Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 _publ_contact_author_name 'Dr Jagadese Vittal' _publ_contact_author_address ; National University of Singapore 3 Science Drive 3 Singapore 117543 SINGAPORE ; _publ_contact_author_phone '(65) 6874 2975' _publ_contact_author_fax '(65) 6779 1691' _publ_contact_author_email chmjjv@nus.edu.sg # 3. TITLE AND AUTHOR LIST _publ_section_title ; Trialkyl Ammonium Salts of [M(SC{O}R]~-~ (M = Ga~3+~ and In~3+~) as Precursors for Metal Sulfide Bulk Materials and Thin Films ; loop_ _publ_author_name _publ_author_address 'Theivanayagam C. Deivaraj' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; 'Ming Lin' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; 'Kian Ping Loh' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; 'Mark Yeadon' ; Insstitute of Materials Research and Engineering 3 Research Link, Singapore 117602 ; 'Jagadese J. Vittal' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117543 ; _publ_requested_journal 'Journal of Materials Chemistry' #============================================================================== data_compound_3 _database_code_CSD 200806 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 Ga N O5 S4' _chemical_formula_weight 738.61 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.7250(3) _cell_length_b 12.8573(1) _cell_length_c 21.6933(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3549.2(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4849 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9145 _exptl_absorpt_correction_T_max 0.7082 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15161 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6957 _reflns_number_gt 4112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, 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^)+(0.0565P)^2^+1.4010P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(18) _refine_ls_number_reflns 6957 _refine_ls_number_parameters 392 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1299 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _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 Ga1 Ga 0.21349(6) 0.22609(6) 0.31709(3) 0.0526(2) Uani 1 1 d D . . S1 S 0.3130(10) 0.0905(9) 0.3524(5) 0.042(5) Uani 0.33 1 d PD . . S1A S 0.3458(9) 0.1153(10) 0.3441(5) 0.063(4) Uani 0.33 1 d PD . . S1B S 0.2816(10) 0.0847(11) 0.3664(5) 0.058(4) Uani 0.33 1 d PD . . S2 S 0.05400(17) 0.22006(16) 0.36383(10) 0.0751(6) Uani 1 1 d . . . S3 S 0.19372(14) 0.18959(15) 0.21513(8) 0.0623(5) Uani 1 1 d . . . S4 S 0.27796(16) 0.38642(14) 0.33775(9) 0.0673(5) Uani 1 1 d . . . O1 O 0.3589(15) 0.2246(10) 0.4428(8) 0.065(5) Uiso 0.33 1 d PD . . O1A O 0.3114(13) 0.2008(11) 0.4524(7) 0.073(5) Uiso 0.33 1 d PD . . O1B O 0.3982(11) 0.2260(10) 0.4204(7) 0.058(4) Uiso 0.33 1 d PD . . O2 O 0.0724(4) 0.0304(4) 0.3223(2) 0.0712(14) Uani 1 1 d . . . O3 O 0.3956(4) 0.2114(5) 0.2279(3) 0.0907(19) Uani 1 1 d . . . O4 O 0.0938(4) 0.4205(3) 0.2881(2) 0.0622(13) Uani 1 1 d . . . C1 C 0.3652(6) 0.1325(6) 0.4194(3) 0.075(2) Uani 1 1 d D . . C2 C 0.0249(6) 0.0873(5) 0.3565(3) 0.0514(17) Uani 1 1 d . . . C3 C 0.3257(6) 0.1879(5) 0.1930(4) 0.0588(19) Uani 1 1 d . . . C4 C 0.1692(5) 0.4591(5) 0.3134(3) 0.0496(16) Uani 1 1 d . . . C1A C 0.4216(5) 0.0535(5) 0.4572(3) 0.0537(18) Uani 1 1 d D . . C2A C 0.4451(6) -0.0435(6) 0.4346(3) 0.0611(19) Uani 1 1 d . . . H2A H 0.4304 -0.0596 0.3937 0.073 Uiso 1 1 calc R . . C3A C 0.4897(7) -0.1159(6) 0.4716(4) 0.079(2) Uani 1 1 d . . . H3A H 0.5054 -0.1815 0.4561 0.094 Uiso 1 1 calc R . . C4A C 0.5121(7) -0.0925(8) 0.5329(4) 0.080(3) Uani 1 1 d . . . H4A H 0.5437 -0.1416 0.5584 0.096 Uiso 1 1 calc R . . C5A C 0.4873(8) 0.0025(8) 0.5546(4) 0.095(3) Uani 1 1 d . . . H5A H 0.4994 0.0183 0.5958 0.114 Uiso 1 1 calc R . . C6A C 0.4452(8) 0.0744(7) 0.5173(4) 0.097(3) Uani 1 1 d . . . H6A H 0.4316 0.1404 0.5329 0.117 Uiso 1 1 calc R . . C1B C -0.0648(5) 0.0493(5) 0.3942(3) 0.0491(17) Uani 1 1 d . . . C2B C -0.0981(6) 0.0989(6) 0.4477(3) 0.0599(19) Uani 1 1 d . . . H2B H -0.0649 0.1592 0.4611 0.072 Uiso 1 1 calc R . . C3B C -0.1798(6) 0.0585(7) 0.4803(4) 0.073(2) Uani 1 1 d . . . H3B H -0.2006 0.0914 0.5165 0.087 Uiso 1 1 calc R . . C4B C -0.2318(7) -0.0274(7) 0.4620(5) 0.093(3) Uani 1 1 d . . . H4B H -0.2874 -0.0542 0.4849 0.112 Uiso 1 1 calc R . . C5B C -0.1995(9) -0.0740(7) 0.4081(5) 0.097(3) Uani 1 1 d . . . H5B H -0.2355 -0.1323 0.3940 0.117 Uiso 1 1 calc R . . C6B C -0.1161(7) -0.0378(7) 0.3743(4) 0.079(2) Uani 1 1 d . . . H6B H -0.0949 -0.0718 0.3385 0.095 Uiso 1 1 calc R . . C1C C 0.3472(6) 0.1550(5) 0.1286(3) 0.0508(17) Uani 1 1 d . . . C2C C 0.2724(7) 0.1452(6) 0.0841(3) 0.070(2) Uani 1 1 d . . . H2C H 0.2025 0.1583 0.0939 0.084 Uiso 1 1 calc R . . C3C C 0.2978(9) 0.1162(7) 0.0250(4) 0.093(3) Uani 1 1 d . . . H3C H 0.2460 0.1096 -0.0050 0.112 Uiso 1 1 calc R . . C4C C 0.4015(10) 0.0971(8) 0.0111(4) 0.096(3) Uani 1 1 d . . . H4C H 0.4199 0.0776 -0.0287 0.115 Uiso 1 1 calc R . . C5C C 0.4762(8) 0.1063(7) 0.0541(5) 0.093(3) Uani 1 1 d . . . H5C H 0.5462 0.0940 0.0442 0.111 Uiso 1 1 calc R . . C6C C 0.4488(6) 0.1341(6) 0.1132(3) 0.070(2) Uani 1 1 d . . . H6C H 0.5007 0.1388 0.1433 0.084 Uiso 1 1 calc R . . C1D C 0.1729(5) 0.5733(5) 0.3260(3) 0.0451(16) Uani 1 1 d . . . C2D C 0.0949(5) 0.6344(5) 0.3027(3) 0.0514(18) Uani 1 1 d . . . H2D H 0.0416 0.6043 0.2795 0.062 Uiso 1 1 calc R . . C3D C 0.0941(6) 0.7385(6) 0.3130(4) 0.0643(19) Uani 1 1 d . . . H3D H 0.0412 0.7797 0.2962 0.077 Uiso 1 1 calc R . . C4D C 0.1721(7) 0.7829(6) 0.3483(4) 0.077(2) Uani 1 1 d . . . H4D H 0.1713 0.8541 0.3560 0.093 Uiso 1 1 calc R . . C5D C 0.2500(6) 0.7229(7) 0.3720(4) 0.076(2) Uani 1 1 d . . . H5D H 0.3027 0.7535 0.3955 0.091 Uiso 1 1 calc R . . C6D C 0.2517(5) 0.6183(6) 0.3617(3) 0.0598(19) Uani 1 1 d . . . H6D H 0.3050 0.5774 0.3783 0.072 Uiso 1 1 calc R . . O5 O 0.8487(5) 0.4177(5) 0.3039(3) 0.112(2) Uani 1 1 d . . . N1 N 0.6683(5) 0.2965(5) 0.3380(3) 0.081(2) Uani 1 1 d D . . H1 H 0.7215 0.3429 0.3324 0.097 Uiso 1 1 calc R . . C5 C 0.5776(10) 0.3416(10) 0.3126(6) 0.174(2) Uiso 1 1 d D . . H5E H 0.5262 0.2863 0.3089 0.209 Uiso 1 1 calc R . . H5F H 0.5506 0.3896 0.3432 0.209 Uiso 1 1 calc R . . C6 C 0.5771(11) 0.3943(11) 0.2571(6) 0.174(2) Uiso 1 1 d D . . H6E H 0.5203 0.4434 0.2567 0.261 Uiso 1 1 calc R . . H6F H 0.5682 0.3456 0.2240 0.261 Uiso 1 1 calc R . . H6G H 0.6426 0.4304 0.2520 0.261 Uiso 1 1 calc R . . C7 C 0.6630(11) 0.2753(11) 0.4035(5) 0.174(2) Uiso 1 1 d D . . H7A H 0.6017 0.2315 0.4091 0.209 Uiso 1 1 calc R . . H7B H 0.7234 0.2318 0.4125 0.209 Uiso 1 1 calc R . . C8 C 0.6593(11) 0.3410(11) 0.4458(6) 0.174(2) Uiso 1 1 d D . . H8A H 0.6924 0.3131 0.4820 0.261 Uiso 1 1 calc R . . H8B H 0.5874 0.3573 0.4548 0.261 Uiso 1 1 calc R . . H8C H 0.6955 0.4030 0.4332 0.261 Uiso 1 1 calc R . . C9 C 0.7009(11) 0.1982(9) 0.3070(6) 0.174(2) Uiso 1 1 d D . . H9A H 0.7147 0.2142 0.2641 0.209 Uiso 1 1 calc R . . H9B H 0.7671 0.1766 0.3251 0.209 Uiso 1 1 calc R . . C10 C 0.6324(11) 0.1124(11) 0.3087(6) 0.174(2) Uiso 1 1 d D . . H10A H 0.6695 0.0509 0.2963 0.261 Uiso 1 1 calc R . . H10B H 0.5746 0.1243 0.2811 0.261 Uiso 1 1 calc R . . H10C H 0.6062 0.1034 0.3499 0.261 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 Ga1 0.0589(4) 0.0511(4) 0.0479(4) -0.0002(4) -0.0040(4) 0.0104(4) S1 0.049(10) 0.047(6) 0.029(5) 0.002(4) 0.005(6) 0.015(7) S1A 0.058(7) 0.078(8) 0.052(5) 0.012(4) 0.011(4) 0.015(5) S1B 0.062(8) 0.058(5) 0.054(7) 0.001(4) -0.008(6) 0.002(5) S2 0.0912(15) 0.0461(11) 0.0879(14) 0.0017(11) 0.0352(12) 0.0021(11) S3 0.0478(11) 0.0884(15) 0.0508(10) -0.0023(9) -0.0027(9) 0.0050(9) S4 0.0529(11) 0.0577(11) 0.0912(14) -0.0030(9) -0.0139(12) 0.0093(10) O2 0.083(4) 0.062(3) 0.068(3) -0.017(3) 0.013(3) 0.012(3) O3 0.052(3) 0.146(6) 0.073(4) -0.031(4) -0.014(3) 0.003(4) O4 0.063(3) 0.055(3) 0.069(3) 0.002(2) -0.022(3) -0.007(2) C1 0.095(6) 0.053(5) 0.077(6) -0.017(4) -0.022(5) 0.002(5) C2 0.058(5) 0.048(4) 0.048(4) 0.001(4) -0.011(4) -0.003(3) C3 0.051(4) 0.060(5) 0.066(5) -0.008(4) 0.005(4) 0.005(3) C4 0.051(4) 0.056(4) 0.042(4) 0.011(4) 0.001(4) 0.004(3) C1A 0.052(4) 0.055(5) 0.054(4) 0.002(4) -0.020(4) 0.002(4) C2A 0.066(5) 0.062(5) 0.056(4) 0.002(4) -0.010(4) 0.011(4) C3A 0.083(6) 0.057(5) 0.095(6) 0.000(5) -0.016(5) 0.014(4) C4A 0.069(6) 0.094(7) 0.078(6) 0.027(5) -0.016(5) 0.014(5) C5A 0.111(8) 0.111(8) 0.063(5) -0.006(6) -0.028(5) 0.030(6) C6A 0.132(8) 0.077(6) 0.083(6) -0.021(5) -0.051(6) 0.046(6) C1B 0.059(4) 0.043(4) 0.045(4) 0.003(3) -0.001(4) 0.007(3) C2B 0.063(5) 0.059(5) 0.058(5) 0.007(4) 0.003(4) -0.006(4) C3B 0.072(6) 0.085(6) 0.062(5) 0.006(4) 0.007(4) -0.001(5) C4B 0.079(6) 0.087(7) 0.114(8) 0.020(6) 0.019(6) -0.021(6) C5B 0.110(8) 0.078(6) 0.104(7) -0.003(5) -0.003(7) -0.030(6) C6B 0.085(6) 0.068(6) 0.084(6) -0.016(5) 0.012(5) -0.014(5) C1C 0.057(5) 0.044(4) 0.051(4) -0.002(3) 0.009(4) -0.001(3) C2C 0.060(5) 0.090(6) 0.061(5) -0.020(4) -0.004(4) 0.000(5) C3C 0.096(7) 0.111(7) 0.073(6) -0.032(5) -0.012(6) 0.005(7) C4C 0.122(9) 0.093(7) 0.074(7) -0.028(6) 0.025(7) 0.006(7) C5C 0.075(6) 0.107(7) 0.096(7) -0.018(6) 0.020(6) 0.016(6) C6C 0.063(5) 0.081(6) 0.066(5) -0.009(4) 0.005(4) 0.011(5) C1D 0.046(4) 0.048(4) 0.041(4) 0.007(3) 0.007(3) -0.004(3) C2D 0.047(4) 0.050(5) 0.056(5) 0.007(3) -0.001(3) -0.001(3) C3D 0.056(4) 0.057(5) 0.080(5) 0.007(4) 0.000(4) 0.004(4) C4D 0.092(6) 0.048(5) 0.092(6) -0.003(5) 0.023(5) 0.005(5) C5D 0.072(5) 0.062(5) 0.093(6) -0.017(5) -0.012(4) -0.009(5) C6D 0.056(5) 0.057(5) 0.067(4) 0.003(4) -0.010(4) -0.003(3) O5 0.095(4) 0.109(5) 0.132(6) -0.021(4) -0.001(4) -0.016(4) N1 0.072(4) 0.091(5) 0.079(4) 0.009(4) -0.005(4) 0.005(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 Ga1 S4 2.264(2) . ? Ga1 S2 2.270(2) . ? Ga1 S3 2.2749(19) . ? Ga1 S1B 2.281(12) . ? Ga1 S1A 2.282(12) . ? Ga1 S1 2.287(10) . ? S1 S1B 0.51(2) . ? S1 S1A 0.555(17) . ? S1 C1 1.688(13) . ? S1A S1B 1.03(2) . ? S1A C1 1.668(14) . ? S1B C1 1.683(14) . ? S2 C2 1.754(7) . ? S3 C3 1.747(7) . ? S4 C4 1.751(6) . ? O1 O1B 0.70(2) . ? O1 O1A 0.71(2) . ? O1 C1 1.291(13) . ? O1A C1 1.323(13) . ? O1A O1B 1.35(2) . ? O1B C1 1.273(13) . ? O2 C2 1.205(7) . ? O3 C3 1.206(8) . ? O4 C4 1.211(7) . ? C1 C1A 1.490(10) . ? C2 C1B 1.485(10) . ? C3 C1C 1.486(10) . ? C4 C1D 1.495(9) . ? C1A C6A 1.365(10) . ? C1A C2A 1.373(9) . ? C2A C3A 1.354(10) . ? C3A C4A 1.392(11) . ? C4A C5A 1.346(12) . ? C5A C6A 1.339(11) . ? C1B C6B 1.367(10) . ? C1B C2B 1.390(9) . ? C2B C3B 1.360(10) . ? C3B C4B 1.348(11) . ? C4B C5B 1.377(12) . ? C5B C6B 1.371(12) . ? C1C C6C 1.361(10) . ? C1C C2C 1.362(10) . ? C2C C3C 1.373(10) . ? C3C C4C 1.375(13) . ? C4C C5C 1.338(12) . ? C5C C6C 1.375(10) . ? C1D C2D 1.363(8) . ? C1D C6D 1.392(8) . ? C2D C3D 1.356(9) . ? C3D C4D 1.378(10) . ? C4D C5D 1.357(10) . ? C5D C6D 1.364(10) . ? N1 C5 1.405(11) . ? N1 C7 1.448(11) . ? N1 C9 1.490(11) . ? C5 C6 1.381(12) . ? C7 C8 1.250(12) . ? C9 C10 1.408(13) . ? 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 S4 Ga1 S2 105.47(8) . . ? S4 Ga1 S3 114.86(8) . . ? S2 Ga1 S3 109.17(8) . . ? S4 Ga1 S1B 119.7(3) . . ? S2 Ga1 S1B 95.9(4) . . ? S3 Ga1 S1B 109.5(3) . . ? S4 Ga1 S1A 104.5(3) . . ? S2 Ga1 S1A 121.6(3) . . ? S3 Ga1 S1A 101.7(3) . . ? S1B Ga1 S1A 26.1(6) . . ? S4 Ga1 S1 115.3(3) . . ? S2 Ga1 S1 108.6(3) . . ? S3 Ga1 S1 103.3(3) . . ? S1B Ga1 S1 12.8(5) . . ? S1A Ga1 S1 14.0(4) . . ? S1B S1 S1A 150(4) . . ? S1B S1 C1 81(2) . . ? S1A S1 C1 78.4(19) . . ? S1B S1 Ga1 83(2) . . ? S1A S1 Ga1 82.5(18) . . ? C1 S1 Ga1 105.2(6) . . ? S1 S1A S1B 14.1(18) . . ? S1 S1A C1 82.5(18) . . ? S1B S1A C1 72.9(10) . . ? S1 S1A Ga1 83.5(18) . . ? S1B S1A Ga1 76.9(11) . . ? C1 S1A Ga1 106.1(7) . . ? S1 S1B S1A 15(2) . . ? S1 S1B C1 82(2) . . ? S1A S1B C1 71.3(11) . . ? S1 S1B Ga1 84(2) . . ? S1A S1B Ga1 77.0(11) . . ? C1 S1B Ga1 105.6(7) . . ? C2 S2 Ga1 100.5(3) . . ? C3 S3 Ga1 99.4(3) . . ? C4 S4 Ga1 98.0(2) . . ? O1B O1 O1A 146(3) . . ? O1B O1 C1 72.8(14) . . ? O1A O1 C1 76.8(14) . . ? O1 O1A C1 71.8(14) . . ? O1 O1A O1B 17.0(14) . . ? C1 O1A O1B 57.0(7) . . ? O1 O1B C1 75.6(14) . . ? O1 O1B O1A 17.3(15) . . ? C1 O1B O1A 60.6(8) . . ? O1B C1 O1 31.6(9) . . ? O1B C1 O1A 62.4(10) . . ? O1 C1 O1A 31.5(9) . . ? O1B C1 C1A 118.4(9) . . ? O1 C1 C1A 116.0(10) . . ? O1A C1 C1A 113.9(9) . . ? O1B C1 S1A 100.9(9) . . ? O1 C1 S1A 119.9(11) . . ? O1A C1 S1A 122.8(10) . . ? C1A C1 S1A 121.3(7) . . ? O1B C1 S1B 124.4(10) . . ? O1 C1 S1B 124.4(10) . . ? O1A C1 S1B 106.5(9) . . ? C1A C1 S1B 115.6(7) . . ? S1A C1 S1B 35.8(8) . . ? O1B C1 S1 116.5(10) . . ? O1 C1 S1 127.5(10) . . ? O1A C1 S1 118.3(9) . . ? C1A C1 S1 116.4(6) . . ? S1A C1 S1 19.0(6) . . ? S1B C1 S1 17.4(7) . . ? O2 C2 C1B 121.7(6) . . ? O2 C2 S2 122.7(6) . . ? C1B C2 S2 115.6(5) . . ? O3 C3 C1C 121.7(6) . . ? O3 C3 S3 122.3(6) . . ? C1C C3 S3 116.0(6) . . ? O4 C4 C1D 120.7(6) . . ? O4 C4 S4 123.0(5) . . ? C1D C4 S4 116.3(5) . . ? C6A C1A C2A 118.1(7) . . ? C6A C1A C1 119.9(7) . . ? C2A C1A C1 121.9(6) . . ? C3A C2A C1A 120.3(7) . . ? C2A C3A C4A 120.2(8) . . ? C5A C4A C3A 118.8(8) . . ? C6A C5A C4A 120.6(8) . . ? C5A C6A C1A 121.9(8) . . ? C6B C1B C2B 119.6(7) . . ? C6B C1B C2 117.6(7) . . ? C2B C1B C2 122.9(7) . . ? C3B C2B C1B 119.5(7) . . ? C4B C3B C2B 122.4(8) . . ? C3B C4B C5B 117.3(8) . . ? C6B C5B C4B 122.5(9) . . ? C1B C6B C5B 118.6(8) . . ? C6C C1C C2C 118.1(7) . . ? C6C C1C C3 117.4(7) . . ? C2C C1C C3 124.4(7) . . ? C1C C2C C3C 121.5(8) . . ? C2C C3C C4C 118.6(9) . . ? C5C C4C C3C 120.8(8) . . ? C4C C5C C6C 119.5(9) . . ? C1C C6C C5C 121.3(8) . . ? C2D C1D C6D 119.4(6) . . ? C2D C1D C4 118.4(6) . . ? C6D C1D C4 122.2(6) . . ? C3D C2D C1D 120.9(7) . . ? C2D C3D C4D 119.6(7) . . ? C5D C4D C3D 120.1(7) . . ? C4D C5D C6D 120.7(7) . . ? C5D C6D C1D 119.3(7) . . ? C5 N1 C7 115.1(8) . . ? C5 N1 C9 113.7(8) . . ? C7 N1 C9 107.1(8) . . ? C6 C5 N1 123.2(12) . . ? C8 C7 N1 126.6(14) . . ? C10 C9 N1 118.7(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.438 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.063