A bicapped trigonal‒prismatic lead complex: <i>catena</i>-poly[[[aquabis(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')lead(II)]-μ-squarato-κ<i>O</i>^1^:κ^2^<i>O</i>^2^,<i>O</i>^3^] dihydrate]
Uçar, İbrahim; Bulut, Ahmet; Kazak, Canan; Acta Crystallographica Section C 61 (2005) m428–m431; doi:10.1107/S0108270105024613

data_2015066
_publ_section_title
;A bicapped trigonal--prismatic lead complex:
 <i>catena</i>-poly[[[aquabis(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')lead(II)]-\m-squarato-\k<i>O</i>^1^:\k^2^<i>O</i>^2^,<i>O</i>^3^]
 dihydrate]
;
_journal_coeditor_code           SK1858
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m428
_journal_page_last               m431
_journal_paper_doi               10.1107/S0108270105024613
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Pb (C4 O4) (C12 H8 N2)2 (H2 O)], 2H2 O'
_chemical_formula_moiety         'C28 H18 N4 O5 Pb, 2H2 O'
_chemical_formula_sum            'C28 H22 N4 O7 Pb'
_chemical_formula_weight         733.70
_chemical_name_systematic
;
catena-poly[[[aquabis(1,10-phenanthroline-\k^2^N,N')lead(II)]-
\m~1,2,3~-squarato-\kO:O':O''] dihydrate]
;
_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                 106.578(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5438(10)
_cell_length_b                   7.2746(3)
_cell_length_c                   19.8774(11)
_cell_measurement_reflns_used    5847
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      1.77
_cell_volume                     2570.0(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEPIII (Farrugia, 1997)'
_computing_publication_material  'WinGX  (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       \w
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39366
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.12
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.621
_exptl_absorpt_correction_T_max  0.6658
_exptl_absorpt_correction_T_min  0.2548
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.205
_refine_ls_extinction_coef       0.00113(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5638
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0451P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                4842
_reflns_number_total             5638
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1858.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2015066
_cod_database_fobs_code          2015066