#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/50/2225046.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2225046
loop_
_publ_author_name
'Starosta, Wojciech'
'Leciejewicz, Janusz'
_publ_section_title
catena-Poly[lead(II)-bis(μ₂-pyridazine-3-carboxylato-κ³N²,O:O)]
_journal_coeditor_code           KP2247
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m192
_journal_paper_doi               10.1107/S1600536810002199
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C5 H3 N2 O2)2]'
_chemical_formula_moiety         'C10 H6 N4 O4 Pb'
_chemical_formula_sum            'C10 H6 N4 O4 Pb'
_chemical_formula_weight         453.38
_chemical_name_systematic
;
catena-Poly[lead(II)-bis(μ₂-pyridazine-3-carboxylato-
κ³N²,O:O)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0336(16)
_cell_length_b                   10.386(2)
_cell_length_c                   13.766(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      6
_cell_volume                     1146.2(4)
_computing_cell_refinement       'KM-4 Software (Kuma, 1996)'
_computing_data_collection       'KM-4 Software (Kuma, 1996)'
_computing_data_reduction        'DATAPROC (Kuma, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Kuma KM-4 four-circle diffractometer'
_diffrn_measurement_method       'profile data from ω/2θ 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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3587
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        1.27
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.736
_exptl_absorpt_correction_T_max  0.37881
_exptl_absorpt_correction_T_min  0.28392
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.081
_refine_diff_density_max         6.566
_refine_diff_density_min         -4.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0903P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                2119
_reflns_number_total             3365
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            kp2247.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2225046
_cod_database_fobs_code          2225046
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.25237(3) 1.03613(3) 1.006155(19) 0.02242(12) Uani d . 1 . .
O O11 0.0180(7) 0.9406(6) 0.8924(4) 0.0250(12) Uani d . 1 . .
N N12 0.3296(8) 0.8553(6) 0.8814(5) 0.0224(13) Uani d . 1 . .
N N22 0.1664(8) 0.8074(6) 1.0764(5) 0.0214(13) Uani d . 1 . .
O O21 0.4781(8) 0.9011(6) 1.0862(5) 0.0301(13) Uani d . 1 . .
N N21 0.0078(8) 0.7670(7) 1.0745(5) 0.0259(15) Uani d . 1 . .
O O12 -0.0827(8) 0.7546(6) 0.8339(6) 0.0388(17) Uani d . 1 . .
O O22 0.5838(9) 0.7035(7) 1.1022(7) 0.052(2) Uani d . 1 . .
N N11 0.4876(9) 0.8212(8) 0.8732(6) 0.0291(16) Uani d . 1 . .
C C16 0.5237(12) 0.7161(9) 0.8257(7) 0.033(2) Uani d . 1 . .
H H16 0.6349 0.6937 0.8203 0.039 Uiso calc R 1 . .
C C14 0.2380(10) 0.6694(8) 0.7923(6) 0.0257(16) Uani d . 1 . .
H H14 0.1517 0.6183 0.7656 0.031 Uiso calc R 1 . .
C C26 -0.0251(11) 0.6477(9) 1.0961(7) 0.0311(19) Uani d . 1 . .
H H26 -0.1358 0.6214 1.0959 0.037 Uiso calc R 1 . .
C C17 0.0322(10) 0.8273(8) 0.8564(6) 0.0207(15) Uani d . 1 . .
C C13 0.2049(9) 0.7810(7) 0.8424(5) 0.0182(14) Uani d . 1 . .
C C23 0.2885(10) 0.7262(8) 1.0976(6) 0.0260(17) Uani d . 1 . .
C C15 0.3974(11) 0.6369(9) 0.7831(6) 0.0316(19) Uani d . 1 . .
H H15 0.4240 0.5631 0.7492 0.038 Uiso calc R 1 . .
C C27 0.4639(10) 0.7783(8) 1.0958(6) 0.0256(17) Uani d . 1 . .
C C24 0.2584(14) 0.5976(9) 1.1172(9) 0.047(3) Uani d . 1 . .
H H24 0.3460 0.5399 1.1286 0.056 Uiso calc R 1 . .
C C25 0.1003(13) 0.5593(10) 1.1192(9) 0.045(3) Uani d . 1 . .
H H25 0.0747 0.4751 1.1357 0.055 Uiso calc R 1 . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O21 Pb1 O11 . . 122.4(2) ?
O21 Pb1 N12 . . 72.1(2) ?
O11 Pb1 N12 . . 61.55(19) ?
O21 Pb1 O21 . 3_677 76.0(2) ?
O11 Pb1 O21 . 3_677 112.9(2) ?
N12 Pb1 O21 . 3_677 68.4(2) ?
O21 Pb1 O11 . 3_577 114.4(2) ?
O11 Pb1 O11 . 3_577 76.4(2) ?
N12 Pb1 O11 . 3_577 129.6(2) ?
O21 Pb1 O11 3_677 3_577 160.5(2) ?
O21 Pb1 N22 . . 62.5(2) ?
O11 Pb1 N22 . . 71.4(2) ?
N12 Pb1 N22 . . 71.4(2) ?
O21 Pb1 N22 3_677 . 128.9(2) ?
O11 Pb1 N22 3_577 . 69.7(2) ?
C17 O11 Pb1 . . 120.6(5) ?
C17 O11 Pb1 . 3_577 112.3(5) ?
Pb1 O11 Pb1 . 3_577 103.6(2) ?
N11 N12 C13 . . 120.1(7) ?
N11 N12 Pb1 . . 120.6(5) ?
C13 N12 Pb1 . . 117.8(5) ?
C23 N22 N21 . . 119.9(7) ?
C23 N22 Pb1 . . 116.4(5) ?
N21 N22 Pb1 . . 122.6(5) ?
C27 O21 Pb1 . . 122.4(5) ?
C27 O21 Pb1 . 3_677 111.8(6) ?
Pb1 O21 Pb1 . 3_677 104.0(2) ?
C26 N21 N22 . . 120.0(8) ?
C16 N11 N12 . . 120.4(7) ?
N11 C16 C15 . . 121.1(8) ?
N11 C16 H16 . . 119.4 ?
C15 C16 H16 . . 119.4 ?
C15 C14 C13 . . 118.4(8) ?
C15 C14 H14 . . 120.8 ?
C13 C14 H14 . . 120.8 ?
N21 C26 C25 . . 121.8(9) ?
N21 C26 H26 . . 119.1 ?
C25 C26 H26 . . 119.1 ?
O12 C17 O11 . . 125.6(8) ?
O12 C17 C13 . . 117.6(7) ?
O11 C17 C13 . . 116.8(7) ?
N12 C13 C14 . . 121.1(7) ?
N12 C13 C17 . . 115.9(6) ?
C14 C13 C17 . . 123.0(7) ?
N22 C23 C24 . . 121.7(8) ?
N22 C23 C27 . . 116.8(7) ?
C24 C23 C27 . . 121.5(8) ?
C14 C15 C16 . . 118.9(8) ?
C14 C15 H15 . . 120.6 ?
C16 C15 H15 . . 120.6 ?
O22 C27 O21 . . 123.7(8) ?
O22 C27 C23 . . 119.8(8) ?
O21 C27 C23 . . 116.5(7) ?
C25 C24 C23 . . 118.0(9) ?
C25 C24 H24 . . 121.0 ?
C23 C24 H24 . . 121.0 ?
C24 C25 C26 . . 118.5(9) ?
C24 C25 H25 . . 120.8 ?
C26 C25 H25 . . 120.8 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 O21 . 2.492(7) yes
Pb1 O11 . 2.569(6) yes
Pb1 N12 . 2.645(7) yes
Pb1 O21 3_677 2.662(7) yes
Pb1 O11 3_577 2.669(6) yes
Pb1 N22 . 2.672(6) yes
O11 C17 . 1.285(10) ?
O11 Pb1 3_577 2.669(6) ?
N12 N11 . 1.330(10) ?
N12 C13 . 1.348(9) ?
N22 C23 . 1.312(10) ?
N22 N21 . 1.340(9) ?
O21 C27 . 1.289(10) ?
O21 Pb1 3_677 2.662(7) ?
N21 C26 . 1.305(11) ?
O12 C17 . 1.217(10) ?
O22 C27 . 1.237(10) ?
N11 C16 . 1.315(12) ?
C16 C15 . 1.405(12) ?
C16 H16 . 0.9300 ?
C14 C15 . 1.338(12) ?
C14 C13 . 1.384(11) ?
C14 H14 . 0.9300 ?
C26 C25 . 1.385(13) ?
C26 H26 . 0.9300 ?
C17 C13 . 1.493(11) ?
C23 C24 . 1.386(12) ?
C23 C27 . 1.511(12) ?
C15 H15 . 0.9300 ?
C24 C25 . 1.334(14) ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C16 H16 O12 1_655 0.93 2.35 3.182(12) 148.5
C14 H14 O21 4_575 0.93 2.76 3.489(10) 135.6
C26 H26 O22 1_455 0.93 2.42 3.201(12) 142.2
C15 H15 O11 2_546 0.93 2.40 3.266(10) 155.4
C25 H25 O12 3_567 0.93 2.42 3.328(12) 164.8
