#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010938.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_7010938
loop_
_publ_author_name
'Muthu, Sebastian'
'Yip, John H. K.'
'Vittal, Jagadese J.'
_publ_section_title
;
 Coordination polymers of d10 metals and
 N,N'-bis(3-pyridinecarboxamide)-1,2-ethane
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3577
_journal_paper_doi               10.1039/b105696b
_journal_year                    2001
_chemical_formula_sum            'C14 H16.5 Ag N5 O6.25'
_chemical_formula_weight         462.69
_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                92.612(1)
_cell_angle_beta                 98.041(1)
_cell_angle_gamma                97.386(1)
_cell_formula_units_Z            2
_cell_length_a                   9.0861(1)
_cell_length_b                   9.5617(1)
_cell_length_c                   10.1841(1)
_cell_measurement_reflns_used    6805
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     866.990(16)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_method       'ω scans'
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0216
_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       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6347
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.8288
_exptl_absorpt_correction_T_min  0.7182
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'distorted hexagnal blocks'
_exptl_crystal_F_000             465
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0048(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3000
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0262
_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)+(0.0420P)²+0.4010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                2758
_reflns_number_total             3000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105696b.txt
_cod_data_source_block           99171
_cod_original_cell_volume        866.997(16)
_cod_original_formula_sum        'C14 H16.50 Ag N5 O6.25'
_cod_database_code               7010938
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.52950(3) 0.26904(2) 0.496114(19) 0.05704(13) Uani 1 1 d . . .
O1 O 0.7076(2) -0.18595(17) 0.93514(19) 0.0473(4) Uani 1 1 d . . .
O2 O 0.2944(2) 0.68769(17) 0.03505(19) 0.0466(4) Uani 1 1 d . . .
N1 N 0.4812(2) 0.1064(2) 0.6297(2) 0.0421(5) Uani 1 1 d . . .
N2 N 0.8061(2) 0.0442(2) 0.9522(2) 0.0386(5) Uani 1 1 d . . .
H2 H 0.7933 0.1283 0.9309 0.046 Uiso 1 1 calc R . .
N3 N 0.5540(3) 0.4251(2) 0.3518(2) 0.0444(5) Uani 1 1 d . . .
N4 N 0.1963(2) 0.4611(2) 0.0488(2) 0.0370(4) Uani 1 1 d . . .
H4 H 0.2094 0.3813 0.0811 0.044 Uiso 1 1 calc R . .
C1 C 0.3435(3) 0.0331(3) 0.6271(3) 0.0502(7) Uani 1 1 d . . .
H1A H 0.2648 0.0543 0.5659 0.060 Uiso 1 1 calc R . .
C2 C 0.3156(3) -0.0717(3) 0.7117(3) 0.0537(7) Uani 1 1 d . . .
H2' H 0.2193 -0.1202 0.7072 0.064 Uiso 1 1 calc R . .
C3 C 0.4308(3) -0.1051(3) 0.8037(3) 0.0432(6) Uani 1 1 d . . .
H3 H 0.4140 -0.1767 0.8609 0.052 Uiso 1 1 calc R . .
C4 C 0.5727(3) -0.0283(2) 0.8083(2) 0.0333(5) Uani 1 1 d . . .
C5 C 0.5930(3) 0.0751(2) 0.7197(2) 0.0354(5) Uani 1 1 d . . .
H5 H 0.6882 0.1252 0.7225 0.042 Uiso 1 1 calc R . .
C6 C 0.7014(3) -0.0640(2) 0.9044(2) 0.0337(5) Uani 1 1 d . . .
C7 C 0.9416(3) 0.0230(3) 1.0399(3) 0.0419(6) Uani 1 1 d . . .
H7A H 0.9168 -0.0485 1.1008 0.050 Uiso 1 1 calc R . .
H7B H 0.9824 0.1103 1.0919 0.050 Uiso 1 1 calc R . .
C8 C 0.4332(3) 0.4461(2) 0.2663(2) 0.0370(5) Uani 1 1 d . . .
H8 H 0.3419 0.3911 0.2701 0.044 Uiso 1 1 calc R . .
C9 C 0.4396(3) 0.5468(2) 0.1725(2) 0.0331(5) Uani 1 1 d . . .
C10 C 0.5756(3) 0.6308(3) 0.1689(3) 0.0418(5) Uani 1 1 d . . .
H10 H 0.5831 0.7009 0.1089 0.050 Uiso 1 1 calc R . .
C11 C 0.6994(3) 0.6078(3) 0.2565(3) 0.0521(7) Uani 1 1 d . . .
H11A H 0.7917 0.6622 0.2553 0.062 Uiso 1 1 calc R . .
C12 C 0.6861(3) 0.5051(3) 0.3448(3) 0.0521(7) Uani 1 1 d . . .
H12 H 0.7709 0.4897 0.4019 0.063 Uiso 1 1 calc R . .
C13 C 0.3032(3) 0.5710(2) 0.0799(2) 0.0333(5) Uani 1 1 d . . .
C14 C 0.0573(3) 0.4725(3) -0.0386(3) 0.0411(5) Uani 1 1 d . . .
H14A H 0.0162 0.3804 -0.0815 0.042(7) Uiso 1 1 calc R . .
H14B H 0.0785 0.5360 -0.1073 0.054(8) Uiso 1 1 calc R . .
O3 O 0.8234(3) 0.3468(4) 0.6315(3) 0.0850(8) Uani 1 1 d D . .
H3A H 0.870(4) 0.426(3) 0.622(4) 0.080 Uiso 1 1 d D . .
H3B H 0.892(4) 0.295(4) 0.624(4) 0.080 Uiso 1 1 d D . .
N5 N 0.9124(3) 0.7450(3) 0.6044(4) 0.0814(10) Uani 1 1 d D . .
O4 O 0.9729(4) 0.7997(5) 0.5055(4) 0.0824(11) Uani 0.65 1 d PD . .
O5 O 0.8089(5) 0.8009(6) 0.6366(5) 0.0908(13) Uani 0.65 1 d PD . .
O6 O 0.9601(7) 0.6393(6) 0.6406(8) 0.131(3) Uani 0.65 1 d PD . .
O4A O 0.954(2) 0.6881(17) 0.6984(16) 0.166(4) Uiso 0.35 1 d PD . .
O5A O 0.7877(15) 0.7184(17) 0.5726(16) 0.166(4) Uiso 0.35 1 d PD . .
O6A O 0.9427(17) 0.8679(14) 0.6244(16) 0.166(4) Uiso 0.35 1 d PD . .
O7 O 1.0302(12) 0.8872(12) 0.3565(11) 0.080(3) Uiso 0.25 1 d P . .
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
N3 Ag1 N1 173.95(8) . . ?
C5 N1 C1 117.9(2) . . ?
C5 N1 Ag1 118.93(17) . . ?
C1 N1 Ag1 123.16(17) . . ?
C6 N2 C7 121.5(2) . . ?
C8 N3 C12 118.2(2) . . ?
C8 N3 Ag1 119.21(18) . . ?
C12 N3 Ag1 122.56(17) . . ?
C13 N4 C14 121.7(2) . . ?
N1 C1 C2 122.3(2) . . ?
C1 C2 C3 120.0(3) . . ?
C2 C3 C4 118.1(2) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 C6 121.4(2) . . ?
C3 C4 C6 119.6(2) . . ?
N1 C5 C4 122.9(2) . . ?
O1 C6 N2 123.3(2) . . ?
O1 C6 C4 120.9(2) . . ?
N2 C6 C4 115.82(19) . . ?
N2 C7 C7 110.8(3) . 2_757 ?
N3 C8 C9 122.5(2) . . ?
C8 C9 C10 118.6(2) . . ?
C8 C9 C13 121.8(2) . . ?
C10 C9 C13 119.6(2) . . ?
C11 C10 C9 118.5(2) . . ?
C12 C11 C10 119.9(3) . . ?
N3 C12 C11 122.2(2) . . ?
O2 C13 N4 123.0(2) . . ?
O2 C13 C9 120.3(2) . . ?
N4 C13 C9 116.76(19) . . ?
N4 C14 C14 111.1(3) . 2_565 ?
O5A N5 O4A 112.1(11) . . ?
O5A N5 O6A 109.0(10) . . ?
O4A N5 O6A 110.2(10) . . ?
O5A N5 O6 108.1(9) . . ?
O4A N5 O6 36.8(10) . . ?
O6A N5 O6 138.7(8) . . ?
O5A N5 O5 49.4(8) . . ?
O4A N5 O5 103.4(11) . . ?
O6A N5 O5 67.3(8) . . ?
O6 N5 O5 130.3(5) . . ?
O5A N5 O4 108.7(9) . . ?
O4A N5 O4 136.1(11) . . ?
O6A N5 O4 69.8(9) . . ?
O6 N5 O4 114.0(5) . . ?
O5 N5 O4 115.3(4) . . ?
N5 O4 O6A 50.6(6) . . ?
O5A O5 N5 60.6(9) . . ?
O5A O5 O6A 107.8(12) . . ?
N5 O5 O6A 54.9(6) . . ?
O4A O6 N5 68.7(12) . . ?
O6 O4A N5 74.5(14) . . ?
O5 O5A N5 70.0(9) . . ?
N5 O6A O5 57.9(7) . . ?
N5 O6A O4 59.7(7) . . ?
O5 O6A O4 101.9(9) . . ?
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 N3 2.155(2) . ?
Ag1 N1 2.155(2) . ?
O1 C6 1.227(3) . ?
O2 C13 1.233(3) . ?
N1 C5 1.343(3) . ?
N1 C1 1.350(4) . ?
N2 C6 1.335(3) . ?
N2 C7 1.458(3) . ?
N3 C8 1.345(3) . ?
N3 C12 1.350(4) . ?
N4 C13 1.330(3) . ?
N4 C14 1.459(3) . ?
C1 C2 1.373(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.393(4) . ?
C4 C5 1.381(3) . ?
C4 C6 1.502(3) . ?
C7 C7 1.520(5) 2_757 ?
C8 C9 1.389(3) . ?
C9 C10 1.390(4) . ?
C9 C13 1.498(3) . ?
C10 C11 1.382(4) . ?
C11 C12 1.367(4) . ?
C14 C14 1.521(5) 2_565 ?
N5 O5A 1.127(13) . ?
N5 O4A 1.163(14) . ?
N5 O6A 1.174(13) . ?
N5 O6 1.202(5) . ?
N5 O5 1.215(5) . ?
N5 O4 1.311(5) . ?
O4 O6A 1.426(16) . ?
O5 O5A 0.981(15) . ?
O5 O6A 1.324(16) . ?
O6 O4A 0.75(2) . ?
