# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2005


data_global
_journal_name_full               J.Mater.Chem.

_journal_coden_cambridge         1145
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?

loop_
_publ_author_name
;
P. O'Brien
;
'Madeleine Helliwell'
'Mohammad Malik'

_publ_contact_author_name        
;
ProfD Paul O'Brien
;
_publ_contact_author_address     
;
School of Chemistry
University of Manchester
Oxford Road
Manchester
M13 9PL
UNITED KINGDOM
;

_publ_contact_author_email       PAUL.OBRIEN@MANCHESTER.AC.UK

_publ_section_title              
;
A new synthesis of InAs quantum dots from
[tBu2AsInEt2]2
;

data_h:\s1830\work\s1830abs
_database_code_depnum_ccdc_archive 'CCDC 236645'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
#------------------------------------------------------------------------------

_publ_section_exptl_refinement   
;
The structure was solved by the Patterson method.
The asymmetric unit 1/2 of the molecule.
All non-H atoms were refined anisotropically, with restraints
on the thermal motion of the C atoms.
H atoms were included in calculated positions.

;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H56 As2 In2'
_chemical_formula_weight         724.17

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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/n

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

_cell_length_a                   8.8461(16)
_cell_length_b                   11.626(2)
_cell_length_c                   14.915(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.171(3)
_cell_angle_gamma                90.00
_cell_volume                     1533.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3669
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.43

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    3.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4620
_exptl_absorpt_correction_T_max  0.5286
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  '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            8476
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         26.47
_reflns_number_total             3150
_reflns_number_gt                2739
_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^)+(0.0404P)^2^+5.5195P] 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         3150
_refine_ls_number_parameters     136
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1057
_refine_ls_wR_factor_gt          0.1022
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.148
_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
In1 In 0.15195(4) 0.28472(3) 0.62699(2) 0.02175(13) Uani 1 1 d . . .
As1 As 0.2500 0.43881(6) 0.7500 0.01783(17) Uani 1 2 d S . .
As2 As 0.2500 0.12849(6) 0.7500 0.01582(17) Uani 1 2 d S . .
C1 C -0.0938(7) 0.2901(6) 0.6023(5) 0.0417(16) Uani 1 1 d U . .
H1A H -0.1451 0.2785 0.6599 0.050 Uiso 1 1 calc R . .
H1B H -0.1215 0.3676 0.5799 0.050 Uiso 1 1 calc R . .
C2 C -0.1521(8) 0.2016(7) 0.5359(5) 0.0518(19) Uani 1 1 d U . .
H2A H -0.0948 0.2071 0.4805 0.078 Uiso 1 1 calc R . .
H2B H -0.2594 0.2159 0.5226 0.078 Uiso 1 1 calc R . .
H2C H -0.1397 0.1245 0.5615 0.078 Uiso 1 1 calc R . .
C3 C 0.2813(8) 0.2843(5) 0.5021(3) 0.0369(14) Uani 1 1 d U . .
H3A H 0.2772 0.3626 0.4761 0.044 Uiso 1 1 calc R . .
H3B H 0.3884 0.2677 0.5177 0.044 Uiso 1 1 calc R . .
C4 C 0.2313(8) 0.2025(8) 0.4330(5) 0.057(2) Uani 1 1 d U . .
H4A H 0.2386 0.1241 0.4567 0.086 Uiso 1 1 calc R . .
H4B H 0.2958 0.2097 0.3806 0.086 Uiso 1 1 calc R . .
H4C H 0.1262 0.2190 0.4154 0.086 Uiso 1 1 calc R . .
C5 C 0.0807(7) 0.5369(5) 0.7956(5) 0.0405(14) Uani 1 1 d U . .
C6 C 0.1362(11) 0.6129(9) 0.8720(8) 0.106(3) Uani 1 1 d U . .
H6A H 0.0527 0.6611 0.8925 0.158 Uiso 1 1 calc R . .
H6B H 0.2183 0.6621 0.8513 0.158 Uiso 1 1 calc R . .
H6C H 0.1733 0.5647 0.9217 0.158 Uiso 1 1 calc R . .
C7 C 0.0087(11) 0.6074(8) 0.7190(8) 0.095(3) Uani 1 1 d U . .
H7A H -0.0209 0.5560 0.6697 0.142 Uiso 1 1 calc R . .
H7B H 0.0819 0.6639 0.6977 0.142 Uiso 1 1 calc R . .
H7C H -0.0808 0.6475 0.7408 0.142 Uiso 1 1 calc R . .
C8 C -0.0382(6) 0.4540(5) 0.8293(4) 0.0305(11) Uani 1 1 d U . .
H8A H 0.0067 0.4045 0.8759 0.046 Uiso 1 1 calc R . .
H8B H -0.0758 0.4064 0.7794 0.046 Uiso 1 1 calc R . .
H8C H -0.1222 0.4976 0.8543 0.046 Uiso 1 1 calc R . .
C9 C 0.0804(6) 0.0292(5) 0.7948(4) 0.0238(10) Uani 1 1 d U . .
C10 C -0.0379(8) 0.1110(6) 0.8254(7) 0.072(2) Uani 1 1 d U . .
H10A H -0.1221 0.0677 0.8505 0.109 Uiso 1 1 calc R . .
H10B H -0.0747 0.1569 0.7743 0.109 Uiso 1 1 calc R . .
H10C H 0.0055 0.1620 0.8714 0.109 Uiso 1 1 calc R . .
C11 C 0.0137(10) -0.0445(8) 0.7216(5) 0.074(3) Uani 1 1 d U . .
H11A H -0.0789 -0.0810 0.7426 0.111 Uiso 1 1 calc R . .
H11B H 0.0866 -0.1040 0.7052 0.111 Uiso 1 1 calc R . .
H11C H -0.0103 0.0033 0.6691 0.111 Uiso 1 1 calc R . .
C12 C 0.1300(9) -0.0428(9) 0.8730(6) 0.082(3) Uani 1 1 d U . .
H12A H 0.1742 0.0068 0.9198 0.124 Uiso 1 1 calc R . .
H12B H 0.2057 -0.0986 0.8538 0.124 Uiso 1 1 calc R . .
H12C H 0.0427 -0.0836 0.8969 0.124 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
In1 0.0274(2) 0.0176(2) 0.0199(2) -0.00159(14) -0.00710(14) 0.00165(15)
As1 0.0222(4) 0.0130(3) 0.0181(3) 0.000 -0.0030(3) 0.000
As2 0.0145(3) 0.0134(3) 0.0195(3) 0.000 -0.0002(3) 0.000
C1 0.030(3) 0.035(3) 0.060(4) -0.005(3) -0.027(3) 0.007(3)
C2 0.042(4) 0.074(5) 0.039(4) -0.013(3) 0.001(3) -0.025(4)
C3 0.067(4) 0.031(3) 0.013(2) 0.005(2) 0.007(3) 0.000(3)
C4 0.032(3) 0.093(6) 0.047(4) -0.036(4) -0.004(3) 0.011(4)
C5 0.042(3) 0.022(3) 0.058(4) -0.013(2) 0.013(3) 0.008(2)
C6 0.070(6) 0.104(7) 0.145(7) -0.106(6) 0.053(5) -0.034(4)
C7 0.069(6) 0.072(6) 0.145(7) 0.068(5) 0.040(5) 0.048(5)
C8 0.022(3) 0.037(3) 0.033(3) -0.006(2) 0.002(2) 0.0116(19)
C9 0.019(2) 0.024(3) 0.029(3) 0.0022(19) 0.001(2) -0.0066(18)
C10 0.040(4) 0.036(4) 0.143(7) -0.004(4) 0.055(4) -0.007(2)
C11 0.082(6) 0.088(6) 0.053(4) -0.027(4) 0.018(3) -0.069(5)
C12 0.037(4) 0.121(7) 0.088(5) 0.078(5) -0.016(4) -0.027(4)

_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
In1 C1 2.198(6) . ?
In1 C3 2.206(6) . ?
In1 As1 2.6949(7) . ?
In1 As2 2.7116(7) . ?
As1 C5 2.012(6) . ?
As1 C5 2.012(6) 2_556 ?
As1 In1 2.6949(7) 2_556 ?
As2 C9 2.017(5) . ?
As2 C9 2.017(5) 2_556 ?
As2 In1 2.7116(7) 2_556 ?
C1 C2 1.511(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.464(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.516(10) . ?
C5 C8 1.520(9) . ?
C5 C7 1.534(11) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.492(8) . ?
C9 C12 1.495(9) . ?
C9 C11 1.499(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
C1 In1 C3 112.8(3) . . ?
C1 In1 As1 113.49(18) . . ?
C3 In1 As1 114.26(17) . . ?
C1 In1 As2 115.74(19) . . ?
C3 In1 As2 113.92(17) . . ?
As1 In1 As2 83.72(2) . . ?
C5 As1 C5 110.9(4) . 2_556 ?
C5 As1 In1 112.1(2) . . ?
C5 As1 In1 112.2(2) 2_556 . ?
C5 As1 In1 112.2(2) . 2_556 ?
C5 As1 In1 112.1(2) 2_556 2_556 ?
In1 As1 In1 96.67(3) . 2_556 ?
C9 As2 C9 110.2(3) . 2_556 ?
C9 As2 In1 112.90(15) . 2_556 ?
C9 As2 In1 112.18(15) 2_556 2_556 ?
C9 As2 In1 112.18(15) . . ?
C9 As2 In1 112.90(15) 2_556 . ?
In1 As2 In1 95.89(3) 2_556 . ?
C2 C1 In1 114.4(5) . . ?
C2 C1 H1A 108.7 . . ?
In1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
In1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 In1 116.2(5) . . ?
C4 C3 H3A 108.2 . . ?
In1 C3 H3A 108.2 . . ?
C4 C3 H3B 108.2 . . ?
In1 C3 H3B 108.2 . . ?
H3A C3 H3B 107.4 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C8 109.7(6) . . ?
C6 C5 C7 111.8(8) . . ?
C8 C5 C7 107.8(6) . . ?
C6 C5 As1 110.7(5) . . ?
C8 C5 As1 106.1(4) . . ?
C7 C5 As1 110.6(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C12 108.3(7) . . ?
C10 C9 C11 108.6(7) . . ?
C12 C9 C11 110.7(7) . . ?
C10 C9 As2 105.5(4) . . ?
C12 C9 As2 111.7(4) . . ?
C11 C9 As2 111.7(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 In1 As1 C5 -1.9(3) . . . . ?
C3 In1 As1 C5 129.3(3) . . . . ?
As2 In1 As1 C5 -117.3(2) . . . . ?
C1 In1 As1 C5 -127.5(3) . . . 2_556 ?
C3 In1 As1 C5 3.7(3) . . . 2_556 ?
As2 In1 As1 C5 117.2(2) . . . 2_556 ?
C1 In1 As1 In1 115.4(2) . . . 2_556 ?
C3 In1 As1 In1 -113.44(19) . . . 2_556 ?
As2 In1 As1 In1 0.0 . . . 2_556 ?
C1 In1 As2 C9 4.6(3) . . . . ?
C3 In1 As2 C9 -128.5(3) . . . . ?
As1 In1 As2 C9 117.68(17) . . . . ?
C1 In1 As2 C9 129.8(3) . . . 2_556 ?
C3 In1 As2 C9 -3.3(3) . . . 2_556 ?
As1 In1 As2 C9 -117.10(17) . . . 2_556 ?
C1 In1 As2 In1 -113.1(2) . . . 2_556 ?
C3 In1 As2 In1 113.79(19) . . . 2_556 ?
As1 In1 As2 In1 0.0 . . . 2_556 ?
C3 In1 C1 C2 50.1(6) . . . . ?
As1 In1 C1 C2 -178.0(5) . . . . ?
As2 In1 C1 C2 -83.5(5) . . . . ?
C1 In1 C3 C4 -48.0(6) . . . . ?
As1 In1 C3 C4 -179.5(5) . . . . ?
As2 In1 C3 C4 86.5(5) . . . . ?
C5 As1 C5 C6 -60.2(6) 2_556 . . . ?
In1 As1 C5 C6 173.5(6) . . . . ?
In1 As1 C5 C6 66.0(6) 2_556 . . . ?
C5 As1 C5 C8 -179.1(5) 2_556 . . . ?
In1 As1 C5 C8 54.6(5) . . . . ?
In1 As1 C5 C8 -52.9(5) 2_556 . . . ?
C5 As1 C5 C7 64.2(6) 2_556 . . . ?
In1 As1 C5 C7 -62.0(6) . . . . ?
In1 As1 C5 C7 -169.6(5) 2_556 . . . ?
C9 As2 C9 C10 -179.7(6) 2_556 . . . ?
In1 As2 C9 C10 54.0(5) 2_556 . . . ?
In1 As2 C9 C10 -53.0(5) . . . . ?
C9 As2 C9 C12 62.8(6) 2_556 . . . ?
In1 As2 C9 C12 -63.5(6) 2_556 . . . ?
In1 As2 C9 C12 -170.5(6) . . . . ?
C9 As2 C9 C11 -61.8(5) 2_556 . . . ?
In1 As2 C9 C11 171.9(5) 2_556 . . . ?
In1 As2 C9 C11 64.9(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.47
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.146