# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/097 data_pbnew _audit_creation_method SHELXL-97 _chemical_name_systematic ; lead(II)diaquo-3,6-dicarboxylatopyridazine ; _chemical_name_common lead(II)diaquo-3,6-dicarboxylatopyridazine _chemical_formula_moiety 'C6 H6 N2 O6 Pb' _chemical_formula_sum 'C6 H6 N2 O6 Pb' _chemical_formula_weight 409.32 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, y+1/2, -z+1/4' '-x, -y+1/2, -z+1/4' 'y, -x, -z' '-y, x, -z' '-y, x+1/2, z+1/4' 'y, -x+1/2, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, y+1, -z+3/4' '-x+1/2, -y+1, -z+3/4' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-y+1/2, x+1, z+3/4' 'y+1/2, -x+1, z+3/4' _cell_length_a 15.278(2) _cell_length_b 15.278(2) _cell_length_c 15.218(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3552.1(10) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.1 _cell_measurement_theta_max 19.0 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 3.03(3) _exptl_crystal_density_diffrn 3.062 _exptl_crystal_density_method 'Helium pycnometer' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 19.011 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.2652 _exptl_absorpt_correction_T_max 0.8328 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method 'omega-2 theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time '2 hours' _diffrn_standards_decay_% none _diffrn_reflns_number 4892 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.09 _reflns_number_total 1450 _reflns_number_gt 1316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 package' _computing_cell_refinement id _computing_data_reduction id _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP(Siemens, 1990)' _computing_publication_material 'XPUBL (Siemens 1991)' _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 w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+16.9366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00048(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 1450 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.001 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.27112(2) 0.30217(2) 0.03571(2) 0.02490(13) Uani 1 d . . . O1 O 0.2477(4) 0.1367(4) -0.3011(4) 0.0348(15) Uani 1 d . . . O2 O 0.3253(4) 0.0138(4) -0.3160(4) 0.0412(16) Uani 1 d . . . O3 O 0.3395(4) 0.1784(4) 0.1224(4) 0.0316(14) Uani 1 d . . . O4 O 0.4017(4) 0.0446(4) 0.1304(4) 0.0440(17) Uani 1 d . . . C1 C 0.3212(5) 0.0791(5) -0.1769(5) 0.0222(17) Uani 1 d . . . N2 N 0.2911(4) 0.1467(4) -0.1335(4) 0.0263(15) Uani 1 d . . . N3 N 0.3095(5) 0.1549(4) -0.0479(5) 0.0293(16) Uani 1 d . . . C4 C 0.3531(5) 0.0920(5) -0.0069(5) 0.0218(17) Uani 1 d . . . C5 C 0.3859(5) 0.0189(5) -0.0500(6) 0.029(2) Uani 1 d . . . H5A H 0.4178 -0.0259 -0.0193 0.080 Uiso 1 d R . . C6 C 0.3703(5) 0.0130(5) -0.1377(6) 0.0290(19) Uani 1 d . . . H6A H 0.3938 -0.0346 -0.1715 0.080 Uiso 1 d R . . C7 C 0.2974(5) 0.0757(6) -0.2734(6) 0.0283(19) Uani 1 d . . . C8 C 0.3663(5) 0.1060(6) 0.0907(6) 0.0275(19) Uani 1 d . . . O31 O 0.4399(5) 0.3511(5) 0.0500(5) 0.056(2) Uani 1 d . . . H31B H 0.4758 0.3347 0.0892 0.080 Uiso 1 d R . . H31A H 0.4510 0.3861 0.0082 0.050 Uiso 1 d R . . O32 O 0.1966(5) 0.4656(4) 0.0062(5) 0.0493(18) Uani 1 d . . . H32B H 0.1479 0.4751 -0.0192 0.080 Uiso 1 d R . . H32A H 0.2308 0.5045 0.0270 0.050 Uiso 1 d R . . 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 Pb1 0.0282(2) 0.0276(2) 0.01888(18) -0.00053(14) -0.00022(14) 0.00136(13) O1 0.050(4) 0.031(3) 0.023(3) 0.004(3) -0.002(3) 0.009(3) O2 0.053(4) 0.041(4) 0.029(3) -0.016(3) 0.005(3) 0.005(3) O3 0.040(4) 0.035(3) 0.019(3) 0.002(3) 0.001(3) 0.010(3) O4 0.058(4) 0.043(4) 0.032(4) 0.004(3) -0.010(3) 0.022(3) C1 0.029(4) 0.022(4) 0.015(4) -0.002(3) 0.004(3) -0.004(3) N2 0.034(4) 0.025(4) 0.020(4) 0.001(3) 0.001(3) 0.003(3) N3 0.032(4) 0.030(4) 0.026(4) -0.004(3) -0.002(3) 0.002(3) C4 0.013(4) 0.028(4) 0.025(4) 0.004(4) -0.005(3) 0.003(3) C5 0.026(4) 0.026(4) 0.036(6) 0.009(4) -0.004(4) 0.003(3) C6 0.035(5) 0.025(4) 0.027(5) -0.002(4) 0.007(4) 0.001(4) C7 0.027(4) 0.035(5) 0.023(5) 0.000(4) 0.005(4) -0.013(4) C8 0.023(4) 0.038(5) 0.021(5) 0.001(4) -0.002(4) 0.000(4) O31 0.048(4) 0.067(5) 0.055(5) 0.011(4) -0.010(4) -0.011(4) O32 0.054(4) 0.047(4) 0.047(4) 0.002(4) -0.009(4) 0.004(3) _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 Pb1 O3 2.532(6) . yes Pb1 O1 2.558(6) 8 yes Pb1 N3 2.651(7) . yes Pb1 O3 2.664(6) 15_544 yes Pb1 O1 2.668(6) 10 yes Pb1 N2 2.675(7) 8 yes Pb1 O31 2.694(7) . yes O1 C7 1.275(10) . yes O1 Pb1 2.558(6) 15_544 no O1 Pb1 2.668(6) 10_554 no O2 C7 1.222(10) . yes O3 C8 1.275(10) . yes O3 Pb1 2.664(6) 8 no O4 C8 1.241(10) . yes C1 N2 1.309(10) . yes C1 C6 1.393(12) . yes C1 C7 1.514(11) . yes N2 N3 1.339(10) . yes N2 Pb1 2.675(7) 15_544 no N3 C4 1.325(10) . yes C4 C5 1.388(12) . yes C4 C8 1.514(12) . yes C5 C6 1.359(12) . yes 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 O3 Pb1 O1 112.22(19) . 8 yes O3 Pb1 N3 61.6(2) . . yes O1 Pb1 N3 71.1(2) 8 . yes O3 Pb1 O3 121.78(15) . 15_544 yes O1 Pb1 O3 79.30(17) 8 15_544 yes N3 Pb1 O3 70.7(2) . 15_544 yes O3 Pb1 O1 79.68(18) . 10 yes O1 Pb1 O1 119.90(15) 8 10 yes N3 Pb1 O1 140.1(2) . 10 yes O3 Pb1 O1 145.51(18) 15_544 10 yes O3 Pb1 N2 69.9(2) . 8 yes O1 Pb1 N2 60.5(2) 8 8 yes N3 Pb1 N2 85.7(2) . 8 yes O3 Pb1 N2 138.48(19) 15_544 8 yes O1 Pb1 N2 71.48(19) 10 8 yes O3 Pb1 O31 76.7(2) . . yes O1 Pb1 O31 153.2(2) 8 . yes N3 Pb1 O31 93.6(2) . . yes O3 Pb1 O31 74.8(2) 15_544 . yes O1 Pb1 O31 86.0(2) 10 . yes N2 Pb1 O31 142.3(2) 8 . yes C7 O1 Pb1 126.4(5) . 15_544 yes C7 O1 Pb1 128.9(5) . 10_554 yes Pb1 O1 Pb1 99.65(19) 15_544 10_554 yes C8 O3 Pb1 125.7(5) . . yes C8 O3 Pb1 132.4(5) . 8 yes Pb1 O3 Pb1 100.45(19) . 8 yes N2 C1 C6 123.0(8) . . no N2 C1 C7 115.7(7) . . no C6 C1 C7 121.3(7) . . no C1 N2 N3 119.4(7) . . no C1 N2 Pb1 121.0(5) . 15_544 no N3 N2 Pb1 119.5(5) . 15_544 no C4 N3 N2 119.7(7) . . no C4 N3 Pb1 120.1(5) . . no N2 N3 Pb1 120.0(5) . . no N3 C4 C5 122.9(8) . . no N3 C4 C8 115.2(7) . . no C5 C4 C8 121.9(7) . . no C6 C5 C4 117.0(8) . . no C5 C6 C1 117.9(8) . . no O2 C7 O1 126.7(8) . . no O2 C7 C1 117.3(8) . . no O1 C7 C1 116.0(8) . . no O4 C8 O3 127.7(8) . . no O4 C8 C4 115.4(7) . . no O3 C8 C4 116.9(7) . . no _diffrn_measured_fraction_theta_max 0.458 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.458 _refine_diff_density_max 0.773 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.177