#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/28/8102816.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_8102816
loop_
_publ_author_name
'Hu Zang'
'Li-Ying Han'
'Da-Jun Sun'
_publ_section_title
;
 Crystal structure of
 {2-(4-fluorophenyl)-1H-imidazo[4,5-f]-(1,10-phenanthroline)}-(1,4-benzenedicarboxylato)lead(II)
 trihydrate, Pb(C19H11FN4)(C8H4O4) · 3H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              601
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C27 H21 F N4 O7 Pb'
_chemical_formula_sum            'C27 H21 F N4 O7 Pb'
_chemical_formula_weight         739.67
_chemical_name_systematic
;
poly-[1,4-benzenedicarboxylato-lead(II)-
[11-fluoro-dipyrido[3,2-a:2',3'-c]phenazine]]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.6520(10)
_cell_angle_beta                 107.9730(10)
_cell_angle_gamma                104.6670(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5757(6)
_cell_length_b                   10.6964(7)
_cell_length_c                   13.2466(8)
_cell_measurement_reflns_used    4719
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.64
_cell_volume                     1233.61(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       'φ and 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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6923
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.903
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0267
_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)+(0.0443P)²+1.2894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                4466
_reflns_number_total             4719
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            1267-3138.cff
_cod_data_source_block           1
_cod_database_code               8102816
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5951(5) 0.6271(4) 0.8181(4) 0.0304(9) Uani 1 1 d . . .
H1 H 0.5187 0.6376 0.8445 0.036 Uiso 1 1 calc R . .
C2 C 0.6916(6) 0.7387(5) 0.7982(4) 0.0347(10) Uani 1 1 d . . .
H2 H 0.6791 0.8209 0.8117 0.042 Uiso 1 1 calc R . .
C3 C 0.8028(5) 0.7249(4) 0.7590(4) 0.0324(10) Uani 1 1 d . . .
H3 H 0.8673 0.7976 0.7453 0.039 Uiso 1 1 calc R . .
C4 C 0.8200(5) 0.5995(4) 0.7393(3) 0.0252(9) Uani 1 1 d . . .
C5 C 0.7200(5) 0.4919(4) 0.7628(3) 0.0233(8) Uani 1 1 d . . .
C6 C 0.7388(5) 0.3610(4) 0.7484(3) 0.0233(8) Uani 1 1 d . . .
C7 C 0.8558(5) 0.3395(4) 0.7124(3) 0.0245(8) Uani 1 1 d . . .
C8 C 0.8674(5) 0.2111(4) 0.7011(4) 0.0329(10) Uani 1 1 d . . .
H8 H 0.9419 0.1929 0.6761 0.039 Uiso 1 1 calc R . .
C9 C 0.7684(6) 0.1140(5) 0.7274(5) 0.0428(13) Uani 1 1 d . . .
H9 H 0.7754 0.0289 0.7216 0.051 Uiso 1 1 calc R . .
C10 C 0.6555(6) 0.1440(5) 0.7633(4) 0.0376(11) Uani 1 1 d . . .
H10 H 0.5881 0.0767 0.7806 0.045 Uiso 1 1 calc R . .
C11 C 0.9545(5) 0.4511(4) 0.6904(3) 0.0237(8) Uani 1 1 d . . .
C12 C 0.9371(5) 0.5738(4) 0.7028(3) 0.0240(8) Uani 1 1 d . . .
C13 C 1.2575(5) 0.6526(4) 0.6110(3) 0.0254(9) Uani 1 1 d . . .
C14 C 1.3272(5) 0.5786(4) 0.5624(4) 0.0326(10) Uani 1 1 d . . .
H14 H 1.3003 0.4882 0.5592 0.039 Uiso 1 1 calc R . .
C15 C 1.4366(6) 0.6396(5) 0.5188(4) 0.0393(11) Uani 1 1 d . . .
H15 H 1.4808 0.5908 0.4841 0.047 Uiso 1 1 calc R . .
C16 C 1.4778(5) 0.7730(5) 0.5280(4) 0.0342(10) Uani 1 1 d . . .
C17 C 1.4134(6) 0.8491(5) 0.5746(4) 0.0382(11) Uani 1 1 d . . .
H17 H 1.4422 0.9395 0.5778 0.046 Uiso 1 1 calc R . .
C18 C 1.3024(6) 0.7871(5) 0.6175(4) 0.0397(11) Uani 1 1 d . . .
H18 H 1.2581 0.8373 0.6509 0.048 Uiso 1 1 calc R . .
C19 C 1.1307(5) 0.5936(4) 0.6491(3) 0.0265(9) Uani 1 1 d . . .
C20 C 0.2384(5) 0.1646(4) 0.6865(3) 0.0229(8) Uani 1 1 d . . .
C21 C 0.1137(5) 0.0805(4) 0.5898(3) 0.0221(8) Uani 1 1 d . . .
C22 C 0.0789(5) 0.1250(4) 0.4910(3) 0.0247(9) Uani 1 1 d . . .
H22 H 0.1309 0.2088 0.4850 0.030 Uiso 1 1 calc R . .
C23 C -0.0329(5) 0.0444(4) 0.4020(3) 0.0256(9) Uani 1 1 d . . .
H23 H -0.0546 0.0737 0.3358 0.031 Uiso 1 1 calc R . .
C24 C 0.2161(5) 0.4075(5) 0.9254(3) 0.0280(9) Uani 1 1 d . . .
C25 C -0.0083(5) 0.3680(4) 0.9927(3) 0.0276(9) Uani 1 1 d . . .
H25 H -0.0139 0.2796 0.9877 0.033 Uiso 1 1 calc R . .
C26 C 0.1036(5) 0.4554(4) 0.9634(3) 0.0255(9) Uani 1 1 d . . .
C27 C 0.1100(5) 0.5874(4) 0.9711(3) 0.0275(9) Uani 1 1 d . . .
H27 H 0.1836 0.6459 0.9517 0.033 Uiso 1 1 calc R . .
N1 N 0.6404(4) 0.2636(3) 0.7737(3) 0.0279(8) Uani 1 1 d . . .
N2 N 0.6080(4) 0.5073(3) 0.8010(3) 0.0248(7) Uani 1 1 d . . .
N3 N 1.0481(4) 0.6638(3) 0.6777(3) 0.0282(8) Uani 1 1 d . . .
N4 N 1.0792(4) 0.4638(3) 0.6562(3) 0.0253(7) Uani 1 1 d . . .
H4 H 1.1169 0.4026 0.6422 0.030 Uiso 1 1 calc R . .
O1 O 0.2737(3) 0.2883(3) 0.6935(2) 0.0268(6) Uani 1 1 d . . .
O2 O 0.3060(4) 0.1084(3) 0.7602(2) 0.0306(7) Uani 1 1 d . . .
O1W O 0.4828(9) 0.1445(7) 1.0311(6) 0.116(2) Uani 1 1 d . . .
O3 O 0.3279(4) 0.4917(3) 0.9142(3) 0.0334(7) Uani 1 1 d . . .
O2W O 0.0616(11) 0.0257(6) 0.9199(8) 0.139(3) Uani 1 1 d . . .
O4 O 0.1982(4) 0.2867(3) 0.9077(3) 0.0380(8) Uani 1 1 d . . .
O3W O 0.2405(7) -0.1132(6) 0.8638(6) 0.0975(19) Uani 1 1 d . . .
F1 F 1.5845(4) 0.8316(3) 0.4850(3) 0.0525(8) Uani 1 1 d . . .
Pb1 Pb 0.465313(16) 0.322577(14) 0.882039(11) 0.02392(7) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 123.1(4) . . ?
N2 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 118.0(4) . . ?
C3 C4 C12 124.6(4) . . ?
C5 C4 C12 117.3(4) . . ?
N2 C5 C4 121.6(4) . . ?
N2 C5 C6 118.6(4) . . ?
C4 C5 C6 119.8(4) . . ?
N1 C6 C7 122.2(4) . . ?
N1 C6 C5 116.5(4) . . ?
C7 C6 C5 121.3(4) . . ?
C8 C7 C6 118.0(4) . . ?
C8 C7 C11 125.0(4) . . ?
C6 C7 C11 116.9(4) . . ?
C9 C8 C7 119.2(4) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 119.1(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N1 C10 C9 123.2(4) . . ?
N1 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C12 C11 N4 106.3(4) . . ?
C12 C11 C7 122.3(4) . . ?
N4 C11 C7 131.4(4) . . ?
C11 C12 N3 110.6(4) . . ?
C11 C12 C4 122.4(4) . . ?
N3 C12 C4 126.9(4) . . ?
C18 C13 C14 118.8(4) . . ?
C18 C13 C19 118.0(4) . . ?
C14 C13 C19 123.0(4) . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 118.5(4) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
F1 C16 C17 118.6(4) . . ?
F1 C16 C15 118.0(4) . . ?
C17 C16 C15 123.3(4) . . ?
C16 C17 C18 117.9(4) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
C13 C18 C17 121.1(4) . . ?
C13 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
N3 C19 N4 112.2(4) . . ?
N3 C19 C13 122.0(4) . . ?
N4 C19 C13 125.8(4) . . ?
O1 C20 O2 121.8(4) . . ?
O1 C20 C21 120.1(4) . . ?
O2 C20 C21 118.1(4) . . ?
C22 C21 C23 119.5(4) . 2_556 ?
C22 C21 C20 120.7(4) . . ?
C23 C21 C20 119.8(4) 2_556 . ?
C23 C22 C21 119.8(4) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C21 120.7(4) . 2_556 ?
C22 C23 H23 119.7 . . ?
C21 C23 H23 119.7 2_556 . ?
O4 C24 O3 122.3(4) . . ?
O4 C24 C26 119.4(4) . . ?
O3 C24 C26 118.2(4) . . ?
C27 C25 C26 120.2(4) 2_567 . ?
C27 C25 H25 119.9 2_567 . ?
C26 C25 H25 119.9 . . ?
C27 C26 C25 119.1(4) . . ?
C27 C26 C24 120.4(4) . . ?
C25 C26 C24 120.4(4) . . ?
C25 C27 C26 120.7(4) 2_567 . ?
C25 C27 H27 119.7 2_567 . ?
C26 C27 H27 119.7 . . ?
C10 N1 C6 118.2(4) . . ?
C10 N1 Pb1 121.0(3) . . ?
C6 N1 Pb1 119.5(3) . . ?
C1 N2 C5 118.5(4) . . ?
C1 N2 Pb1 118.8(3) . . ?
C5 N2 Pb1 121.2(3) . . ?
C19 N3 C12 104.6(3) . . ?
C19 N4 C11 106.2(3) . . ?
C19 N4 H4 126.9 . . ?
C11 N4 H4 126.9 . . ?
C20 O1 Pb1 93.0(2) . . ?
C20 O2 Pb1 93.2(2) . . ?
C24 O3 Pb1 94.3(3) . . ?
C24 O4 Pb1 92.5(3) . . ?
O2 Pb1 O1 51.89(10) . . ?
O2 Pb1 O3 118.32(10) . . ?
O1 Pb1 O3 81.85(10) . . ?
O2 Pb1 N2 118.14(11) . . ?
O1 Pb1 N2 79.26(10) . . ?
O3 Pb1 N2 83.08(10) . . ?
O2 Pb1 O4 76.98(10) . . ?
O1 Pb1 O4 74.86(11) . . ?
O3 Pb1 O4 50.35(10) . . ?
N2 Pb1 O4 128.87(11) . . ?
O2 Pb1 N1 74.47(11) . . ?
O1 Pb1 N1 82.01(11) . . ?
O3 Pb1 N1 143.66(11) . . ?
N2 Pb1 N1 62.00(11) . . ?
O4 Pb1 N1 150.57(11) . . ?
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
C1 N2 1.330(6) . ?
C1 C2 1.407(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.355(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.410(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.419(6) . ?
C4 C12 1.428(6) . ?
C5 N2 1.358(5) . ?
C5 C6 1.464(6) . ?
C6 N1 1.352(5) . ?
C6 C7 1.408(6) . ?
C7 C8 1.408(6) . ?
C7 C11 1.430(6) . ?
C8 C9 1.359(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.404(7) . ?
C9 H9 0.9300 . ?
C10 N1 1.327(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.370(6) . ?
C11 N4 1.382(5) . ?
C12 N3 1.382(5) . ?
C13 C18 1.383(6) . ?
C13 C14 1.398(6) . ?
C13 C19 1.468(6) . ?
C14 C15 1.390(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.367(7) . ?
C15 H15 0.9300 . ?
C16 F1 1.358(5) . ?
C16 C17 1.359(7) . ?
C17 C18 1.398(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 N3 1.335(6) . ?
C19 N4 1.370(5) . ?
C20 O1 1.269(5) . ?
C20 O2 1.271(5) . ?
C20 C21 1.497(5) . ?
C21 C22 1.393(6) . ?
C21 C23 1.394(6) 2_556 ?
C22 C23 1.380(6) . ?
C22 H22 0.9300 . ?
C23 C21 1.394(6) 2_556 ?
C23 H23 0.9300 . ?
C24 O4 1.257(6) . ?
C24 O3 1.267(5) . ?
C24 C26 1.502(6) . ?
C25 C27 1.378(6) 2_567 ?
C25 C26 1.402(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.393(6) . ?
C27 C25 1.378(6) 2_567 ?
C27 H27 0.9300 . ?
N1 Pb1 2.678(4) . ?
N2 Pb1 2.594(3) . ?
N4 H4 0.8600 . ?
O1 Pb1 2.540(3) . ?
O2 Pb1 2.534(3) . ?
O3 Pb1 2.577(3) . ?
O4 Pb1 2.619(3) . ?
