#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:38:33 +0100 (vie 25 de mar de 2016) $
#$Revision: 180089 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/35/7053540.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_7053540
loop_
_publ_author_name
'Kalf, Irmgard'
'Mathieu, Patrick'
'Englert, Ulli'
_publ_section_title
;
 From crystal to crystal: a new polymorph of
 (4-carboxylatopyridine)silver(i) by topotactic dehydration of its
 monohydrate
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2491
_journal_paper_doi               10.1039/c0nj00144a
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C6 H4 Ag N O2, H2 O'
_chemical_formula_sum            'C6 H6 Ag N O3'
_chemical_formula_weight         247.99
_chemical_name_common            'compound 1'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.982(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   3.6519(5)
_cell_length_b                   12.1512(18)
_cell_length_c                   15.070(2)
_cell_measurement_reflns_used    1754
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      2.15
_cell_volume                     668.63(16)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full .989
_diffrn_measured_fraction_theta_max .989
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6029
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.961
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'PLATON (Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.797
_refine_diff_density_min         -2.468
_refine_diff_density_rms         .208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1447
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0749
_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)+(0.0400P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                941
_reflns_number_total             1447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00144a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7053540
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
Ag1 Ag 0.6044(3) 0.57393(8) 0.07548(6) 0.0600(4) Uani 1 1 d .
O1 O 1.116(2) 0.4462(9) 0.1015(8) 0.093(4) Uani 1 1 d U
O2 O 1.169(2) 0.2889(9) 0.0226(6) 0.073(3) Uani 1 1 d U
N1 N 0.617(2) 0.1693(8) 0.3069(5) 0.035(2) Uani 1 1 d .
C1 C 1.069(3) 0.3409(13) 0.0886(10) 0.064(4) Uani 1 1 d .
C2 C 0.905(2) 0.2824(8) 0.1646(7) 0.033(2) Uani 1 1 d .
C3 C 0.861(3) 0.3317(9) 0.2468(8) 0.047(3) Uani 1 1 d .
H3 H 0.9298 0.4064 0.2555 0.056 Uiso 1 1 calc R
C4 C 0.720(3) 0.2724(10) 0.3148(7) 0.044(3) Uani 1 1 d .
H4 H 0.6950 0.3073 0.3708 0.053 Uiso 1 1 calc R
C5 C 0.660(2) 0.1205(8) 0.2281(6) 0.028(2) Uani 1 1 d .
H5 H 0.5898 0.0456 0.2218 0.033 Uiso 1 1 calc R
C6 C 0.801(2) 0.1735(8) 0.1564(6) 0.031(2) Uani 1 1 d .
H6 H 0.8269 0.1360 0.1016 0.037 Uiso 1 1 calc R
O3 O 0.245(4) 0.4351(9) 0.4685(7) 0.125(5) Uani 1 1 d .
H3A H 0.1045 0.4762 0.4984 0.187 Uiso 0.50 1 d PR
H3B H 0.4344 0.4638 0.4462 0.187 Uiso 1 1 d R
H3C H 0.2532 0.3682 0.4849 0.187 Uiso 0.50 1 d PR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0838(8) 0.0606(6) 0.0370(5) -0.0220(4) 0.0390(5) -0.0342(5)
O1 0.042(5) 0.088(7) 0.150(10) 0.067(7) 0.006(6) -0.010(5)
O2 0.027(4) 0.134(8) 0.058(5) 0.055(6) 0.007(4) 0.001(5)
N1 0.025(4) 0.061(6) 0.019(4) 0.001(4) 0.005(3) 0.009(4)
C1 0.019(6) 0.086(11) 0.087(11) 0.053(9) 0.005(6) -0.002(6)
C2 0.012(5) 0.042(6) 0.046(6) 0.013(5) -0.002(4) -0.001(4)
C3 0.036(6) 0.039(6) 0.066(8) -0.015(6) -0.007(6) 0.000(5)
C4 0.035(6) 0.058(8) 0.040(6) -0.025(5) 0.001(5) 0.009(5)
C5 0.022(5) 0.037(5) 0.025(5) 0.006(4) 0.000(4) 0.004(4)
C6 0.029(5) 0.046(6) 0.018(4) -0.004(4) 0.003(4) -0.001(5)
O3 0.190(14) 0.113(10) 0.072(7) -0.028(7) 0.046(8) -0.025(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 '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 O2 105.0(4) 2_655 3_765
N1 Ag1 O1 85.8(4) 2_655 1_455
O2 Ag1 O1 145.0(3) 3_765 1_455
N1 Ag1 O1 118.5(4) 2_655 .
O2 Ag1 O1 105.7(3) 3_765 .
O1 Ag1 O1 97.5(3) 1_455 .
N1 Ag1 Ag1 144.0(2) 2_655 3_665
O2 Ag1 Ag1 92.0(3) 3_765 3_665
O1 Ag1 Ag1 63.6(3) 1_455 3_665
O1 Ag1 Ag1 85.7(3) . 3_665
C1 O1 Ag1 134.9(8) . 1_655
C1 O1 Ag1 119.9(8) . .
Ag1 O1 Ag1 97.5(3) 1_655 .
C1 O2 Ag1 104.6(9) . 3_765
C4 N1 C5 117.7(9) . .
C4 N1 Ag1 121.3(7) . 2_645
C5 N1 Ag1 120.9(7) . 2_645
O2 C1 O1 125.4(12) . .
O2 C1 C2 120.3(13) . .
O1 C1 C2 114.2(14) . .
C6 C2 C3 117.2(9) . .
C6 C2 C1 120.3(11) . .
C3 C2 C1 122.4(11) . .
C4 C3 C2 119.6(10) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
N1 C4 C3 123.3(9) . .
N1 C4 H4 118.4 . .
C3 C4 H4 118.4 . .
N1 C5 C6 123.0(9) . .
N1 C5 H5 118.5 . .
C6 C5 H5 118.5 . .
C5 C6 C2 119.2(9) . .
C5 C6 H6 120.4 . .
C2 C6 H6 120.4 . .
H3A O3 H3B 118.1 . .
H3A O3 H3C 115.4 . .
H3B O3 H3C 118.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.277(8) 2_655
Ag1 O2 2.385(8) 3_765
Ag1 O1 2.403(9) 1_455
Ag1 O1 2.454(9) .
Ag1 Ag1 2.9879(17) 3_665
O1 C1 1.305(18) .
O1 Ag1 2.402(9) 1_655
O2 C1 1.239(17) .
O2 Ag1 2.385(8) 3_765
N1 C4 1.312(13) .
N1 C5 1.339(11) .
N1 Ag1 2.277(8) 2_645
C1 C2 1.482(14) .
C2 C6 1.381(14) .
C2 C3 1.388(14) .
C3 C4 1.362(15) .
C3 H3 0.9500 .
C4 H4 0.9500 .
C5 C6 1.366(12) .
C5 H5 0.9500 .
C6 H6 0.9500 .
O3 H3A 0.8500 .
O3 H3B 0.8500 .
O3 H3C 0.8499 .
