#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001495.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_7001495
loop_
_publ_author_name
'Zhu, Bi-Xue'
'Zhang, Qi-Long'
'Zhang, Yun-Qian'
'Tao, Zhu'
'Clegg, Jack K.'
'Reimers, Jeffrey R.'
'Lindoy, Leonard F.'
'Wei, Gang'
_publ_section_title
;
 Polymeric di- and discrete trinuclear silver(I) assemblies
 incorporating γ-carbon bonded, neutral acetylacetone-imine motifs
 assembled from racemic and diastereopure
 N,N′-bis(acetylacetone)cyclohexanediimine units
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              4896
_journal_page_last               4900
_journal_paper_doi               10.1039/b903467f
_journal_year                    2009
_chemical_formula_moiety         'C16 H26 Ag N3 O5'
_chemical_formula_sum            'C16 H26 Ag N3 O5'
_chemical_formula_weight         448.27
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.501(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2127(5)
_cell_length_b                   14.0792(7)
_cell_length_c                   14.6593(8)
_cell_measurement_reflns_used    3648
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.02
_cell_volume                     1869.57(17)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart Apex 2 CCD Area Detector'
_diffrn_measurement_method       'φ and 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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20564
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.8426
_exptl_absorpt_correction_T_min  0.7691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+2.2212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                3325
_reflns_number_total             3648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903467f.txt
_cod_data_source_block           p
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001495
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2557(3) -0.0649(2) 0.0706(2) 0.0480(7) Uani 1 1 d . . .
H1A H 0.1940 -0.0486 0.0126 0.072 Uiso 1 1 calc R . .
H1B H 0.2702 -0.0098 0.1098 0.072 Uiso 1 1 calc R . .
H1C H 0.2093 -0.1140 0.1004 0.072 Uiso 1 1 calc R . .
C2 C 0.4029(3) -0.09961(17) 0.05304(18) 0.0290(5) Uani 1 1 d . . .
C3 C 0.5106(3) -0.12758(17) 0.13109(16) 0.0288(5) Uani 1 1 d . . .
H3 H 0.4923 -0.1140 0.1900 0.035 Uiso 1 1 calc R . .
C4 C 0.6431(3) -0.17455(16) 0.12397(16) 0.0254(5) Uani 1 1 d . . .
C5 C 0.7374(3) -0.2128(2) 0.21044(18) 0.0373(6) Uani 1 1 d . . .
H5A H 0.8231 -0.2430 0.1949 0.056 Uiso 1 1 calc R . .
H5B H 0.6819 -0.2582 0.2388 0.056 Uiso 1 1 calc R . .
H5C H 0.7675 -0.1616 0.2529 0.056 Uiso 1 1 calc R . .
C6 C 0.8049(2) -0.24627(17) 0.02247(16) 0.0261(5) Uani 1 1 d . . .
H6 H 0.8712 -0.2607 0.0811 0.031 Uiso 1 1 calc R . .
C7 C 0.8930(3) -0.19451(19) -0.0411(2) 0.0364(6) Uani 1 1 d . . .
H7A H 0.9349 -0.1368 -0.0111 0.044 Uiso 1 1 calc R . .
H7B H 0.8279 -0.1770 -0.0983 0.044 Uiso 1 1 calc R . .
C8 C 1.0170(3) -0.2584(2) -0.0628(2) 0.0446(7) Uani 1 1 d . . .
H8A H 1.0702 -0.2256 -0.1047 0.053 Uiso 1 1 calc R . .
H8B H 1.0859 -0.2720 -0.0060 0.053 Uiso 1 1 calc R . .
C9 C 0.9548(3) -0.3510(2) -0.1071(2) 0.0425(7) Uani 1 1 d . . .
H9A H 1.0351 -0.3912 -0.1185 0.051 Uiso 1 1 calc R . .
H9B H 0.8917 -0.3377 -0.1662 0.051 Uiso 1 1 calc R . .
C10 C 0.8661(3) -0.40318(19) -0.04426(19) 0.0338(6) Uani 1 1 d . . .
H10A H 0.9311 -0.4211 0.0129 0.041 Uiso 1 1 calc R . .
H10B H 0.8247 -0.4608 -0.0748 0.041 Uiso 1 1 calc R . .
C11 C 0.7415(2) -0.34057(17) -0.02180(16) 0.0261(5) Uani 1 1 d . . .
H11 H 0.6714 -0.3270 -0.0791 0.031 Uiso 1 1 calc R . .
C12 C 0.4136(3) -0.3496(2) -0.0340(2) 0.0382(6) Uani 1 1 d . . .
H12A H 0.4659 -0.3295 -0.0816 0.057 Uiso 1 1 calc R . .
H12B H 0.3616 -0.2966 -0.0142 0.057 Uiso 1 1 calc R . .
H12C H 0.3444 -0.3985 -0.0579 0.057 Uiso 1 1 calc R . .
C13 C 0.5213(3) -0.38758(17) 0.04703(18) 0.0286(5) Uani 1 1 d . . .
C14 C 0.4705(3) -0.42106(19) 0.1248(2) 0.0350(6) Uani 1 1 d . . .
H14 H 0.3694 -0.4190 0.1242 0.042 Uiso 1 1 calc R . .
C15 C 0.5617(3) -0.45762(19) 0.2039(2) 0.0373(6) Uani 1 1 d . . .
C16 C 0.4925(5) -0.4889(3) 0.2845(3) 0.0636(10) Uani 1 1 d . . .
H16A H 0.5679 -0.5122 0.3334 0.095 Uiso 1 1 calc R . .
H16B H 0.4223 -0.5385 0.2647 0.095 Uiso 1 1 calc R . .
H16C H 0.4433 -0.4360 0.3068 0.095 Uiso 1 1 calc R . .
N1 N 0.6850(2) -0.18629(14) 0.04229(13) 0.0256(4) Uani 1 1 d . . .
H1 H 0.6361 -0.1552 -0.0037 0.031 Uiso 1 1 calc R . .
N2 N 0.6649(2) -0.38976(14) 0.04325(14) 0.0265(4) Uani 1 1 d . . .
H2 H 0.7191 -0.4245 0.0842 0.032 Uiso 1 1 calc R . .
N3 N 0.4153(3) 0.16734(19) 0.26161(16) 0.0428(6) Uani 1 1 d . . .
O1 O 0.4258(2) -0.10405(13) -0.02839(12) 0.0344(4) Uani 1 1 d . . .
O2 O 0.6999(2) -0.46737(14) 0.20948(14) 0.0408(5) Uani 1 1 d . . .
O3 O 0.4459(5) 0.0959(3) 0.3084(2) 0.0996(11) Uani 1 1 d . . .
O4 O 0.4505(3) 0.17004(18) 0.18385(15) 0.0568(6) Uani 1 1 d . . .
O5 O 0.3585(4) 0.2369(3) 0.2913(2) 0.0963(11) Uani 1 1 d . . .
Ag1 Ag 0.59912(3) 0.027351(16) 0.175344(14) 0.04429(10) 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'
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
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 122.5(2) . . ?
O1 C2 C1 119.5(2) . . ?
C3 C2 C1 118.0(2) . . ?
C4 C3 C2 123.8(2) . . ?
C4 C3 Ag1 101.07(16) . . ?
C2 C3 Ag1 96.87(15) . . ?
C4 C3 H3 118.1 . . ?
C2 C3 H3 118.1 . . ?
Ag1 C3 H3 70.7 . . ?
N1 C4 C3 121.4(2) . . ?
N1 C4 C5 119.8(2) . . ?
C3 C4 C5 118.8(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 110.5(2) . . ?
N1 C6 C11 109.76(18) . . ?
C7 C6 C11 110.9(2) . . ?
N1 C6 H6 108.5 . . ?
C7 C6 H6 108.5 . . ?
C11 C6 H6 108.5 . . ?
C6 C7 C8 110.2(2) . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C7 110.8(2) . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 C10 110.9(2) . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 C11 111.0(2) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 C10 109.8(2) . . ?
N2 C11 C6 108.91(18) . . ?
C10 C11 C6 110.11(19) . . ?
N2 C11 H11 109.3 . . ?
C10 C11 H11 109.3 . . ?
C6 C11 H11 109.3 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 120.7(2) . . ?
N2 C13 C12 119.5(2) . . ?
C14 C13 C12 119.8(2) . . ?
C13 C14 C15 124.2(2) . . ?
C13 C14 H14 117.9 . . ?
C15 C14 H14 117.9 . . ?
O2 C15 C14 122.5(2) . . ?
O2 C15 C16 118.7(3) . . ?
C14 C15 C16 118.7(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 N1 C6 127.1(2) . . ?
C4 N1 H1 116.4 . . ?
C6 N1 H1 116.4 . . ?
C13 N2 C11 128.1(2) . . ?
C13 N2 H2 116.0 . . ?
C11 N2 H2 116.0 . . ?
O3 N3 O5 121.9(3) . . ?
O3 N3 O4 118.0(3) . . ?
O5 N3 O4 120.1(3) . . ?
C2 O1 Ag1 146.57(16) . 3_655 ?
C15 O2 Ag1 136.51(18) . 2_645 ?
N3 O4 Ag1 105.29(18) . . ?
O2 Ag1 C3 115.22(8) 2_655 . ?
O2 Ag1 O1 126.10(7) 2_655 3_655 ?
C3 Ag1 O1 101.38(7) . 3_655 ?
O2 Ag1 O4 108.88(8) 2_655 . ?
C3 Ag1 O4 126.85(9) . . ?
O1 Ag1 O4 73.23(7) 3_655 . ?
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
C1 C2 1.506(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.251(3) . ?
C2 C3 1.426(4) . ?
C3 C4 1.409(3) . ?
C3 Ag1 2.377(2) . ?
C3 H3 0.9300 . ?
C4 N1 1.334(3) . ?
C4 C5 1.500(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N1 1.461(3) . ?
C6 C7 1.527(3) . ?
C6 C11 1.545(3) . ?
C6 H6 0.9800 . ?
C7 C8 1.533(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.521(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.526(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.530(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.460(3) . ?
C11 H11 0.9800 . ?
C12 C13 1.500(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N2 1.335(3) . ?
C13 C14 1.391(4) . ?
C14 C15 1.400(4) . ?
C14 H14 0.9300 . ?
C15 O2 1.268(4) . ?
C15 C16 1.507(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
N3 O3 1.221(4) . ?
N3 O5 1.227(4) . ?
N3 O4 1.241(3) . ?
O1 Ag1 2.3831(18) 3_655 ?
O2 Ag1 2.268(2) 2_645 ?
O4 Ag1 2.447(2) . ?
Ag1 O2 2.268(2) 2_655 ?
Ag1 O1 2.3831(18) 3_655 ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 -9.1(4) . . . . ?
C1 C2 C3 C4 170.0(2) . . . . ?
O1 C2 C3 Ag1 99.1(2) . . . . ?
C1 C2 C3 Ag1 -81.7(2) . . . . ?
C2 C3 C4 N1 8.0(4) . . . . ?
Ag1 C3 C4 N1 -98.1(2) . . . . ?
C2 C3 C4 C5 -171.3(2) . . . . ?
Ag1 C3 C4 C5 82.6(2) . . . . ?
N1 C6 C7 C8 -179.1(2) . . . . ?
C11 C6 C7 C8 -57.1(3) . . . . ?
C6 C7 C8 C9 57.4(3) . . . . ?
C7 C8 C9 C10 -57.4(3) . . . . ?
C8 C9 C10 C11 57.1(3) . . . . ?
C9 C10 C11 N2 -176.2(2) . . . . ?
C9 C10 C11 C6 -56.3(3) . . . . ?
N1 C6 C11 N2 -60.5(2) . . . . ?
C7 C6 C11 N2 177.10(19) . . . . ?
N1 C6 C11 C10 179.08(19) . . . . ?
C7 C6 C11 C10 56.7(3) . . . . ?
N2 C13 C14 C15 0.8(4) . . . . ?
C12 C13 C14 C15 -179.9(2) . . . . ?
C13 C14 C15 O2 -3.3(4) . . . . ?
C13 C14 C15 C16 178.3(3) . . . . ?
C3 C4 N1 C6 -169.1(2) . . . . ?
C5 C4 N1 C6 10.3(4) . . . . ?
C7 C6 N1 C4 -137.4(2) . . . . ?
C11 C6 N1 C4 100.0(3) . . . . ?
C14 C13 N2 C11 -165.7(2) . . . . ?
C12 C13 N2 C11 15.0(4) . . . . ?
C10 C11 N2 C13 -144.4(2) . . . . ?
C6 C11 N2 C13 95.0(3) . . . . ?
C3 C2 O1 Ag1 -137.0(2) . . . 3_655 ?
C1 C2 O1 Ag1 43.8(4) . . . 3_655 ?
C14 C15 O2 Ag1 154.5(2) . . . 2_645 ?
C16 C15 O2 Ag1 -27.1(4) . . . 2_645 ?
O3 N3 O4 Ag1 -7.2(4) . . . . ?
O5 N3 O4 Ag1 169.2(3) . . . . ?
C4 C3 Ag1 O2 -46.41(17) . . . 2_655 ?
C2 C3 Ag1 O2 -172.84(13) . . . 2_655 ?
C4 C3 Ag1 O1 92.98(15) . . . 3_655 ?
C2 C3 Ag1 O1 -33.45(15) . . . 3_655 ?
C4 C3 Ag1 O4 170.44(13) . . . . ?
C2 C3 Ag1 O4 44.02(17) . . . . ?
N3 O4 Ag1 O2 -60.2(2) . . . 2_655 ?
N3 O4 Ag1 C3 84.8(2) . . . . ?
N3 O4 Ag1 O1 176.6(2) . . . 3_655 ?
