#Supplementary Material (ESI) for Journal of Materials Chemistry
#This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               J.Mater.Chem.

_journal_coden_Cambridge         1145
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        "Paul O'Brien"
_publ_contact_author_email       paul.obrien@manchester.ac.uk

_publ_section_title              
;
Controlled Synthesis of PbS Nanoparticles and the Deposition
of Thin films by Aerosol-Assisted Chemical Vapour Deposition (AACVD)

;
loop_
_publ_author_name
'Javeed Akhtar'
'Mohammad Malik'
"Paul O'Brien"
'Madeleine Helliwell'

# Attachment '- s2630abs.cif'

data_s2630abs
_database_code_depnum_ccdc_archive 'CCDC 685543'
#TrackingRef '- s2630abs.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H20 N2 Pb S4'
_chemical_formula_weight         599.79

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   10.1600(17)
_cell_length_b                   5.1600(9)
_cell_length_c                   18.758(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.687(4)
_cell_angle_gamma                90.00
_cell_volume                     980.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    817
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      24.20

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    9.037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7384
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         26.42
_reflns_number_total             2021
_reflns_number_gt                1986
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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^)+(0.0148P)^2^+0.3578P] 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         2021
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0132
_refine_ls_R_factor_gt           0.0129
_refine_ls_wR_factor_ref         0.0306
_refine_ls_wR_factor_gt          0.0305
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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 1.0000 1.179726(19) 0.2500 0.01938(4) Uani 1 2 d S . .
S1 S 0.81159(5) 0.81382(9) 0.21995(3) 0.01734(10) Uani 1 1 d . . .
S2 S 0.98873(5) 0.97191(10) 0.10817(3) 0.01839(10) Uani 1 1 d . . .
N1 N 0.79531(16) 0.6219(3) 0.08806(9) 0.0144(3) Uani 1 1 d . . .
C1 C 0.85989(19) 0.7865(4) 0.13353(10) 0.0143(4) Uani 1 1 d . . .
C2 C 0.83527(19) 0.5751(4) 0.01578(10) 0.0166(4) Uani 1 1 d . . .
H2A H 0.8397 0.3897 0.0079 0.020 Uiso 1 1 calc R . .
H2B H 0.9231 0.6455 0.0124 0.020 Uiso 1 1 calc R . .
C3 C 0.74280(19) 0.6937(4) -0.04225(11) 0.0149(4) Uani 1 1 d . . .
C4 C 0.7369(2) 0.5921(4) -0.11153(11) 0.0197(4) Uani 1 1 d . . .
H4 H 0.7868 0.4470 -0.1210 0.024 Uiso 1 1 calc R . .
C5 C 0.6568(2) 0.7071(4) -0.16618(12) 0.0239(5) Uani 1 1 d . . .
H5 H 0.6534 0.6388 -0.2122 0.029 Uiso 1 1 calc R . .
C6 C 0.5817(2) 0.9246(5) -0.15231(11) 0.0240(4) Uani 1 1 d . . .
H6 H 0.5278 1.0014 -0.1889 0.029 Uiso 1 1 calc R . .
C7 C 0.5877(2) 1.0252(4) -0.08394(11) 0.0218(4) Uani 1 1 d . . .
H7 H 0.5378 1.1703 -0.0745 0.026 Uiso 1 1 calc R . .
C8 C 0.66777(19) 0.9116(4) -0.02918(11) 0.0174(4) Uani 1 1 d . . .
H8 H 0.6713 0.9817 0.0166 0.021 Uiso 1 1 calc R . .
C9 C 0.68460(19) 0.4630(4) 0.10865(11) 0.0168(4) Uani 1 1 d . . .
H9A H 0.6364 0.5570 0.1422 0.025 Uiso 1 1 calc R . .
H9B H 0.7180 0.3051 0.1303 0.025 Uiso 1 1 calc R . .
H9C H 0.6271 0.4232 0.0669 0.025 Uiso 1 1 calc 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 0.02317(7) 0.01386(6) 0.01974(7) 0.000 -0.00665(4) 0.000
S1 0.0201(2) 0.0201(2) 0.0116(2) 0.00031(18) 0.00005(18) -0.00254(19)
S2 0.0177(2) 0.0213(2) 0.0159(2) 0.00360(19) -0.00027(19) -0.00342(19)
N1 0.0150(8) 0.0153(7) 0.0128(8) 0.0011(6) 0.0003(6) 0.0006(6)
C1 0.0146(9) 0.0148(9) 0.0130(9) 0.0029(7) -0.0015(7) 0.0038(7)
C2 0.0163(9) 0.0189(9) 0.0148(10) -0.0027(8) 0.0025(7) 0.0030(8)
C3 0.0142(9) 0.0164(9) 0.0144(10) 0.0009(7) 0.0018(7) -0.0044(7)
C4 0.0216(10) 0.0205(10) 0.0177(10) -0.0017(8) 0.0052(8) -0.0006(8)
C5 0.0307(12) 0.0284(11) 0.0128(10) -0.0013(9) 0.0033(9) -0.0057(9)
C6 0.0233(11) 0.0303(11) 0.0180(11) 0.0078(9) -0.0018(8) -0.0010(9)
C7 0.0228(10) 0.0205(10) 0.0223(11) 0.0031(8) 0.0023(8) 0.0027(8)
C8 0.0207(10) 0.0172(9) 0.0146(9) -0.0016(8) 0.0017(8) 0.0000(8)
C9 0.0156(9) 0.0162(9) 0.0183(10) 0.0012(8) -0.0003(7) 0.0001(8)

_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 S1 2.7148(15) 2_755 ?
Pb1 S1 2.7149(15) . ?
Pb1 S2 2.8621(9) 2_755 ?
Pb1 S2 2.8621(9) . ?
S1 C1 1.737(2) . ?
S2 C1 1.719(2) . ?
N1 C1 1.337(3) . ?
N1 C2 1.467(2) . ?
N1 C9 1.469(2) . ?
C2 C3 1.508(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C8 1.392(3) . ?
C3 C4 1.398(3) . ?
C4 C5 1.388(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.380(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 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
S1 Pb1 S1 91.87(7) 2_755 . ?
S1 Pb1 S2 64.69(2) 2_755 2_755 ?
S1 Pb1 S2 84.63(3) . 2_755 ?
S1 Pb1 S2 84.63(3) 2_755 . ?
S1 Pb1 S2 64.69(2) . . ?
S2 Pb1 S2 135.99(5) 2_755 . ?
C1 S1 Pb1 90.11(7) . . ?
C1 S2 Pb1 85.69(7) . . ?
C1 N1 C2 122.39(17) . . ?
C1 N1 C9 122.23(17) . . ?
C2 N1 C9 115.27(16) . . ?
N1 C1 S2 121.46(15) . . ?
N1 C1 S1 119.03(15) . . ?
S2 C1 S1 119.50(12) . . ?
N1 C2 C3 113.40(16) . . ?
N1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C8 C3 C4 118.96(19) . . ?
C8 C3 C2 121.23(18) . . ?
C4 C3 C2 119.73(18) . . ?
C5 C4 C3 120.3(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C8 120.6(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C3 120.49(19) . . ?
C7 C8 H8 119.8 . . ?
C3 C8 H8 119.8 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.42
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.072