#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:36:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180046 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/40/7034025.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_7034025
loop_
_publ_author_name
'Huang, Jing'
'Deng, Zhao-Peng'
'Xiao, Ying-Hui'
'Huo, Li-Hua'
'Zhao, Shu-Nan'
'Ge, Fa-Yuan'
'Gao, Shan'
_publ_section_title
;
 Macrocyclic dinuclear, helical, layered and 3-D Ag(i) complexes
 constructed from AgX (X = NO3(-) and ClO4(-)) and flexible bis(pyridyl)
 ligands with a chelating spacer: syntheses, structures and
 photoluminescence properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5837
_journal_page_last               5847
_journal_paper_doi               10.1039/c5dt00265f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C15 H20 Ag N4, N O3'
_chemical_formula_sum            'C15 H20 Ag N5 O3'
_chemical_formula_weight         426.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-02 deposited with the CCDC.
2015-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.884(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1494(8)
_cell_length_b                   10.3138(7)
_cell_length_c                   17.0067(11)
_cell_measurement_reflns_used    1447
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.14
_cell_volume                     1770.9(2)
_computing_cell_refinement
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis Pro (Agilent, 2013)
;
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6426
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.8543
_exptl_absorpt_correction_T_min  0.7842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0482
_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)+(0.0332P)²+0.8865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                2870
_reflns_number_total             4057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00265f2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
'Adding full bibliography for 7034023--7034030.cif.'
_cod_original_cell_volume        1770.8(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7034025
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ag1 Ag 0.49724(4) 0.76298(3) 0.399318(17) 0.05938(14) Uani 1 1 d .
O1 O 0.3822(4) -0.1301(4) 0.7251(3) 0.1170(15) Uani 1 1 d .
O2 O 0.5668(4) -0.2221(3) 0.7535(3) 0.1051(14) Uani 1 1 d .
O3 O 0.4070(4) -0.2554(3) 0.8247(2) 0.0954(12) Uani 1 1 d .
N1 N 0.3677(3) 0.6443(3) 0.47463(18) 0.0562(8) Uani 1 1 d .
N2 N 0.3952(3) 0.3571(3) 0.69411(17) 0.0430(7) Uani 1 1 d D
H2N H 0.3164(18) 0.326(4) 0.690(2) 0.065 Uiso 1 1 d D
N3 N 0.5881(3) 0.0887(3) 0.69844(17) 0.0461(7) Uani 1 1 d D
H3N H 0.529(3) 0.029(3) 0.689(2) 0.069 Uiso 1 1 d D
N4 N 0.6507(3) -0.1095(3) 0.48035(19) 0.0602(9) Uani 1 1 d .
N5 N 0.4539(4) -0.2017(3) 0.7690(2) 0.0631(9) Uani 1 1 d .
C1 C 0.4075(4) 0.6099(3) 0.5488(2) 0.0510(9) Uani 1 1 d .
H1A H 0.4871 0.6438 0.5720 0.061 Uiso 1 1 calc R
C2 C 0.3383(4) 0.5275(3) 0.5934(2) 0.0442(8) Uani 1 1 d .
C3 C 0.2216(5) 0.4770(5) 0.5584(2) 0.0720(13) Uani 1 1 d .
H3A H 0.1725 0.4195 0.5857 0.086 Uiso 1 1 calc R
C4 C 0.1787(5) 0.5129(5) 0.4820(3) 0.0889(16) Uani 1 1 d .
H4A H 0.0991 0.4809 0.4576 0.107 Uiso 1 1 calc R
C5 C 0.2537(5) 0.5959(5) 0.4424(2) 0.0712(13) Uani 1 1 d .
H5A H 0.2236 0.6193 0.3908 0.085 Uiso 1 1 calc R
C6 C 0.3903(4) 0.4973(3) 0.6774(2) 0.0520(9) Uani 1 1 d .
H6A H 0.4787 0.5332 0.6881 0.062 Uiso 1 1 calc R
H6B H 0.3342 0.5390 0.7128 0.062 Uiso 1 1 calc R
C7 C 0.4456(4) 0.3355(4) 0.7775(2) 0.0540(10) Uani 1 1 d .
H7A H 0.3854 0.3758 0.8109 0.065 Uiso 1 1 calc R
H7B H 0.5309 0.3779 0.7879 0.065 Uiso 1 1 calc R
C8 C 0.4610(5) 0.1946(4) 0.7997(2) 0.0618(11) Uani 1 1 d .
H8A H 0.3869 0.1472 0.7729 0.074 Uiso 1 1 calc R
H8B H 0.4552 0.1868 0.8560 0.074 Uiso 1 1 calc R
C9 C 0.5878(5) 0.1299(4) 0.7806(2) 0.0669(12) Uani 1 1 d .
H9A H 0.6607 0.1897 0.7932 0.080 Uiso 1 1 calc R
H9B H 0.6037 0.0547 0.8145 0.080 Uiso 1 1 calc R
C10 C 0.7169(4) 0.0303(4) 0.6854(2) 0.0511(9) Uani 1 1 d .
H10A H 0.7279 -0.0500 0.7150 0.061 Uiso 1 1 calc R
H10B H 0.7874 0.0887 0.7054 0.061 Uiso 1 1 calc R
C11 C 0.6454(4) -0.0819(4) 0.5568(2) 0.0537(10) Uani 1 1 d .
H11A H 0.5805 -0.1229 0.5826 0.064 Uiso 1 1 calc R
C12 C 0.7293(4) 0.0029(3) 0.6002(2) 0.0433(8) Uani 1 1 d .
C13 C 0.8238(4) 0.0637(4) 0.5613(2) 0.0661(12) Uani 1 1 d .
H13A H 0.8828 0.1216 0.5881 0.079 Uiso 1 1 calc R
C14 C 0.8308(5) 0.0385(5) 0.4823(3) 0.0845(15) Uani 1 1 d .
H14A H 0.8937 0.0797 0.4549 0.101 Uiso 1 1 calc R
C15 C 0.7437(5) -0.0482(5) 0.4447(2) 0.0711(13) Uani 1 1 d .
H15A H 0.7497 -0.0651 0.3915 0.085 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 '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
N1 Ag1 N3 123.55(12) . 3_666
N1 Ag1 N2 115.31(11) . 3_666
N3 Ag1 N2 91.56(10) 3_666 3_666
N1 Ag1 N4 110.69(12) . 1_565
N3 Ag1 N4 102.83(11) 3_666 1_565
N2 Ag1 N4 111.09(11) 3_666 1_565
C5 N1 C1 117.3(3) . .
C5 N1 Ag1 119.8(3) . .
C1 N1 Ag1 122.5(3) . .
C6 N2 C7 109.6(3) . .
C6 N2 Ag1 113.1(2) . 3_666
C7 N2 Ag1 115.4(2) . 3_666
C6 N2 H2N 110(3) . .
C7 N2 H2N 104(3) . .
Ag1 N2 H2N 104(3) 3_666 .
C9 N3 C10 110.5(3) . .
C9 N3 Ag1 116.7(2) . 3_666
C10 N3 Ag1 115.2(2) . 3_666
C9 N3 H3N 109(3) . .
C10 N3 H3N 107(3) . .
Ag1 N3 H3N 97(3) 3_666 .
C15 N4 C11 116.2(4) . .
C15 N4 Ag1 117.0(3) . 1_545
C11 N4 Ag1 126.5(3) . 1_545
O2 N5 O1 118.8(4) . .
O2 N5 O3 122.2(4) . .
O1 N5 O3 118.8(4) . .
N1 C1 C2 124.3(4) . .
N1 C1 H1A 117.9 . .
C2 C1 H1A 117.9 . .
C3 C2 C1 117.4(3) . .
C3 C2 C6 122.5(3) . .
C1 C2 C6 120.1(3) . .
C2 C3 C4 118.9(4) . .
C2 C3 H3A 120.5 . .
C4 C3 H3A 120.5 . .
C5 C4 C3 119.6(4) . .
C5 C4 H4A 120.2 . .
C3 C4 H4A 120.2 . .
N1 C5 C4 122.5(4) . .
N1 C5 H5A 118.7 . .
C4 C5 H5A 118.7 . .
N2 C6 C2 112.8(3) . .
N2 C6 H6A 109.0 . .
C2 C6 H6A 109.0 . .
N2 C6 H6B 109.0 . .
C2 C6 H6B 109.0 . .
H6A C6 H6B 107.8 . .
N2 C7 C8 113.8(3) . .
N2 C7 H7A 108.8 . .
C8 C7 H7A 108.8 . .
N2 C7 H7B 108.8 . .
C8 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
C7 C8 C9 116.1(3) . .
C7 C8 H8A 108.3 . .
C9 C8 H8A 108.3 . .
C7 C8 H8B 108.3 . .
C9 C8 H8B 108.3 . .
H8A C8 H8B 107.4 . .
N3 C9 C8 114.7(4) . .
N3 C9 H9A 108.6 . .
C8 C9 H9A 108.6 . .
N3 C9 H9B 108.6 . .
C8 C9 H9B 108.6 . .
H9A C9 H9B 107.6 . .
N3 C10 C12 112.7(3) . .
N3 C10 H10A 109.0 . .
C12 C10 H10A 109.0 . .
N3 C10 H10B 109.0 . .
C12 C10 H10B 109.0 . .
H10A C10 H10B 107.8 . .
N4 C11 C12 124.8(4) . .
N4 C11 H11A 117.6 . .
C12 C11 H11A 117.6 . .
C13 C12 C11 117.1(3) . .
C13 C12 C10 120.9(3) . .
C11 C12 C10 122.0(3) . .
C12 C13 C14 119.5(4) . .
C12 C13 H13A 120.3 . .
C14 C13 H13A 120.3 . .
C15 C14 C13 118.9(4) . .
C15 C14 H14A 120.6 . .
C13 C14 H14A 120.6 . .
N4 C15 C14 123.5(4) . .
N4 C15 H15A 118.2 . .
C14 C15 H15A 118.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.283(3) .
Ag1 N3 2.358(3) 3_666
Ag1 N2 2.367(3) 3_666
Ag1 N4 2.369(3) 1_565
O1 N5 1.234(5) .
O2 N5 1.219(5) .
O3 N5 1.235(5) .
N1 C5 1.326(5) .
N1 C1 1.332(4) .
N2 C6 1.474(4) .
N2 C7 1.474(4) .
N2 Ag1 2.367(3) 3_666
N2 H2N 0.86(5) .
N3 C9 1.461(4) .
N3 C10 1.477(5) .
N3 Ag1 2.358(3) 3_666
N3 H3N 0.86(5) .
N4 C15 1.332(5) .
N4 C11 1.337(4) .
N4 Ag1 2.369(3) 1_545
C1 C2 1.379(5) .
C1 H1A 0.9300 .
C2 C3 1.373(5) .
C2 C6 1.504(5) .
C3 C4 1.377(6) .
C3 H3A 0.9300 .
C4 C5 1.369(6) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.505(5) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.514(6) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C12 1.494(5) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.381(5) .
C11 H11A 0.9300 .
C12 C13 1.372(5) .
C13 C14 1.378(6) .
C13 H13A 0.9300 .
C14 C15 1.369(6) .
C14 H14A 0.9300 .
C15 H15A 0.9300 .
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
N2 H2N O3 0.86(5) 2.408(12) 3.264(5) 178(4) 2_556
N2 H2N O1 0.86(5) 2.63(3) 3.260(5) 131(3) 2_556
N3 H3N O1 0.86(5) 2.35(2) 3.140(5) 154(4) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N3 Ag1 N1 C5 38.7(4) 3_666
N2 Ag1 N1 C5 -71.8(4) 3_666
N4 Ag1 N1 C5 161.0(3) 1_565
N3 Ag1 N1 C1 -148.1(3) 3_666
N2 Ag1 N1 C1 101.4(3) 3_666
N4 Ag1 N1 C1 -25.7(3) 1_565
C5 N1 C1 C2 0.3(6) .
Ag1 N1 C1 C2 -173.1(3) .
N1 C1 C2 C3 0.7(6) .
N1 C1 C2 C6 -178.6(3) .
C1 C2 C3 C4 -1.4(7) .
C6 C2 C3 C4 177.8(4) .
C2 C3 C4 C5 1.1(8) .
C1 N1 C5 C4 -0.7(7) .
Ag1 N1 C5 C4 173.0(4) .
C3 C4 C5 N1 -0.1(8) .
C7 N2 C6 C2 -179.4(3) .
Ag1 N2 C6 C2 50.4(4) 3_666
C3 C2 C6 N2 51.3(5) .
C1 C2 C6 N2 -129.5(4) .
C6 N2 C7 C8 -177.1(3) .
Ag1 N2 C7 C8 -48.1(4) 3_666
N2 C7 C8 C9 83.1(5) .
C10 N3 C9 C8 178.4(3) .
Ag1 N3 C9 C8 44.2(5) 3_666
C7 C8 C9 N3 -80.6(5) .
C9 N3 C10 C12 -172.2(3) .
Ag1 N3 C10 C12 -37.3(4) 3_666
C15 N4 C11 C12 -0.8(6) .
Ag1 N4 C11 C12 -173.4(3) 1_545
N4 C11 C12 C13 0.6(6) .
N4 C11 C12 C10 179.4(4) .
N3 C10 C12 C13 117.2(4) .
N3 C10 C12 C11 -61.5(5) .
C11 C12 C13 C14 0.2(6) .
C10 C12 C13 C14 -178.6(4) .
C12 C13 C14 C15 -0.7(7) .
C11 N4 C15 C14 0.2(7) .
Ag1 N4 C15 C14 173.5(4) 1_545
C13 C14 C15 N4 0.6(8) .
