#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/04/7050467.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_7050467
loop_
_publ_author_name
'Carlucci, Lucia'
'Ciani, Gianfranco'
'Proserpio, Davide M.'
'Rizzato, Silvia'
_publ_section_title
;
 Silver(i) polymeric coordination frameworks assembled with the new
 multimodal ligand 2,2'-azobispyrazine
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              483
_journal_paper_doi               10.1039/b209580g
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C16 H12 Ag Cl N12 O4'
_chemical_formula_weight         579.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8840(10)
_cell_length_b                   9.5010(10)
_cell_length_c                   19.445(2)
_cell_measurement_reflns_used    5343
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.
_cell_measurement_theta_min      3.
_cell_volume                     2119.6(4)
_computing_molecular_graphics    SCHAKAL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            CCD_plate
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       SMART
_diffrn_measurement_method       omega-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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11555
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3045
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_obs          0.0226
_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)+(0.0270P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0531
_refine_ls_wR_factor_obs         0.0523
_reflns_number_observed          2535
_reflns_number_total             3045
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b209580g.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7050467
#BEGIN Tags that were not found in dictionaries:
_diffrn_measurement_domega       0.30
_diffrn_measurement_rtime        20
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ag Ag 0.120844(19) 0.15829(2) 0.119706(10) 0.04506(9) Uani 1 1 d . . .
N1 N 0.08731(19) 0.1420(2) -0.05044(11) 0.0394(5) Uani 1 1 d . . .
N2 N 0.15365(19) 0.1017(2) 0.00700(11) 0.0389(5) Uani 1 1 d . . .
C11 C 0.0011(2) 0.2410(3) -0.04164(13) 0.0357(6) Uani 1 1 d . . .
N12 N -0.02504(19) 0.2528(2) 0.02060(11) 0.0406(5) Uani 1 1 d . . .
C13 C -0.1091(3) 0.3455(3) 0.02231(15) 0.0498(7) Uani 1 1 d . . .
H13 H -0.1312 0.3574 0.0644 0.060 Uiso 1 1 calc R . .
C14 C -0.1640(3) 0.4242(3) -0.03688(16) 0.0555(8) Uani 1 1 d . . .
H14 H -0.2220 0.4872 -0.0331 0.067 Uiso 1 1 calc R . .
N15 N -0.1372(2) 0.4130(3) -0.09889(13) 0.0547(7) Uani 1 1 d . . .
C16 C -0.0530(3) 0.3204(3) -0.10014(14) 0.0463(7) Uani 1 1 d . . .
H16 H -0.0302 0.3092 -0.1421 0.056 Uiso 1 1 calc R . .
C21 C 0.2424(2) 0.0054(3) -0.00070(14) 0.0380(6) Uani 1 1 d . . .
N22 N 0.2942(2) -0.0605(3) 0.05969(12) 0.0508(6) Uani 1 1 d . . .
C23 C 0.3779(3) -0.1507(3) 0.05517(17) 0.0580(8) Uani 1 1 d . . .
H23 H 0.4170 -0.2000 0.0957 0.070 Uiso 1 1 calc R . .
C24 C 0.4084(3) -0.1731(3) -0.00798(18) 0.0582(8) Uani 1 1 d . . .
H24 H 0.4661 -0.2389 -0.0086 0.070 Uiso 1 1 calc R . .
N25 N 0.3586(2) -0.1045(3) -0.06783(13) 0.0542(6) Uani 1 1 d . . .
C26 C 0.2751(2) -0.0143(3) -0.06339(14) 0.0467(7) Uani 1 1 d . . .
H26 H 0.2376 0.0370 -0.1036 0.056 Uiso 1 1 calc R . .
N3 N -0.10138(19) -0.1636(2) 0.28759(11) 0.0357(5) Uani 1 1 d . . .
N4 N -0.18884(19) -0.1007(2) 0.25095(11) 0.0404(5) Uani 1 1 d . . .
C31 C 0.0025(2) -0.1393(3) 0.26508(13) 0.0325(6) Uani 1 1 d . . .
N32 N 0.09138(18) -0.2212(2) 0.29755(11) 0.0386(5) Uani 1 1 d . . .
C33 C 0.1904(2) -0.2018(3) 0.27882(15) 0.0432(7) Uani 1 1 d . . .
H33 H 0.2548 -0.2570 0.2999 0.052 Uiso 1 1 calc R . .
C34 C 0.2006(2) -0.1015(3) 0.22862(14) 0.0425(7) Uani 1 1 d . . .
H34 H 0.2713 -0.0918 0.2170 0.051 Uiso 1 1 calc R . .
N35 N 0.11145(18) -0.0191(2) 0.19687(11) 0.0369(5) Uani 1 1 d . . .
C36 C 0.0118(2) -0.0378(3) 0.21565(13) 0.0354(6) Uani 1 1 d . . .
H36 H -0.0523 0.0182 0.1952 0.043 Uiso 1 1 calc R . .
C41 C -0.2921(2) -0.1216(3) 0.27431(14) 0.0395(7) Uani 1 1 d . . .
N42 N -0.29148(19) -0.2028(2) 0.33034(12) 0.0448(6) Uani 1 1 d . . .
C43 C -0.3904(3) -0.2075(4) 0.34976(16) 0.0587(9) Uani 1 1 d . . .
H43 H -0.3947 -0.2624 0.3886 0.070 Uiso 1 1 calc R . .
C44 C -0.4869(3) -0.1327(4) 0.31371(19) 0.0748(11) Uani 1 1 d . . .
H44 H -0.5531 -0.1354 0.3307 0.090 Uiso 1 1 calc R . .
N45 N -0.4903(2) -0.0569(4) 0.25579(15) 0.0776(9) Uani 1 1 d . . .
C46 C -0.3906(3) -0.0527(3) 0.23642(16) 0.0575(8) Uani 1 1 d . . .
H46 H -0.3876 -0.0017 0.1961 0.069 Uiso 1 1 calc R . .
Cl Cl -0.30321(7) -0.39108(8) 0.09841(4) 0.0528(2) Uani 1 1 d D . .
O1 O -0.3173(2) -0.3241(2) 0.03083(12) 0.0795(7) Uani 1 1 d D . .
O2 O -0.1832(2) -0.3829(3) 0.13750(15) 0.1016(9) Uani 1 1 d D . .
O3 O -0.3315(2) -0.5361(2) 0.08708(13) 0.0859(8) Uani 1 1 d D . .
O4 O -0.3741(3) -0.3272(3) 0.13631(16) 0.1126(11) 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
N35 Ag N2 119.09(7) . . ?
N35 Ag N42 108.73(8) . 2 ?
N2 Ag N42 99.93(8) . 2 ?
N35 Ag N12 130.92(7) . . ?
N2 Ag N12 66.69(7) . . ?
N42 Ag N12 118.37(8) 2 . ?
N35 Ag N3 89.78(7) . 2 ?
N2 Ag N3 150.91(7) . 2 ?
N42 Ag N3 64.42(7) 2 2 ?
N12 Ag N3 98.09(7) . 2 ?
N2 N1 C11 113.5(2) . . ?
N1 N2 C21 114.4(2) . . ?
N1 N2 Ag 122.46(17) . . ?
C21 N2 Ag 122.75(16) . . ?
N12 C11 C16 122.4(2) . . ?
N12 C11 N1 120.5(2) . . ?
C16 C11 N1 117.1(2) . . ?
C11 N12 C13 115.5(2) . . ?
C11 N12 Ag 114.00(17) . . ?
C13 N12 Ag 127.77(17) . . ?
N12 C13 C14 121.9(3) . . ?
N12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
N15 C14 C13 122.5(3) . . ?
N15 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
C14 N15 C16 115.3(2) . . ?
N15 C16 C11 122.4(3) . . ?
N15 C16 H16 118.8 . . ?
C11 C16 H16 118.8 . . ?
N22 C21 C26 122.8(2) . . ?
N22 C21 N2 113.0(2) . . ?
C26 C21 N2 124.1(2) . . ?
C21 N22 C23 115.2(2) . . ?
N22 C23 C24 122.0(3) . . ?
N22 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
N25 C24 C23 122.7(3) . . ?
N25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C26 N25 C24 115.3(3) . . ?
N25 C26 C21 121.9(3) . . ?
N25 C26 H26 119.0 . . ?
C21 C26 H26 119.0 . . ?
N4 N3 C31 113.8(2) . . ?
N4 N3 Ag 120.70(16) . 2_545 ?
C31 N3 Ag 124.93(16) . 2_545 ?
N3 N4 C41 114.1(2) . . ?
N32 C31 C36 122.6(2) . . ?
N32 C31 N3 113.7(2) . . ?
C36 C31 N3 123.7(2) . . ?
C31 N32 C33 115.9(2) . . ?
N32 C33 C34 122.1(2) . . ?
N32 C33 H33 119.0 . . ?
C34 C33 H33 119.0 . . ?
N35 C34 C33 121.6(2) . . ?
N35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C34 N35 C36 116.6(2) . . ?
C34 N35 Ag 124.78(17) . . ?
C36 N35 Ag 118.47(17) . . ?
N35 C36 C31 121.2(2) . . ?
N35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?
N42 C41 C46 122.4(2) . . ?
N42 C41 N4 121.2(2) . . ?
C46 C41 N4 116.4(2) . . ?
C43 N42 C41 115.8(2) . . ?
C43 N42 Ag 125.8(2) . 2_545 ?
C41 N42 Ag 118.18(16) . 2_545 ?
N42 C43 C44 121.4(3) . . ?
N42 C43 H43 119.3 . . ?
C44 C43 H43 119.3 . . ?
N45 C44 C43 123.3(3) . . ?
N45 C44 H44 118.3 . . ?
C43 C44 H44 118.3 . . ?
C44 N45 C46 115.0(3) . . ?
N45 C46 C41 121.9(3) . . ?
N45 C46 H46 119.0 . . ?
C41 C46 H46 119.0 . . ?
O4 Cl O3 110.67(18) . . ?
O4 Cl O1 110.45(17) . . ?
O3 Cl O1 108.83(15) . . ?
O4 Cl O2 110.5(2) . . ?
O3 Cl O2 107.28(17) . . ?
O1 Cl O2 109.00(16) . . ?
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
Ag N35 2.278(2) . ?
Ag N2 2.385(2) . ?
Ag N42 2.402(2) 2 ?
Ag N12 2.405(2) . ?
Ag N3 2.526(2) 2 ?
N1 N2 1.248(3) . ?
N1 C11 1.433(3) . ?
N2 C21 1.434(3) . ?
C11 N12 1.331(3) . ?
C11 C16 1.377(4) . ?
N12 C13 1.338(3) . ?
C13 C14 1.385(4) . ?
C13 H13 0.9300 . ?
C14 N15 1.330(4) . ?
C14 H14 0.9300 . ?
N15 C16 1.337(4) . ?
C16 H16 0.9300 . ?
C21 N22 1.332(3) . ?
C21 C26 1.385(4) . ?
N22 C23 1.333(4) . ?
C23 C24 1.384(4) . ?
C23 H23 0.9300 . ?
C24 N25 1.331(4) . ?
C24 H24 0.9300 . ?
N25 C26 1.330(3) . ?
C26 H26 0.9300 . ?
N3 N4 1.249(3) . ?
N3 C31 1.432(3) . ?
N3 Ag 2.526(2) 2_545 ?
N4 C41 1.429(3) . ?
C31 N32 1.331(3) . ?
C31 C36 1.386(3) . ?
N32 C33 1.333(3) . ?
C33 C34 1.392(4) . ?
C33 H33 0.9300 . ?
C34 N35 1.333(3) . ?
C34 H34 0.9300 . ?
N35 C36 1.339(3) . ?
C36 H36 0.9300 . ?
C41 N42 1.334(3) . ?
C41 C46 1.375(4) . ?
N42 C43 1.326(3) . ?
N42 Ag 2.402(2) 2_545 ?
C43 C44 1.375(4) . ?
C43 H43 0.9300 . ?
C44 N45 1.329(4) . ?
C44 H44 0.9300 . ?
N45 C46 1.335(4) . ?
C46 H46 0.9300 . ?
Cl O4 1.395(2) . ?
Cl O3 1.422(2) . ?
Cl O1 1.430(2) . ?
Cl O2 1.432(2) . ?
