# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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data_szg195
_database_code_depnum_ccdc_archive 'CCDC 905896'
#TrackingRef 'szg195.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H16 Cl3 N O6 P Pb2'
_chemical_formula_weight         761.91
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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   7.8270(10)
_cell_length_b                   8.2097(11)
_cell_length_c                   13.7455(19)
_cell_angle_alpha                90.374(2)
_cell_angle_beta                 91.578(2)
_cell_angle_gamma                100.994(2)
_cell_volume                     866.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2386
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      28.30
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             686
_exptl_absorpt_coefficient_mu    19.973
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2424
_exptl_absorpt_correction_T_max  0.6566
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      295(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  'Smart Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4895
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3530
_reflns_number_gt                2873
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.0737P)^2^+18.8194P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3530
_refine_ls_number_parameters     157
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1434
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.71234(7) 0.78333(6) 0.89960(4) 0.02627(18) Uani 1 1 d . . .
Pb2 Pb 0.22084(7) 0.69727(7) 1.03947(4) 0.02883(19) Uani 1 1 d . . .
Cl1 Cl 0.5000 1.0000 1.0000 0.0356(12) Uani 1 2 d S . .
Cl2 Cl 1.0000 1.0000 1.0000 0.0368(13) Uani 1 2 d S . .
Cl3 Cl 0.9643(5) 0.5857(5) 0.8543(3) 0.0347(9) Uani 1 1 d . . .
Cl4 Cl 0.2364(7) 0.8716(6) 1.2305(4) 0.0519(11) Uani 1 1 d . . .
P1 P 0.3823(5) 0.4471(4) 0.8815(3) 0.0234(8) Uani 1 1 d . . .
O1 O 0.2651(14) 0.3579(14) 0.9571(8) 0.036(3) Uani 1 1 d . . .
O2 O 0.4016(13) 0.6343(12) 0.8946(8) 0.031(2) Uani 1 1 d . . .
O3 O 0.5562(14) 0.3956(15) 0.8738(8) 0.036(3) Uani 1 1 d . . .
O4 O 0.366(2) -0.3020(19) 0.5854(11) 0.062(4) Uani 1 1 d . . .
O5 O 0.1402(8) -0.2761(7) 0.4911(4) 0.089(6) Uani 1 1 d U . .
H5C H 0.1686 -0.3587 0.4625 0.134 Uiso 1 1 d R . .
O1W O 0.6896(8) 0.7692(7) 0.6733(4) 0.077(5) Uani 1 1 d R . .
H1WA H 0.7542 0.7049 0.6525 0.115 Uiso 1 1 d R . .
H1WB H 0.5849 0.7328 0.6544 0.115 Uiso 1 1 d R . .
H1WC H 0.7236 0.8660 0.6510 0.115 Uiso 1 1 d R . .
N1 N 0.3217(8) 0.2408(7) 0.7194(4) 0.031(3) Uani 1 1 d R . .
H1A H 0.4379 0.2480 0.7223 0.037 Uiso 1 1 d R . .
C1 C 0.2820(8) 0.4022(7) 0.7614(4) 0.040(4) Uani 1 1 d R . .
H1B H 0.3244 0.4921 0.7187 0.048 Uiso 1 1 d R . .
H1C H 0.1582 0.3930 0.7652 0.048 Uiso 1 1 d R . .
C2 C 0.2397(8) 0.0860(7) 0.7739(4) 0.036(4) Uani 1 1 d R . .
H2A H 0.1160 0.0791 0.7754 0.043 Uiso 1 1 d R . .
H2B H 0.2846 0.0930 0.8398 0.043 Uiso 1 1 d R . .
C3 C 0.2781(8) -0.0656(7) 0.7258(4) 0.038(4) Uani 1 1 d R . .
H3B H 0.2274 -0.1615 0.7620 0.046 Uiso 1 1 d R . .
H3C H 0.4018 -0.0597 0.7262 0.046 Uiso 1 1 d R . .
C4 C 0.2059(8) -0.0847(7) 0.6197(4) 0.040(4) Uani 1 1 d R . .
H4A H 0.0825 -0.0884 0.6178 0.048 Uiso 1 1 d R . .
C5 C 0.3019(8) 0.0716(7) 0.5657(4) 0.076(8) Uani 1 1 d R . .
H5A H 0.2638 0.0664 0.4986 0.091 Uiso 1 1 d R . .
H5B H 0.4251 0.0742 0.5683 0.091 Uiso 1 1 d R . .
C6 C 0.2634(8) 0.2282(7) 0.6133(4) 0.068(7) Uani 1 1 d R . .
H6A H 0.3224 0.3237 0.5796 0.082 Uiso 1 1 d R . .
H6B H 0.1406 0.2271 0.6083 0.082 Uiso 1 1 d R . .
C7 C 0.2480(8) -0.2298(7) 0.5658(4) 0.052(5) Uani 1 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 0.0229(3) 0.0199(3) 0.0364(4) 0.0011(2) 0.0033(2) 0.0048(2)
Pb2 0.0229(3) 0.0228(3) 0.0415(4) 0.0018(2) 0.0010(2) 0.0064(2)
Cl1 0.030(3) 0.018(2) 0.060(4) -0.005(2) 0.014(2) 0.0059(19)
Cl2 0.026(3) 0.020(2) 0.062(4) 0.000(2) -0.007(2) -0.0010(19)
Cl3 0.0260(17) 0.0253(18) 0.055(3) -0.0001(17) 0.0094(16) 0.0090(14)
Cl4 0.060(3) 0.039(2) 0.057(3) -0.004(2) 0.012(2) 0.008(2)
P1 0.0226(17) 0.0150(16) 0.033(2) -0.0013(14) -0.0025(15) 0.0052(13)
O1 0.029(6) 0.037(6) 0.037(6) 0.003(5) 0.002(5) -0.005(5)
O2 0.029(5) 0.015(5) 0.047(7) -0.007(4) -0.002(5) -0.001(4)
O3 0.031(6) 0.051(7) 0.031(6) -0.006(5) 0.000(5) 0.017(5)
O4 0.079(11) 0.059(9) 0.057(9) -0.006(7) 0.002(8) 0.033(8)
O5 0.090(6) 0.089(6) 0.089(6) 0.0006(10) 0.0022(10) 0.0174(15)
O1W 0.087(12) 0.056(10) 0.095(13) -0.011(9) -0.003(10) 0.036(9)
N1 0.043(8) 0.022(6) 0.030(7) -0.005(5) 0.006(6) 0.009(5)
C1 0.047(10) 0.028(8) 0.049(11) 0.006(7) 0.003(8) 0.017(7)
C2 0.046(10) 0.029(8) 0.031(9) -0.002(7) 0.008(7) 0.002(7)
C3 0.045(10) 0.025(8) 0.043(10) 0.000(7) -0.002(8) 0.002(7)
C4 0.057(11) 0.033(9) 0.033(9) -0.008(7) -0.007(8) 0.019(8)
C5 0.14(3) 0.038(12) 0.046(13) -0.008(9) 0.022(14) 0.014(14)
C6 0.14(2) 0.047(12) 0.016(9) -0.005(8) -0.018(11) 0.022(13)
C7 0.068(13) 0.042(11) 0.046(11) -0.017(9) -0.014(10) 0.012(10)
_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 O1 2.312(11) 2_667 ?
Pb1 O2 2.504(10) . ?
Pb1 Cl3 2.861(3) . ?
Pb1 Cl2 2.8996(6) . ?
Pb1 Cl1 3.0088(6) . ?
Pb2 O3 2.335(11) 2_667 ?
Pb2 O2 2.580(11) . ?
Pb2 Cl3 2.917(4) 2_667 ?
Pb2 Cl4 2.970(5) . ?
Pb2 Cl1 3.0425(6) . ?
Cl1 Pb1 3.0088(6) 2_677 ?
Cl1 Pb2 3.0425(6) 2_677 ?
Cl2 Pb1 2.8996(6) 2_777 ?
Cl3 Pb2 2.917(4) 2_667 ?
P1 O1 1.505(12) . ?
P1 O3 1.506(11) . ?
P1 O2 1.524(10) . ?
P1 C1 1.814(7) . ?
O1 Pb1 2.312(11) 2_667 ?
O3 Pb2 2.335(10) 2_667 ?
O4 C7 1.212(15) . ?
O5 C7 1.3172 . ?
O5 H5C 0.8500 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O1W H1WC 0.8499 . ?
N1 C6 1.5124 . ?
N1 C2 1.5215 . ?
N1 C1 1.5304 . ?
N1 H1A 0.9000 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.4899 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C3 C4 1.5452 . ?
C3 H3B 0.9599 . ?
C3 H3C 0.9600 . ?
C4 C7 1.4923 . ?
C4 C5 1.5614 . ?
C4 H4A 0.9600 . ?
C5 C6 1.5230 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9599 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
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
O1 Pb1 O2 85.0(4) 2_667 . ?
O1 Pb1 Cl3 77.7(3) 2_667 . ?
O2 Pb1 Cl3 115.7(2) . . ?
O1 Pb1 Cl2 78.4(3) 2_667 . ?
O2 Pb1 Cl2 150.0(3) . . ?
Cl3 Pb1 Cl2 85.10(8) . . ?
O1 Pb1 Cl1 90.0(3) 2_667 . ?
O2 Pb1 Cl1 72.2(2) . . ?
Cl3 Pb1 Cl1 164.34(9) . . ?
Cl2 Pb1 Cl1 82.939(17) . . ?
O3 Pb2 O2 81.3(4) 2_667 . ?
O3 Pb2 Cl3 76.9(3) 2_667 2_667 ?
O2 Pb2 Cl3 117.2(2) . 2_667 ?
O3 Pb2 Cl4 76.1(3) 2_667 . ?
O2 Pb2 Cl4 144.5(2) . . ?
Cl3 Pb2 Cl4 83.99(13) 2_667 . ?
O3 Pb2 Cl1 84.4(3) 2_667 . ?
O2 Pb2 Cl1 70.6(2) . . ?
Cl3 Pb2 Cl1 157.85(9) 2_667 . ?
Cl4 Pb2 Cl1 80.11(10) . . ?
Pb1 Cl1 Pb1 180.000(1) 2_677 . ?
Pb1 Cl1 Pb2 90.229(17) 2_677 2_677 ?
Pb1 Cl1 Pb2 89.771(17) . 2_677 ?
Pb1 Cl1 Pb2 89.771(17) 2_677 . ?
Pb1 Cl1 Pb2 90.229(17) . . ?
Pb2 Cl1 Pb2 180.0 2_677 . ?
Pb1 Cl2 Pb1 180.000(1) 2_777 . ?
Pb1 Cl3 Pb2 92.25(11) . 2_667 ?
O1 P1 O3 115.4(7) . . ?
O1 P1 O2 110.3(7) . . ?
O3 P1 O2 111.9(6) . . ?
O1 P1 C1 109.8(5) . . ?
O3 P1 C1 103.8(5) . . ?
O2 P1 C1 105.0(5) . . ?
P1 O1 Pb1 138.8(7) . 2_667 ?
P1 O2 Pb1 113.1(5) . . ?
P1 O2 Pb2 109.6(6) . . ?
Pb1 O2 Pb2 115.0(4) . . ?
P1 O3 Pb2 144.8(7) . 2_667 ?
C7 O5 H5C 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?
H1WA O1W H1WC 109.5 . . ?
H1WB O1W H1WC 109.5 . . ?
C6 N1 C2 110.8 . . ?
C6 N1 C1 108.1 . . ?
C2 N1 C1 114.1 . . ?
C6 N1 H1A 107.9 . . ?
C2 N1 H1A 107.9 . . ?
C1 N1 H1A 107.9 . . ?
N1 C1 P1 111.3(2) . . ?
N1 C1 H1B 109.4 . . ?
P1 C1 H1B 109.4 . . ?
N1 C1 H1C 109.4 . . ?
P1 C1 H1C 109.4 . . ?
H1B C1 H1C 108.0 . . ?
C3 C2 N1 110.6 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 111.8 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3C 109.3 . . ?
C4 C3 H3C 109.3 . . ?
H3B C3 H3C 107.9 . . ?
C7 C4 C3 114.4 . . ?
C7 C4 C5 105.4 . . ?
C3 C4 C5 105.5 . . ?
C7 C4 H4A 110.4 . . ?
C3 C4 H4A 110.4 . . ?
C5 C4 H4A 110.4 . . ?
C6 C5 C4 109.9 . . ?
C6 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N1 C6 C5 111.3 . . ?
N1 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N1 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
O4 C7 O5 121.2(8) . . ?
O4 C7 C4 126.4(8) . . ?
O5 C7 C4 112.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl4 0.90 2.96 3.792(8) 154.7 2_667
O1W H1WC Cl4 0.85 2.66 3.168(7) 119.9 2_677
O1W H1WB O4 0.85 1.91 2.737(17) 163.9 1_565
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         5.734
_refine_diff_density_min         -2.212
_refine_diff_density_rms         0.385


data_szg196
_database_code_depnum_ccdc_archive 'CCDC 905897'
#TrackingRef 'szg196.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H16 N O11 P Pb2'
_chemical_formula_weight         843.65
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'
P P 0.1023 0.0942 '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           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   6.7505(13)
_cell_length_b                   9.3424(19)
_cell_length_c                   16.747(3)
_cell_angle_alpha                102.497(3)
_cell_angle_beta                 92.402(3)
_cell_angle_gamma                99.285(2)
_cell_volume                     1014.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1052
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      23.72
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    16.716
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3670
_exptl_absorpt_correction_T_max  0.7204
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      295(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  'Smart Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5425
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4057
_reflns_number_gt                2629
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.1053P)^2^+3.3128P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4057
_refine_ls_number_parameters     229
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.1934
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
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
Pb1 Pb -0.28077(12) 0.17898(8) 0.27598(4) 0.0242(2) Uani 1 1 d . . .
Pb2 Pb 0.28254(12) 0.07044(8) 0.09845(4) 0.0259(3) Uani 1 1 d . . .
P1 P -0.1985(8) 0.2060(6) 0.0810(3) 0.0235(11) Uani 1 1 d . . .
O1 O -0.331(2) 0.2505(16) 0.1523(8) 0.028(3) Uani 1 1 d . . .
O2 O -0.074(2) 0.0918(15) 0.0999(9) 0.038(4) Uani 1 1 d . . .
O3 O -0.318(2) 0.1555(18) 0.0000(8) 0.040(4) Uani 1 1 d . . .
O4 O 0.142(3) 0.8916(18) 0.1709(9) 0.043(4) Uani 1 1 d . . .
O5 O 0.478(2) 0.9250(16) 0.1815(9) 0.035(4) Uani 1 1 d . . .
O6 O 0.100(2) 0.3177(16) 0.2751(8) 0.030(3) Uani 1 1 d . . .
O7 O 0.355(2) 0.1901(14) 0.2624(8) 0.025(3) Uani 1 1 d U . .
O8 O 0.254(3) 0.6707(17) 0.5644(9) 0.040(4) Uani 1 1 d . . .
O9 O 0.292(2) 0.5627(16) 0.6671(9) 0.035(4) Uani 1 1 d . . .
O10 O 0.290(3) 0.0246(18) 0.6156(9) 0.061(6) Uani 1 1 d . . .
O11 O 0.2561(7) -0.1100(5) 0.4851(3) 0.039(4) Uani 1 1 d . . .
H11B H 0.2626 -0.1809 0.5090 0.059 Uiso 1 1 d R . .
N1 N 0.0893(7) 0.4635(5) 0.1497(3) 0.025(4) Uani 1 1 d R . .
H1C H 0.1017 0.4026 0.1838 0.030 Uiso 1 1 d R . .
C1 C -0.0270(7) 0.3730(5) 0.0715(3) 0.032(5) Uani 1 1 d R . .
H1A H -0.1037 0.4357 0.0495 0.039 Uiso 1 1 d R . .
H1B H 0.0674 0.3437 0.0325 0.039 Uiso 1 1 d R . .
C2 C 0.2985(7) 0.5306(5) 0.1323(3) 0.027(5) Uani 1 1 d R . .
H2A H 0.2882 0.5920 0.0937 0.032 Uiso 1 1 d R . .
H2B H 0.3690 0.4524 0.1083 0.032 Uiso 1 1 d R . .
C3 C 0.4163(7) 0.6239(5) 0.2112(3) 0.045(7) Uani 1 1 d R . .
H3B H 0.5470 0.6672 0.1989 0.054 Uiso 1 1 d R . .
H3C H 0.4346 0.5608 0.2482 0.054 Uiso 1 1 d R . .
C4 C 0.3050(7) 0.7492(5) 0.2532(3) 0.041(6) Uani 1 1 d R . .
H4A H 0.3750 0.7981 0.3055 0.049 Uiso 1 1 d R . .
C5 C 0.0885(7) 0.6802(5) 0.2667(3) 0.028(5) Uani 1 1 d R . .
H5A H 0.0166 0.7592 0.2879 0.033 Uiso 1 1 d R . .
H5B H 0.0951 0.6226 0.3075 0.033 Uiso 1 1 d R . .
C6 C -0.0281(7) 0.5821(5) 0.1903(3) 0.027(5) Uani 1 1 d R . .
H6A H -0.1549 0.5349 0.2043 0.033 Uiso 1 1 d R . .
H6B H -0.0548 0.6419 0.1525 0.033 Uiso 1 1 d R . .
C7 C 0.3073(7) 0.8624(5) 0.1992(3) 0.034(5) Uani 1 1 d R . .
C8 C 0.2404(7) 0.2669(5) 0.3924(3) 0.017(4) Uani 1 1 d RU . .
C9 C 0.2386(7) 0.3996(5) 0.4463(3) 0.020(4) Uani 1 1 d RU . .
H9A H 0.2234 0.4861 0.4261 0.024 Uiso 1 1 d R . .
C10 C 0.2593(7) 0.4097(5) 0.5329(3) 0.021(4) Uani 1 1 d RU . .
C11 C 0.2728(7) 0.2856(5) 0.5611(3) 0.026(5) Uani 1 1 d R . .
H11A H 0.2885 0.2927 0.6192 0.031 Uiso 1 1 d R . .
C12 C 0.2641(7) 0.1468(5) 0.5065(3) 0.029(5) Uani 1 1 d R . .
C13 C 0.2594(7) 0.1417(5) 0.4231(3) 0.024(5) Uani 1 1 d R . .
H13A H 0.2695 0.0501 0.3855 0.029 Uiso 1 1 d R . .
C14 C 0.2333(7) 0.2540(5) 0.2991(3) 0.032(5) Uani 1 1 d RU . .
C15 C 0.2699(7) 0.5581(5) 0.5897(3) 0.021(4) Uani 1 1 d RU . .
C16 C 0.2728(7) 0.0141(5) 0.5396(3) 0.029(5) Uani 1 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 0.0283(5) 0.0258(4) 0.0157(4) 0.0017(3) -0.0006(3) 0.0015(3)
Pb2 0.0245(5) 0.0305(4) 0.0209(4) 0.0047(3) -0.0012(3) 0.0021(3)
P1 0.026(3) 0.029(3) 0.014(2) 0.003(2) 0.004(2) 0.002(2)
O1 0.026(8) 0.040(8) 0.013(7) 0.006(6) 0.005(6) -0.008(6)
O2 0.052(11) 0.021(7) 0.037(9) 0.005(6) -0.007(8) 0.000(7)
O3 0.039(10) 0.057(10) 0.012(7) -0.010(7) -0.011(7) 0.003(8)
O4 0.050(11) 0.050(10) 0.029(9) 0.016(8) 0.007(8) -0.003(8)
O5 0.042(10) 0.036(8) 0.020(8) -0.001(6) 0.002(7) -0.004(7)
O6 0.026(8) 0.045(9) 0.020(7) 0.014(6) -0.008(6) 0.001(7)
O7 0.025(3) 0.025(3) 0.025(3) 0.0050(12) 0.0022(10) 0.0043(11)
O8 0.063(12) 0.037(9) 0.023(8) 0.014(7) 0.006(8) 0.011(8)
O9 0.047(10) 0.037(8) 0.022(8) 0.013(6) 0.001(7) 0.005(7)
O10 0.128(19) 0.043(10) 0.011(8) 0.010(7) -0.005(9) 0.011(11)
O11 0.065(12) 0.029(8) 0.019(8) 0.002(6) -0.007(7) 0.001(8)
N1 0.038(11) 0.020(8) 0.008(7) -0.003(6) -0.003(7) -0.009(7)
C1 0.043(14) 0.038(11) 0.014(10) 0.009(9) 0.005(9) -0.002(10)
C2 0.026(12) 0.025(10) 0.031(12) 0.005(9) 0.005(9) 0.009(9)
C3 0.045(16) 0.027(11) 0.058(17) 0.014(11) -0.026(13) -0.008(11)
C4 0.060(18) 0.034(12) 0.029(13) 0.007(10) -0.008(12) 0.015(12)
C5 0.037(13) 0.016(9) 0.026(11) 0.004(8) 0.000(10) -0.003(9)
C6 0.030(12) 0.031(10) 0.021(10) 0.010(9) -0.002(9) 0.000(9)
C7 0.049(16) 0.039(12) 0.010(10) -0.007(9) 0.006(10) 0.012(12)
C8 0.017(4) 0.017(4) 0.017(4) 0.0040(13) 0.0013(11) 0.0030(12)
C9 0.020(4) 0.020(4) 0.020(4) 0.0045(13) 0.0014(11) 0.0034(12)
C10 0.021(4) 0.021(4) 0.021(4) 0.0050(13) 0.0016(11) 0.0035(12)
C11 0.038(13) 0.029(10) 0.012(9) 0.003(8) -0.001(9) 0.008(9)
C12 0.029(12) 0.042(12) 0.029(11) 0.027(10) 0.012(10) 0.017(10)
C13 0.034(12) 0.010(8) 0.026(11) -0.003(7) -0.011(9) 0.007(8)
C14 0.032(5) 0.032(5) 0.032(5) 0.0074(15) 0.0024(11) 0.0056(13)
C15 0.021(4) 0.022(4) 0.021(4) 0.0050(14) 0.0019(11) 0.0036(12)
C16 0.047(15) 0.024(10) 0.018(10) 0.011(8) -0.007(10) 0.002(10)
_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 O1 2.339(13) . ?
Pb1 O9 2.410(15) 2_566 ?
Pb1 O7 2.481(13) 1_455 ?
Pb1 O6 2.688(14) . ?
Pb1 O8 2.721(15) 2_566 ?
Pb2 O4 2.373(15) 1_545 ?
Pb2 O3 2.434(15) 2 ?
Pb2 O2 2.451(16) . ?
Pb2 O5 2.599(16) 1_545 ?
Pb2 O7 2.722(13) . ?
Pb2 C7 2.854(5) 1_545 ?
P1 O3 1.491(14) . ?
P1 O2 1.533(16) . ?
P1 O1 1.548(13) . ?
P1 C1 1.828(7) . ?
O3 Pb2 2.434(15) 2 ?
O4 C7 1.287(18) . ?
O4 Pb2 2.373(15) 1_565 ?
O5 C7 1.280(16) . ?
O5 Pb2 2.599(16) 1_565 ?
O6 C14 1.254(15) . ?
O7 C14 1.204(14) . ?
O7 Pb1 2.481(13) 1_655 ?
O8 C15 1.234(15) . ?
O8 Pb1 2.721(15) 2_566 ?
O9 C15 1.290(14) . ?
O9 Pb1 2.410(15) 2_566 ?
O10 C16 1.254(15) . ?
O11 C16 1.2968 . ?
O11 H11B 0.8501 . ?
N1 C1 1.5052 . ?
N1 C2 1.5167 . ?
N1 C6 1.5235 . ?
N1 H1C 0.8999 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C2 C3 1.5263 . ?
C2 H2A 0.9601 . ?
C2 H2B 0.9600 . ?
C3 C4 1.5499 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9601 . ?
C4 C7 1.5328 . ?
C4 C5 1.5456 . ?
C4 H4A 0.9599 . ?
C5 C6 1.5073 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C6 H6A 0.9599 . ?
C6 H6B 0.9600 . ?
C7 Pb2 2.854(5) 1_565 ?
C8 C9 1.3685 . ?
C8 C13 1.3972 . ?
C8 C14 1.5388 . ?
C9 C10 1.4319 . ?
C9 H9A 0.9600 . ?
C10 C11 1.3572 . ?
C10 C15 1.4911 . ?
C11 C12 1.4074 . ?
C11 H11A 0.9600 . ?
C12 C13 1.3867 . ?
C12 C16 1.4711 . ?
C13 H13A 0.9600 . ?
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
O1 Pb1 O9 82.3(5) . 2_566 ?
O1 Pb1 O7 74.9(5) . 1_455 ?
O9 Pb1 O7 76.7(5) 2_566 1_455 ?
O1 Pb1 O6 84.3(4) . . ?
O9 Pb1 O6 75.9(5) 2_566 . ?
O7 Pb1 O6 147.5(4) 1_455 . ?
O1 Pb1 O8 132.6(5) . 2_566 ?
O9 Pb1 O8 50.3(4) 2_566 2_566 ?
O7 Pb1 O8 90.6(5) 1_455 2_566 ?
O6 Pb1 O8 85.4(5) . 2_566 ?
O4 Pb2 O3 80.8(6) 1_545 2 ?
O4 Pb2 O2 75.6(6) 1_545 . ?
O3 Pb2 O2 109.1(5) 2 . ?
O4 Pb2 O5 53.1(5) 1_545 1_545 ?
O3 Pb2 O5 75.1(5) 2 1_545 ?
O2 Pb2 O5 127.7(5) . 1_545 ?
O4 Pb2 O7 71.2(5) 1_545 . ?
O3 Pb2 O7 138.8(5) 2 . ?
O2 Pb2 O7 92.7(5) . . ?
O5 Pb2 O7 64.0(4) 1_545 . ?
O4 Pb2 C7 26.5(4) 1_545 1_545 ?
O3 Pb2 C7 77.0(4) 2 1_545 ?
O2 Pb2 C7 101.6(4) . 1_545 ?
O5 Pb2 C7 26.6(3) 1_545 1_545 ?
O7 Pb2 C7 64.4(3) . 1_545 ?
O3 P1 O2 113.2(9) . . ?
O3 P1 O1 112.1(9) . . ?
O2 P1 O1 110.0(9) . . ?
O3 P1 C1 104.0(7) . . ?
O2 P1 C1 109.0(7) . . ?
O1 P1 C1 108.2(6) . . ?
P1 O1 Pb1 120.0(8) . . ?
P1 O2 Pb2 134.7(9) . . ?
P1 O3 Pb2 122.5(9) . 2 ?
C7 O4 Pb2 98.1(9) . 1_565 ?
C7 O5 Pb2 87.9(8) . 1_565 ?
C14 O6 Pb1 115.2(8) . . ?
C14 O7 Pb1 139.3(9) . 1_655 ?
C14 O7 Pb2 119.9(9) . . ?
Pb1 O7 Pb2 98.5(4) 1_655 . ?
C15 O8 Pb1 87.5(8) . 2_566 ?
C15 O9 Pb1 100.8(8) . 2_566 ?
C16 O11 H11B 109.5 . . ?
C1 N1 C2 110.3 . . ?
C1 N1 C6 109.3 . . ?
C2 N1 C6 112.1 . . ?
C1 N1 H1C 108.4 . . ?
C2 N1 H1C 108.4 . . ?
C6 N1 H1C 108.4 . . ?
N1 C1 P1 115.7(2) . . ?
N1 C1 H1A 108.3 . . ?
P1 C1 H1A 108.4 . . ?
N1 C1 H1B 108.3 . . ?
P1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.4 . . ?
N1 C2 C3 110.5 . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 111.3 . . ?
C2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C2 C3 H3C 109.4 . . ?
C4 C3 H3C 109.4 . . ?
H3B C3 H3C 108.0 . . ?
C7 C4 C5 112.1 . . ?
C7 C4 C3 108.5 . . ?
C5 C4 C3 109.3 . . ?
C7 C4 H4A 108.9 . . ?
C5 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C6 C5 C4 114.0 . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 N1 110.9 . . ?
C5 C6 H6A 109.5 . . ?
N1 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
O5 C7 O4 120.8(10) . . ?
O5 C7 C4 118.4(7) . . ?
O4 C7 C4 120.7(7) . . ?
O5 C7 Pb2 65.5(7) . 1_565 ?
O4 C7 Pb2 55.4(7) . 1_565 ?
C4 C7 Pb2 176.11(9) . 1_565 ?
C9 C8 C13 119.1 . . ?
C9 C8 C14 121.7 . . ?
C13 C8 C14 119.1 . . ?
C8 C9 C10 120.2 . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C11 C10 C9 119.6 . . ?
C11 C10 C15 121.8 . . ?
C9 C10 C15 118.6 . . ?
C10 C11 C12 120.9 . . ?
C10 C11 H11A 119.5 . . ?
C12 C11 H11A 119.5 . . ?
C13 C12 C11 118.4 . . ?
C13 C12 C16 122.2 . . ?
C11 C12 C16 119.2 . . ?
C12 C13 C8 121.5 . . ?
C12 C13 H13A 119.3 . . ?
C8 C13 H13A 119.3 . . ?
O7 C14 O6 131.2(10) . . ?
O7 C14 C8 116.9(7) . . ?
O6 C14 C8 111.9(7) . . ?
O8 C15 O9 121.3(10) . . ?
O8 C15 C10 122.1(7) . . ?
O9 C15 C10 116.6(7) . . ?
O10 C16 O11 124.2(8) . . ?
O10 C16 C12 120.5(8) . . ?
O11 C16 C12 115.2 . . ?
_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         6.930
_refine_diff_density_min         -2.830
_refine_diff_density_rms         0.425