# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2002

data_329 
_database_code_CSD                  189047

_journal_coden_Cambridge      440
_journal_volume           ?
_journal_year             ? 
_journal_page_first       ?

_publ_requested_journal       'New Journal of Chemistry'

loop_
_publ_author_name
'Chen, Xuetai'
'Li, Yi-Zhi'
'Shi, Yu-Jun'
'Xue, Ziling'
'You, Xiao-Zeng'

_publ_contact_author_name     	'Dr Xuetai Chen'  
_publ_contact_author_address 
;
College of Chemistry and Chemical Engineering
Coordination Chemistry Institute
Hankou Road 22
Nanjing
Jiangsu
210093
CHINA
;

_publ_contact_author_email       'XTCHEN@NETRA.NJU.EDU.CN'

_publ_section_title
;
Pb(dca)2 (dca = dicyanamide): a novel 3D compound with three
unprecedented coordination modes of dicyanamide
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety         'C4 N6 Pb'  
_chemical_formula_sum            'C4 N6 Pb' 
_chemical_formula_weight          339.29 

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' 
'N'  'N'   0.0061   0.0033 
'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           'Orthorhombic'
_symmetry_space_group_name_H-M   'Pnma'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x+1/2, -y, z+1/2' 
'x+1/2, -y+1/2, -z+1/2' 
'-x, y+1/2, -z' 
'-x, -y, -z' 
'x-1/2, y, -z-1/2' 
'-x-1/2, y-1/2, z-1/2' 
'x, -y-1/2, z' 

_cell_length_a                    13.501(2) 
_cell_length_b                    3.995(1) 
_cell_length_c                    11.980(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      646.2(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       2.2 
_cell_measurement_theta_max       25.0 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.11
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.488 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              592 
_exptl_absorpt_coefficient_mu     26.039 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.044
_exptl_absorpt_correction_T_max   0.075
_exptl_absorpt_process_details    'Bruker SADABS' 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  'graphite'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.001 
_diffrn_reflns_number             657 
_diffrn_reflns_av_R_equivalents   0.0221
_diffrn_reflns_av_sigmaI/netI     0.0227 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        4 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.27 
_diffrn_reflns_theta_max          24.97 
_reflns_number_total              657 
_reflns_number_gt                 537 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection      'Bruker XSCANS'
_computing_cell_refinement      'Bruker XSCANS'
_computing_data_reduction       'Bruker SHELXTL'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_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^)+(0.1180P)^2^+1.9900P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          657 
_refine_ls_number_parameters      68 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0478 
_refine_ls_R_factor_gt            0.0380 
_refine_ls_wR_factor_ref          0.1366 
_refine_ls_wR_factor_gt           0.1240 
_refine_ls_goodness_of_fit_ref    1.002 
_refine_ls_restrained_S_all       1.002 
_refine_ls_shift/su_max           0.000 
_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 0.71407(5) 1.2500 0.38005(5) 0.0177(4) Uani 1 2 d S . . 
N1 N 1.0669(15) 0.7500 0.1109(12) 0.026(4) Uani 1 2 d S . . 
N2 N 0.8864(12) 0.7500 0.0866(14) 0.026(4) Uani 1 2 d S . . 
N3 N 0.7644(12) 0.7500 0.2478(14) 0.026(4) Uani 1 2 d S . . 
N5 N 1.0927(11) 1.2500 0.3433(14) 0.026(4) Uani 1 2 d S . . 
N4 N 0.9097(12) 1.2500 0.3573(14) 0.026(4) Uani 1 2 d S . . 
N6 N 0.7824(10) 0.7500 0.5051(15) 0.026(4) Uani 1 2 d S . . 
C1 C 0.9797(15) 0.7500 0.1116(15) 0.026(5) Uani 1 2 d S . . 
C2 C 0.8274(14) 0.7500 0.1734(16) 0.026(4) Uani 1 2 d S . . 
C3 C 0.9959(16) 1.2500 0.3597(16) 0.026(4) Uani 1 2 d S . . 
C4 C 0.8467(14) 0.7500 0.5684(16) 0.026(4) Uani 1 2 d S . . 

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 0.0223(6) 0.0251(6) 0.0056(5) 0.000 0.0013(2) 0.000 
N1 0.024(8) 0.047(11) 0.007(7) 0.000 0.004(6) 0.000 
N2 0.023(9) 0.047(11) 0.008(8) 0.000 0.005(6) 0.000 
N3 0.023(8) 0.047(11) 0.008(8) 0.000 0.004(6) 0.000 
N5 0.022(8) 0.045(10) 0.011(8) 0.000 -0.010(6) 0.000 
N4 0.022(9) 0.045(11) 0.012(7) 0.000 -0.010(6) 0.000 
N6 0.022(8) 0.045(12) 0.011(8) 0.000 -0.010(6) 0.000 
C1 0.023(11) 0.047(14) 0.007(9) 0.000 0.005(7) 0.000 
C2 0.023(9) 0.047(13) 0.008(9) 0.000 0.004(7) 0.000 
C3 0.022(9) 0.045(12) 0.011(9) 0.000 -0.010(8) 0.000 
C4 0.022(10) 0.045(12) 0.011(9) 0.000 -0.009(8) 0.000 

_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 N3 2.639(11) . ? 
Pb1 N3 2.639(11) 1_565 ? 
Pb1 N4 2.655(17) . ? 
Pb1 N6 2.662(11) 1_565 ? 
Pb1 N6 2.662(11) . ? 
Pb1 N1 2.820(14) 6_556 ? 
Pb1 N1 2.820(14) 6_566 ? 
Pb1 N2 2.822(17) 2_675 ? 
Pb1 N5 3.138(17) 6_556 ? 
Pb1 Pb1 3.9950(10) 1_545 ? 
Pb1 Pb1 3.9950(10) 1_565 ? 
N1 C1 1.18(3) . ? 
N1 Pb1 2.820(14) 6_656 ? 
N1 Pb1 2.820(14) 6_646 ? 
N2 C1 1.29(2) . ? 
N2 C2 1.31(3) . ? 
N2 Pb1 2.822(17) 2_674 ? 
N3 C2 1.23(3) . ? 
N3 Pb1 2.639(11) 1_545 ? 
N5 C3 1.32(3) . ? 
N5 C4 1.34(2) 5_776 ? 
N5 Pb1 3.138(17) 6_656 ? 
N4 C3 1.16(3) . ? 
N6 C4 1.15(2) . ? 
N6 Pb1 2.662(11) 1_545 ? 
C4 N5 1.34(2) 5_776 ? 

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 
N3 Pb1 N3 98.4(5) . 1_565 ? 
N3 Pb1 N4 71.5(4) . . ? 
N3 Pb1 N4 71.5(4) 1_565 . ? 
N3 Pb1 N6 144.8(5) . 1_565 ? 
N3 Pb1 N6 71.4(5) 1_565 1_565 ? 
N4 Pb1 N6 73.3(4) . 1_565 ? 
N3 Pb1 N6 71.4(5) . . ? 
N3 Pb1 N6 144.8(5) 1_565 . ? 
N4 Pb1 N6 73.3(4) . . ? 
N6 Pb1 N6 97.3(5) 1_565 . ? 
N3 Pb1 N1 70.6(4) . 6_556 ? 
N3 Pb1 N1 137.8(5) 1_565 6_556 ? 
N4 Pb1 N1 134.8(3) . 6_556 ? 
N6 Pb1 N1 139.0(5) 1_565 6_556 ? 
N6 Pb1 N1 72.0(4) . 6_556 ? 
N3 Pb1 N1 137.8(5) . 6_566 ? 
N3 Pb1 N1 70.6(4) 1_565 6_566 ? 
N4 Pb1 N1 134.8(3) . 6_566 ? 
N6 Pb1 N1 72.0(4) 1_565 6_566 ? 
N6 Pb1 N1 139.0(5) . 6_566 ? 
N1 Pb1 N1 90.2(6) 6_556 6_566 ? 
N3 Pb1 N2 130.6(3) . 2_675 ? 
N3 Pb1 N2 130.6(3) 1_565 2_675 ? 
N4 Pb1 N2 124.6(5) . 2_675 ? 
N6 Pb1 N2 70.9(4) 1_565 2_675 ? 
N6 Pb1 N2 70.9(4) . 2_675 ? 
N1 Pb1 N2 68.1(4) 6_556 2_675 ? 
N1 Pb1 N2 68.1(4) 6_566 2_675 ? 
N3 Pb1 N5 67.8(4) . 6_556 ? 
N3 Pb1 N5 67.8(4) 1_565 6_556 ? 
N4 Pb1 N5 115.6(5) . 6_556 ? 
N6 Pb1 N5 131.4(3) 1_565 6_556 ? 
N6 Pb1 N5 131.4(3) . 6_556 ? 
N1 Pb1 N5 70.4(3) 6_556 6_556 ? 
N1 Pb1 N5 70.4(3) 6_566 6_556 ? 
N2 Pb1 N5 119.8(5) 2_675 6_556 ? 
N3 Pb1 Pb1 40.8(3) . 1_545 ? 
N3 Pb1 Pb1 139.2(3) 1_565 1_545 ? 
N4 Pb1 Pb1 90.0 . 1_545 ? 
N6 Pb1 Pb1 138.6(3) 1_565 1_545 ? 
N6 Pb1 Pb1 41.4(3) . 1_545 ? 
N1 Pb1 Pb1 44.9(3) 6_556 1_545 ? 
N1 Pb1 Pb1 135.1(3) 6_566 1_545 ? 
N2 Pb1 Pb1 90.000(1) 2_675 1_545 ? 
N5 Pb1 Pb1 90.000(1) 6_556 1_545 ? 
N3 Pb1 Pb1 139.2(3) . 1_565 ? 
N3 Pb1 Pb1 40.8(3) 1_565 1_565 ? 
N4 Pb1 Pb1 90.0 . 1_565 ? 
N6 Pb1 Pb1 41.4(3) 1_565 1_565 ? 
N6 Pb1 Pb1 138.6(3) . 1_565 ? 
N1 Pb1 Pb1 135.1(3) 6_556 1_565 ? 
N1 Pb1 Pb1 44.9(3) 6_566 1_565 ? 
N2 Pb1 Pb1 90.000(1) 2_675 1_565 ? 
N5 Pb1 Pb1 90.000(1) 6_556 1_565 ? 
Pb1 Pb1 Pb1 180.0 1_545 1_565 ? 
C1 N1 Pb1 134.8(3) . 6_656 ? 
C1 N1 Pb1 134.8(3) . 6_646 ? 
Pb1 N1 Pb1 90.2(6) 6_656 6_646 ? 
C1 N2 C2 114.1(18) . . ? 
C1 N2 Pb1 132.1(13) . 2_674 ? 
C2 N2 Pb1 113.8(13) . 2_674 ? 
C2 N3 Pb1 127.7(5) . . ? 
C2 N3 Pb1 127.7(5) . 1_545 ? 
Pb1 N3 Pb1 98.4(5) . 1_545 ? 
C3 N5 C4 119.2(18) . 5_776 ? 
C3 N5 Pb1 130.0(13) . 6_656 ? 
C4 N5 Pb1 110.8(12) 5_776 6_656 ? 
C3 N4 Pb1 172.7(15) . . ? 
C4 N6 Pb1 129.1(4) . 1_545 ? 
C4 N6 Pb1 129.1(4) . . ? 
Pb1 N6 Pb1 97.3(5) 1_545 . ? 
N1 C1 N2 166.2(19) . . ? 
N3 C2 N2 174(2) . . ? 
N4 C3 N5 170(2) . . ? 
N6 C4 N5 169(2) . 5_776 ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              24.97 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    2.781 
_refine_diff_density_min   -2.319 
_refine_diff_density_rms    0.349