# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 440/081 # CIF for {[Ag(pyrazine)]NO2}n data_NOAGPZ _audit_creation_date 97-09-27 _audit_creation_method CRYSTALS # noagpz in Cc _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution DIRDIF _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Stoe Stadi-4 diffractometer equipped with an Oxford Cryosystems l.t. device. ; _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Patterson _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment 'Placed geometrically after each cycle' #**************************************************************************** _chemical_name_systematic ; '[Silver(I)(pyrazine)NO2]' ? ; _cell_length_a 12.378(5) _cell_angle_alpha 90 _cell_length_b 7.934(3) _cell_angle_beta 99.07(3) _cell_length_c 6.322(3) _cell_angle_gamma 90 _cell_volume 613.04 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0170 0.0090 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0290 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0470 0.0320 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Ag ' -0.0600 4.2820 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C4 H4 Ag1 N3 O2' _chemical_formula_moiety '[Ag(C4H4N2)(NO2)]' _chemical_compound_source ; ? ; _chemical_formula_weight 233.96 _cell_measurement_reflns_used 42 _cell_measurement_theta_min 17 _cell_measurement_theta_max 22 _cell_measurement_temperature 220 _cell_formula_units_Z 4.00 _exptl_crystal_description 'plate developed in (100) ' _exptl_crystal_colour 'Colourless ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 2.53 _exptl_crystal_density_meas ? _exptl_crystal_F_000 449.02 _exptl_absorpt_coefficient_mu 26.42 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.203 _exptl_absorpt_correction_T_max 0.785 _diffrn_standards_interval_time 60 _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 220 _diffrn_reflns_number 2068 _reflns_number_total 554 _diffrn_reflns_av_R_equivalents 0.10 _reflns_number_observed 480 _diffrn_reflns_theta_min 6.65 _diffrn_reflns_theta_max 70.18 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 7 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -1.28 _refine_diff_density_max 1.65 _refine_ls_number_reflns 480 _refine_ls_number_parameters 48 _refine_ls_R_factor_obs 0.0443 _refine_ls_wR_factor_obs 0.0459 _refine_ls_goodness_of_fit_obs 1.0532 _refine_ls_shift/esd_max 0.022061 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method Omega-theta loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type AG1 0.0000 0.03765(9) 0.2500 0.0423 1.0000 Uani N1 0.1585(4) 0.1680(7) 0.3941(9) 0.0368 1.0000 Uani C2 0.2412(5) 0.0811(8) 0.506(1) 0.0384 1.0000 Uani C3 0.1676(5) 0.3358(8) 0.389(1) 0.0370 1.0000 Uani N4 0.0000 -0.332(1) 0.2500 0.0449 1.0000 Uani O5 -0.0718(5) -0.2464(7) 0.1357(9) 0.0562 1.0000 Uani H21 0.2371 -0.0444 0.5125 0.0371 1.0000 Uiso H31 0.1070 0.4033 0.3056 0.0355 1.0000 Uiso 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 0.0347(4) 0.0311(5) 0.0559(5) 0.0000 -0.0085(3) 0.0000 N1 0.035(3) 0.031(3) 0.040(3) 0.001(2) -0.004(2) -0.002(2) C2 0.040(3) 0.029(3) 0.044(3) -0.000(3) -0.001(3) 0.001(3) C3 0.032(3) 0.032(3) 0.044(3) 0.005(2) -0.003(2) -0.000(2) N4 0.052(5) 0.023(4) 0.056(5) 0.0000 -0.003(4) 0.0000 O5 0.053(3) 0.046(3) 0.065(3) 0.003(3) -0.004(2) 0.005(2) _refine_ls_extinction_coef 6.1(9) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag AG1 . AG1 2_555 3.2168(3) yes AG1 . AG1 2_556 3.2168(3) yes AG1 . N1 . 2.277(5) yes AG1 . N1 5_555 2.277(5) yes AG1 . O5 . 2.487(6) yes AG1 . O5 5_555 2.487(6) yes N1 . C2 . 1.339(8) yes N1 . C3 . 1.336(8) yes C2 . C3 4_556 1.385(9) yes C2 . H21 . 0.998(6) no C3 . H31 . 1.001(6) no N4 . O5 . 1.254(7) yes N4 . O5 5_555 1.254(7) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag AG1 2_555 AG1 . AG1 2_556 158.59(5) yes AG1 2_555 AG1 . N1 . 110.1(1) yes AG1 2_556 AG1 . N1 . 79.9(1) yes AG1 2_555 AG1 . N1 5_555 79.9(1) yes AG1 2_556 AG1 . N1 5_555 110.1(1) yes N1 . AG1 . N1 5_555 126.0(3) yes AG1 2_555 AG1 . O5 . 66.5(1) yes AG1 2_556 AG1 . O5 . 93.5(1) yes N1 . AG1 . O5 . 140.7(2) yes N1 5_555 AG1 . O5 . 92.8(2) yes AG1 2_555 AG1 . O5 5_555 93.5(1) yes AG1 2_556 AG1 . O5 5_555 66.5(1) yes N1 . AG1 . O5 5_555 92.8(2) yes N1 5_555 AG1 . O5 5_555 140.7(2) yes O5 . AG1 . O5 5_555 50.1(2) yes AG1 . N1 . C2 . 121.1(4) yes AG1 . N1 . C3 . 120.8(4) yes C2 . N1 . C3 . 117.8(5) yes N1 . C2 . C3 4_556 120.4(6) yes N1 . C2 . H21 . 119.7(6) no C3 4_556 C2 . H21 . 119.8(6) no N1 . C3 . C2 4_556 121.8(6) yes N1 . C3 . H31 . 119.2(6) no C2 4_556 C3 . H31 . 119.0(6) no O5 . N4 . O5 5_555 114.4(8) yes AG1 . O5 . N4 . 97.7(4) yes # CIF for {[Ag(4,4'bipy)]NO2}n data_agbpno _audit_creation_method SHELXL-97 _chemical_name_systematic ; '[Silver(I)(4,4'-bipyridyl)]nitrite' ; _chemical_name_common '[Ag(4,4'bipy)NO2]' _chemical_melting_point ? _chemical_formula_moiety [Ag(C10H8N2)]NO2 _chemical_formula_sum 'C10 H8 Ag N3 O2' _chemical_formula_weight 310.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 7.2931(12) _cell_length_b 6.087(2) _cell_length_c 11.481(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.871(17) _cell_angle_gamma 90.00 _cell_volume 496.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description 'plate developed in (010)' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 16.195 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.198 _exptl_absorpt_correction_T_max 0.720 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4' _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2432 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 6.59 _diffrn_reflns_theta_max 70.01 _reflns_number_total 880 _reflns_number_gt 838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0485P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 880 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.2500 0.02322(4) 0.2500 0.03118(14) Uani 1 2 d S . . N1 N 0.2474(3) -0.0021(3) 0.0578(2) 0.0257(5) Uani 1 1 d . . . C2 C 0.1904(4) 0.1725(4) -0.0125(2) 0.0272(6) Uani 1 1 d . . . H2 H 0.1498 0.2982 0.0221 0.033 Uiso 1 1 calc R . . C3 C 0.1884(4) 0.1766(4) -0.1327(2) 0.0255(5) Uani 1 1 d . . . H3 H 0.1474 0.3028 -0.1783 0.031 Uiso 1 1 calc R . . C4 C 0.2478(3) -0.0080(4) -0.1865(3) 0.0241(5) Uani 1 1 d . . . C5 C 0.3059(4) -0.1900(4) -0.1131(3) 0.0258(6) Uani 1 1 d . . . H5 H 0.3464 -0.3184 -0.1454 0.031 Uiso 1 1 calc R . . C6 C 0.3037(4) -0.1807(4) 0.0063(2) 0.0271(6) Uani 1 1 d . . . H6 H 0.3433 -0.3048 0.0540 0.032 Uiso 1 1 calc R . . N10 N 0.2500 0.5339(5) 0.2500 0.0392(9) Uani 1 2 d S . . O11 O 0.3952(3) 0.4259(4) 0.2537(2) 0.0442(6) Uani 1 1 d . . . 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 0.04372(19) 0.03633(18) 0.0155(2) 0.000 0.01079(12) 0.000 N1 0.0292(10) 0.0290(10) 0.0192(13) -0.0010(9) 0.0059(9) -0.0041(8) C2 0.0301(13) 0.0291(12) 0.0233(16) -0.0025(11) 0.0074(11) 0.0010(10) C3 0.0306(13) 0.0280(11) 0.0177(14) 0.0015(10) 0.0050(10) 0.0023(10) C4 0.0238(11) 0.0269(11) 0.0219(15) -0.0002(10) 0.0060(9) -0.0025(10) C5 0.0312(13) 0.0253(11) 0.0219(14) -0.0007(10) 0.0082(11) -0.0003(10) C6 0.0334(13) 0.0275(12) 0.0207(15) 0.0026(11) 0.0068(11) -0.0005(10) N10 0.059(2) 0.0276(15) 0.034(2) 0.000 0.0170(18) 0.000 O11 0.0402(12) 0.0413(11) 0.0537(16) -0.0073(11) 0.0163(11) -0.0056(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.208(3) . ? Ag1 N1 2.208(3) 2 ? N1 C2 1.343(3) . ? N1 C6 1.345(3) . ? C2 C3 1.377(4) . ? C3 C4 1.396(4) . ? C4 C5 1.399(4) . ? C4 C4 1.466(6) 2_554 ? C5 C6 1.376(4) . ? N10 O11 1.239(3) 2 ? N10 O11 1.239(3) . ? 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 171.98(10) . 2 ? C2 N1 C6 117.3(2) . . ? C2 N1 Ag1 118.54(17) . . ? C6 N1 Ag1 124.13(18) . . ? N1 C2 C3 123.3(2) . . ? C2 C3 C4 119.6(2) . . ? C3 C4 C5 116.9(3) . . ? C3 C4 C4 121.16(18) . 2_554 ? C5 C4 C4 121.88(18) . 2_554 ? C6 C5 C4 119.9(2) . . ? N1 C6 C5 123.0(2) . . ? O11 N10 O11 115.9(3) 2 . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 70.01 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.497 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.071