#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/09/7010935.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_7010935
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 H14 Ag Cl N4 O6'
_chemical_formula_weight         477.61
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.284(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.1132(2)
_cell_length_b                   13.2742(3)
_cell_length_c                   24.2679(7)
_cell_measurement_reflns_used    4305
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     1640.15(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4189
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.7108
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rectangular shape, cut'
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1441
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0253
_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)+(0.0263P)²+4.2225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                1376
_reflns_number_total             1441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105696b.txt
_cod_data_source_block           99145
_cod_original_cell_volume        1640.2(1)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010935
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_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 0.0000 0.34455(2) 0.2500 0.04085(15) Uani 1 2 d S . .
N1 N 0.1992(5) 0.34133(16) 0.17565(9) 0.0298(5) Uani 1 1 d . . .
C1 C 0.3893(5) 0.4075(2) 0.16751(11) 0.0326(6) Uani 1 1 d . . .
H1 H 0.4109 0.4633 0.1907 0.039 Uiso 1 1 calc R . .
C2 C 0.5535(6) 0.3963(2) 0.12626(12) 0.0351(6) Uani 1 1 d . . .
H2A H 0.6869 0.4426 0.1223 0.042 Uiso 1 1 calc R . .
C3 C 0.5178(5) 0.3150(2) 0.09055(12) 0.0340(6) Uani 1 1 d . . .
H3 H 0.6262 0.3061 0.0622 0.041 Uiso 1 1 calc R . .
C4 C 0.3181(5) 0.24756(19) 0.09785(11) 0.0264(5) Uani 1 1 d . . .
C5 C 0.1638(5) 0.26320(19) 0.14102(11) 0.0280(5) Uani 1 1 d . . .
H5 H 0.0302 0.2175 0.1461 0.034 Uiso 1 1 calc R . .
C6 C 0.2539(5) 0.1594(2) 0.06064(14) 0.0384(7) Uani 1 1 d . . .
O1 O 0.0257(4) 0.13129(17) 0.05020(11) 0.0498(6) Uani 1 1 d . . .
N2 N 0.4563(5) 0.1156(3) 0.03988(17) 0.0779(13) Uani 1 1 d D . .
H2 H 0.6191 0.1412 0.0496 0.094 Uiso 1 1 calc R . .
C7 C 0.4242(10) 0.0458(4) -0.0098(2) 0.0305(10) Uani 0.60 1 d PD . .
H7A H 0.485(7) 0.066(3) -0.0424(13) 0.049(10) Uiso 1 1 d D . .
H7B H 0.256(7) 0.017(3) -0.0156(17) 0.098(16) Uiso 1 1 d D . .
C7A C 0.4351(14) -0.0003(6) 0.0262(3) 0.0344(16) Uani 0.40 1 d PD . .
Cl1 Cl 0.0000 0.61579(7) 0.2500 0.0381(2) Uani 1 2 d SD . .
O2 O 0.1610(6) 0.5537(2) 0.28707(13) 0.0726(8) Uani 1 1 d D . .
O3 O 0.1611(5) 0.6782(2) 0.21943(12) 0.0679(8) Uani 1 1 d 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'
Cl Cl 0.1484 0.1585 '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
N1 Ag1 N1 177.72(11) . 2 ?
C5 N1 C1 118.3(2) . . ?
C5 N1 Ag1 119.70(17) . . ?
C1 N1 Ag1 121.12(18) . . ?
N1 C1 C2 122.5(2) . . ?
C1 C2 C3 119.1(3) . . ?
C4 C3 C2 118.7(2) . . ?
C3 C4 C5 118.6(2) . . ?
C3 C4 C6 123.6(2) . . ?
C5 C4 C6 117.7(2) . . ?
N1 C5 C4 122.6(2) . . ?
O1 C6 N2 123.2(3) . . ?
O1 C6 C4 120.9(2) . . ?
N2 C6 C4 115.9(2) . . ?
C6 N2 C7 122.6(3) . . ?
C6 N2 C7A 117.9(4) . . ?
C7 N2 C7A 40.2(3) . . ?
C7A C7 C7A 89.7(8) 5_655 . ?
C7A C7 C7 45.3(6) 5_655 5_655 ?
C7A C7 C7 44.4(5) . 5_655 ?
C7A C7 N2 128.9(6) 5_655 . ?
C7A C7 N2 72.8(5) . . ?
C7 C7 N2 103.3(5) 5_655 . ?
C7 C7A C7 90.3(8) 5_655 . ?
C7 C7A C7A 45.6(5) 5_655 5_655 ?
C7 C7A C7A 44.7(5) . 5_655 ?
C7 C7A N2 127.4(6) 5_655 . ?
C7 C7A N2 66.9(5) . . ?
C7A C7A N2 98.5(7) 5_655 . ?
O3 Cl1 O3 108.8(3) . 2 ?
O3 Cl1 O2 109.63(18) . 2 ?
O3 Cl1 O2 109.70(18) 2 2 ?
O3 Cl1 O2 109.70(18) . . ?
O3 Cl1 O2 109.63(18) 2 . ?
O2 Cl1 O2 109.3(3) 2 . ?
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 N1 2.153(2) . ?
Ag1 N1 2.153(2) 2 ?
N1 C5 1.337(3) . ?
N1 C1 1.338(4) . ?
C1 C2 1.373(4) . ?
C2 C3 1.385(4) . ?
C3 C4 1.382(4) . ?
C4 C5 1.384(4) . ?
C4 C6 1.496(4) . ?
C6 O1 1.229(3) . ?
C6 N2 1.327(4) . ?
N2 C7 1.516(5) . ?
N2 C7A 1.575(7) . ?
C7 C7A 1.047(8) 5_655 ?
C7 C7A 1.064(9) . ?
C7 C7 1.497(10) 5_655 ?
C7A C7 1.047(8) 5_655 ?
C7A C7A 1.489(15) 5_655 ?
Cl1 O3 1.424(3) . ?
Cl1 O3 1.424(3) 2 ?
Cl1 O2 1.424(2) 2 ?
Cl1 O2 1.424(2) . ?
