) 1_565 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O4 0.86 2.11 2.949(5) 164.4 1_545
N1 H1B O1 0.86 2.11 2.969(6) 175.3 2_657
N4 H4B O2 0.86 2.09 2.919(6) 160.7 .
N4 H4C O3 0.86 2.06 2.904(5) 166.8 2_666
O1W H1WA O1 0.85 2.09 2.877(12) 153.8 1_455
O1W H1WB O1 0.85 1.98 2.772(12) 154.5 2_667
O2W H2WA O1W 0.85 1.81 2.653(14) 171.3 .
O2W H2WB O4 0.85 1.98 2.822(10) 169.2 .
