Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 loop_ _publ_author_name P.O'Brien 'Mohammad Afzaal' 'David Crouch' 'Mohammad A. Malik' 'Majid Motevalli' 'Jin-Ho Park' _publ_contact_author_name ; Prof Paul O'Brien ; _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email PAUL.OBRIEN@MAN.AC.UK _publ_section_title ; Deposition of CdSe thin films using a novel single-source precursor; [MeCd(SePiPr2)2N]2 ; data_ma3 _database_code_CSD 193982 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H62 Cd2 N2 P4 Se4' _chemical_formula_weight 1067.30 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' Cd Cd -0.8075 1.2024 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.625(8) _cell_length_b 10.143(9) _cell_length_c 11.180(9) _cell_angle_alpha 103.44(8) _cell_angle_beta 80.97(9) _cell_angle_gamma 111.88(9) _cell_volume 982.1(14) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 4.971 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2132 _exptl_absorpt_correction_T_max 0.6363 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3715 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3449 _reflns_number_gt 2931 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0491P)^2^+0.5274P] 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 3449 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.001 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 Cd1 Cd 0.10588(3) 0.52843(3) 0.33404(3) 0.01946(10) Uani 1 1 d . . . Se1 Se 0.07777(4) 0.26858(4) 0.19480(4) 0.01773(11) Uani 1 1 d . . . Se2 Se -0.16651(4) 0.53059(4) 0.43838(3) 0.01350(11) Uani 1 1 d . . . N1 N -0.2772(3) 0.2057(3) 0.2691(3) 0.0138(7) Uani 1 1 d . . . P1 P -0.15571(10) 0.13239(10) 0.22131(9) 0.0103(2) Uani 1 1 d . . . P2 P -0.31289(10) 0.34964(10) 0.31043(9) 0.0099(2) Uani 1 1 d . . . C1 C 0.2636(5) 0.7028(5) 0.2497(4) 0.0275(10) Uani 1 1 d . . . H1A H 0.3410 0.6700 0.1978 0.041 Uiso 1 1 calc R . . H1B H 0.3109 0.7849 0.3141 0.041 Uiso 1 1 calc R . . H1C H 0.2108 0.7327 0.1988 0.041 Uiso 1 1 calc R . . C2 C -0.1726(4) 0.0142(4) 0.3278(4) 0.0156(8) Uani 1 1 d . . . H2 H -0.2810 -0.0478 0.3362 0.019 Uiso 1 1 calc R . . C3 C -0.1309(5) 0.1039(5) 0.4555(4) 0.0267(10) Uani 1 1 d . . . H3A H -0.1529 0.0392 0.5142 0.040 Uiso 1 1 calc R . . H3B H -0.1894 0.1681 0.4822 0.040 Uiso 1 1 calc R . . H3C H -0.0235 0.1620 0.4520 0.040 Uiso 1 1 calc R . . C4 C -0.0840(5) -0.0869(5) 0.2818(4) 0.0255(10) Uani 1 1 d . . . H4A H 0.0234 -0.0298 0.2734 0.038 Uiso 1 1 calc R . . H4B H -0.1164 -0.1457 0.2014 0.038 Uiso 1 1 calc R . . H4C H -0.1017 -0.1504 0.3409 0.038 Uiso 1 1 calc R . . C5 C -0.2077(4) 0.0134(4) 0.0726(3) 0.0160(8) Uani 1 1 d . . . H5 H -0.1312 -0.0342 0.0426 0.019 Uiso 1 1 calc R . . C6 C -0.3619(5) -0.1058(5) 0.0852(4) 0.0252(10) Uani 1 1 d . . . H6A H -0.4386 -0.0615 0.1157 0.038 Uiso 1 1 calc R . . H6B H -0.3594 -0.1637 0.1434 0.038 Uiso 1 1 calc R . . H6C H -0.3861 -0.1684 0.0045 0.038 Uiso 1 1 calc R . . C7 C -0.2057(5) 0.1008(5) -0.0218(4) 0.0247(10) Uani 1 1 d . . . H7A H -0.2250 0.0370 -0.1025 0.037 Uiso 1 1 calc R . . H7B H -0.1072 0.1773 -0.0272 0.037 Uiso 1 1 calc R . . H7C H -0.2836 0.1444 0.0037 0.037 Uiso 1 1 calc R . . C8 C -0.5005(4) 0.2990(4) 0.3876(4) 0.0161(8) Uani 1 1 d . . . H8 H -0.5285 0.3877 0.4129 0.019 Uiso 1 1 calc R . . C9 C -0.5056(5) 0.2426(5) 0.5032(4) 0.0285(10) Uani 1 1 d . . . H9A H -0.6079 0.2165 0.5430 0.043 Uiso 1 1 calc R . . H9B H -0.4364 0.3179 0.5602 0.043 Uiso 1 1 calc R . . H9C H -0.4758 0.1571 0.4810 0.043 Uiso 1 1 calc R . . C10 C -0.6148(5) 0.1875(5) 0.3002(4) 0.0253(10) Uani 1 1 d . . . H10A H -0.5899 0.0993 0.2743 0.038 Uiso 1 1 calc R . . H10B H -0.6122 0.2273 0.2276 0.038 Uiso 1 1 calc R . . H10C H -0.7156 0.1646 0.3428 0.038 Uiso 1 1 calc R . . C11 C -0.3192(4) 0.4220(4) 0.1758(4) 0.0176(8) Uani 1 1 d . . . H11 H -0.3752 0.3375 0.1140 0.021 Uiso 1 1 calc R . . C12 C -0.1635(5) 0.4887(5) 0.1147(4) 0.0241(10) Uani 1 1 d . . . H12A H -0.1724 0.5091 0.0353 0.036 Uiso 1 1 calc R . . H12B H -0.1093 0.4210 0.1012 0.036 Uiso 1 1 calc R . . H12C H -0.1083 0.5789 0.1682 0.036 Uiso 1 1 calc R . . C13 C -0.4040(5) 0.5268(5) 0.2030(5) 0.0305(11) Uani 1 1 d . . . H13A H -0.3528 0.6118 0.2635 0.046 Uiso 1 1 calc R . . H13B H -0.5066 0.4791 0.2363 0.046 Uiso 1 1 calc R . . H13C H -0.4073 0.5571 0.1267 0.046 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 Cd1 0.01476(16) 0.01390(16) 0.02341(18) 0.00380(12) 0.00057(12) -0.00147(12) Se1 0.0086(2) 0.0145(2) 0.0257(2) -0.00066(16) -0.00129(16) 0.00178(15) Se2 0.0116(2) 0.01173(19) 0.0144(2) -0.00096(15) -0.00566(15) 0.00119(15) N1 0.0076(15) 0.0116(15) 0.0206(17) 0.0016(13) -0.0027(13) 0.0016(13) P1 0.0086(5) 0.0081(4) 0.0129(5) 0.0004(4) -0.0026(4) 0.0018(4) P2 0.0079(4) 0.0101(4) 0.0111(5) 0.0007(4) -0.0037(4) 0.0020(4) C1 0.028(2) 0.023(2) 0.022(2) 0.0074(19) -0.0042(19) -0.0052(19) C2 0.0139(19) 0.0123(18) 0.021(2) 0.0046(16) -0.0068(16) 0.0021(16) C3 0.038(3) 0.026(2) 0.020(2) 0.0050(18) -0.012(2) 0.011(2) C4 0.030(2) 0.021(2) 0.031(2) 0.0056(19) -0.006(2) 0.0126(19) C5 0.015(2) 0.0125(18) 0.018(2) -0.0016(16) -0.0040(16) 0.0028(16) C6 0.022(2) 0.021(2) 0.024(2) -0.0011(18) -0.0086(18) -0.0014(18) C7 0.032(3) 0.025(2) 0.014(2) 0.0018(17) -0.0055(18) 0.0066(19) C8 0.0074(18) 0.0161(19) 0.021(2) -0.0009(16) -0.0037(16) 0.0018(15) C9 0.016(2) 0.038(3) 0.021(2) 0.0072(19) 0.0014(18) -0.0033(19) C10 0.012(2) 0.027(2) 0.030(2) 0.0018(19) -0.0065(18) -0.0017(17) C11 0.019(2) 0.0173(19) 0.018(2) 0.0024(16) -0.0080(17) 0.0058(17) C12 0.031(2) 0.023(2) 0.019(2) 0.0100(18) -0.0012(18) 0.0073(19) C13 0.031(3) 0.029(2) 0.042(3) 0.012(2) -0.007(2) 0.017(2) _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 Cd1 C1 2.156(5) . ? Cd1 Se1 2.672(3) . ? Cd1 Se2 2.703(3) . ? Cd1 Se2 2.934(2) 2_566 ? Se1 P1 2.171(3) . ? Se2 P2 2.210(3) . ? Se2 Cd1 2.934(2) 2_566 ? N1 P2 1.572(3) . ? N1 P1 1.573(3) . ? P1 C2 1.827(4) . ? P1 C5 1.830(4) . ? P2 C8 1.815(4) . ? P2 C11 1.839(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.521(6) . ? C2 C3 1.527(6) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.522(6) . ? C5 C6 1.537(6) . ? C5 H5 1.0000 . ? 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 C9 1.517(6) . ? C8 C10 1.530(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.519(6) . ? C11 C12 1.519(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 Cd1 Se1 112.48(15) . . ? C1 Cd1 Se2 122.56(15) . . ? Se1 Cd1 Se2 109.61(10) . . ? C1 Cd1 Se2 121.19(14) . 2_566 ? Se1 Cd1 Se2 96.86(8) . 2_566 ? Se2 Cd1 Se2 89.68(8) . 2_566 ? P1 Se1 Cd1 106.62(10) . . ? P2 Se2 Cd1 100.01(9) . . ? P2 Se2 Cd1 118.41(8) . 2_566 ? Cd1 Se2 Cd1 90.32(8) . 2_566 ? P2 N1 P1 147.7(2) . . ? N1 P1 C2 106.81(19) . . ? N1 P1 C5 107.98(19) . . ? C2 P1 C5 106.11(19) . . ? N1 P1 Se1 119.04(14) . . ? C2 P1 Se1 109.50(15) . . ? C5 P1 Se1 106.72(16) . . ? N1 P2 C8 105.66(19) . . ? N1 P2 C11 110.92(19) . . ? C8 P2 C11 107.3(2) . . ? N1 P2 Se2 118.67(14) . . ? C8 P2 Se2 106.80(16) . . ? C11 P2 Se2 106.92(15) . . ? Cd1 C1 H1A 109.5 . . ? Cd1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Cd1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C3 111.5(4) . . ? C4 C2 P1 113.5(3) . . ? C3 C2 P1 110.2(3) . . ? C4 C2 H2 107.1 . . ? C3 C2 H2 107.1 . . ? P1 C2 H2 107.1 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C6 110.8(3) . . ? C7 C5 P1 110.4(3) . . ? C6 C5 P1 111.4(3) . . ? C7 C5 H5 108.1 . . ? C6 C5 H5 108.1 . . ? P1 C5 H5 108.1 . . ? 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 . . ? C9 C8 C10 110.8(3) . . ? C9 C8 P2 111.3(3) . . ? C10 C8 P2 110.9(3) . . ? C9 C8 H8 107.9 . . ? C10 C8 H8 107.9 . . ? P2 C8 H8 107.9 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 110.8(4) . . ? C13 C11 P2 113.8(3) . . ? C12 C11 P2 111.9(3) . . ? C13 C11 H11 106.6 . . ? C12 C11 H11 106.6 . . ? P2 C11 H11 106.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.951 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.118