Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_tcd27 _database_code_CSD 183392 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Ming Lin' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117 543 ; 'Kian Ping Loh' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117 543 ; 'Theivanayagam C. Deivaraj' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117 543 ; 'Vittal, Jagadese J.' ; Department of Chemistry National University of Singapore 3 Science Drive 3 SINGAPORE 117 543 ; _publ_contact_author_name 'Prof Jagadese Vittal' _publ_contact_author_address ; Chemistry 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 _publ_requested_journal 'Chemical Communications.' _publ_requested_coeditor_name '?' _publ_contact_letter ; Please consider this CIF submission for publication in Chemical Communications ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Heterogenous Reaction Route to CuInS2 Thin Films ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #============================================================================== # 4. TEXT #============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== # 5. CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 In N O5 S4' _chemical_formula_weight 783.71 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' 'In' 'In' -0.7276 1.3100 '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 12.9124(6) _cell_length_b 12.9187(7) _cell_length_c 21.5610(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3596.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6257 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'hexagonal cylinder' _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.929 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4669 _exptl_absorpt_correction_T_max 0.9011 _exptl_absorpt_process_details 'sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 18849 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6331 _reflns_number_gt 5623 _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^)+(0.0569P)^2^+1.8450P] 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 SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 6331 _refine_ls_number_parameters 407 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.053 _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 0.78965(3) 0.78062(3) 0.685011(17) 0.04111(13) Uani 1 1 d . . . S1 S 0.70051(18) 0.93354(12) 0.64172(9) 0.0747(6) Uani 1 1 d . . . S2 S 0.95762(12) 0.77517(12) 0.62921(8) 0.0602(4) Uani 1 1 d . . . S3 S 0.81535(10) 0.82233(13) 0.79599(7) 0.0502(4) Uani 1 1 d . . . S4 S 0.71358(12) 0.60873(10) 0.66519(8) 0.0537(4) Uani 1 1 d . . . O1 O 0.6247(6) 0.7911(4) 0.5729(3) 0.126(3) Uani 1 1 d . . . O2 O 0.9403(3) 0.9626(3) 0.67445(19) 0.0530(10) Uani 1 1 d . . . O3 O 0.6171(3) 0.8011(4) 0.77282(19) 0.0652(13) Uani 1 1 d . . . O4 O 0.8977(3) 0.5828(3) 0.71391(19) 0.0517(10) Uani 1 1 d . . . C1 C 0.6301(5) 0.8822(4) 0.5826(3) 0.0530(15) Uani 1 1 d . . . C2 C 0.9868(4) 0.9069(4) 0.6393(3) 0.0446(13) Uani 1 1 d . . . C3 C 0.6820(4) 0.8230(4) 0.8123(3) 0.0413(11) Uani 1 1 d . . . C4 C 0.8240(4) 0.5395(4) 0.6903(3) 0.0384(11) Uani 1 1 d . . . C1A C 0.5766(4) 0.9592(4) 0.5409(3) 0.0446(13) Uani 1 1 d . . . C2A C 0.5556(5) 1.0589(4) 0.5601(3) 0.0521(15) Uani 1 1 d . . . H2A H 0.5720 1.0802 0.6006 0.063 Uiso 1 1 calc R . . C3A C 0.5093(5) 1.1280(5) 0.5183(3) 0.0608(17) Uani 1 1 d . . . H3A H 0.4924 1.1951 0.5316 0.073 Uiso 1 1 calc R . . C4A C 0.4889(5) 1.1002(6) 0.4598(3) 0.0610(17) Uani 1 1 d . . . H4A H 0.4600 1.1487 0.4323 0.073 Uiso 1 1 calc R . . C5A C 0.5098(5) 1.0006(6) 0.4394(3) 0.0688(19) Uani 1 1 d . . . H5A H 0.4964 0.9806 0.3982 0.083 Uiso 1 1 calc R . . C6A C 0.5517(6) 0.9309(5) 0.4823(3) 0.0663(19) Uani 1 1 d . . . H6A H 0.5629 0.8620 0.4700 0.080 Uiso 1 1 calc R . . C1B C 1.0779(4) 0.9458(4) 0.6025(3) 0.0402(12) Uani 1 1 d . . . C2B C 1.1115(4) 0.8995(4) 0.5483(3) 0.0468(13) Uani 1 1 d . . . H2B H 1.0783 0.8395 0.5338 0.056 Uiso 1 1 calc R . . C3B C 1.1939(5) 0.9408(5) 0.5151(3) 0.0596(17) Uani 1 1 d . . . H3B H 1.2158 0.9092 0.4781 0.072 Uiso 1 1 calc R . . C4B C 1.2429(5) 1.0273(6) 0.5364(4) 0.075(2) Uani 1 1 d . . . H4B H 1.2988 1.0554 0.5141 0.090 Uiso 1 1 calc R . . C5B C 1.2110(7) 1.0733(6) 0.5901(4) 0.081(2) Uani 1 1 d . . . H5B H 1.2459 1.1326 0.6044 0.097 Uiso 1 1 calc R . . C6B C 1.1285(5) 1.0346(5) 0.6241(3) 0.0605(16) Uani 1 1 d . . . H6B H 1.1070 1.0673 0.6609 0.073 Uiso 1 1 calc R . . C1C C 0.6503(4) 0.8539(4) 0.8759(3) 0.0420(13) Uani 1 1 d . . . C2C C 0.7194(5) 0.8583(4) 0.9255(2) 0.0468(13) Uani 1 1 d . . . H2C H 0.7901 0.8449 0.9190 0.056 Uiso 1 1 calc R . . C3C C 0.6842(6) 0.8822(5) 0.9844(3) 0.0621(18) Uani 1 1 d . . . H3C H 0.7303 0.8817 1.0181 0.074 Uiso 1 1 calc R . . C4C C 0.5834(6) 0.9064(5) 0.9935(4) 0.071(2) Uani 1 1 d . . . H4C H 0.5607 0.9267 1.0331 0.085 Uiso 1 1 calc R . . C5C C 0.5142(5) 0.9016(5) 0.9453(3) 0.0602(17) Uani 1 1 d . . . H5C H 0.4440 0.9167 0.9525 0.072 Uiso 1 1 calc R . . C6C C 0.5461(4) 0.8751(5) 0.8872(3) 0.0523(15) Uani 1 1 d . . . H6C H 0.4978 0.8711 0.8547 0.063 Uiso 1 1 calc R . . C1D C 0.8245(4) 0.4252(4) 0.6788(2) 0.0350(11) Uani 1 1 d . . . C2D C 0.9037(4) 0.3671(4) 0.7042(2) 0.0395(12) Uani 1 1 d . . . H2D H 0.9551 0.3997 0.7281 0.047 Uiso 1 1 calc R . . C3D C 0.9079(4) 0.2609(4) 0.6947(3) 0.0473(13) Uani 1 1 d . . . H3D H 0.9613 0.2216 0.7126 0.057 Uiso 1 1 calc R . . C4D C 0.8332(5) 0.2128(5) 0.6587(3) 0.0570(15) Uani 1 1 d . . . H4D H 0.8362 0.1410 0.6520 0.068 Uiso 1 1 calc R . . C5D C 0.7549(4) 0.2698(5) 0.6329(3) 0.0550(14) Uani 1 1 d . . . H5D H 0.7045 0.2371 0.6083 0.066 Uiso 1 1 calc R . . C6D C 0.7500(4) 0.3761(4) 0.6429(3) 0.0461(13) Uani 1 1 d . . . H6D H 0.6959 0.4149 0.6253 0.055 Uiso 1 1 calc R . . O5 O 0.1637(5) 0.5922(4) 0.6868(3) 0.1016(18) Uani 1 1 d . . . N1 N 0.3420(4) 0.7146(4) 0.6581(2) 0.0609(13) Uani 1 1 d D . . H1 H 0.2897 0.6666 0.6615 0.073 Uiso 1 1 calc R . . C5 C 0.4364(6) 0.6653(6) 0.6820(4) 0.096(3) Uani 1 1 d D . . H5E H 0.4926 0.7162 0.6805 0.115 Uiso 1 1 calc R . . H5F H 0.4551 0.6086 0.6540 0.115 Uiso 1 1 calc R . . C6 C 0.4307(7) 0.6235(8) 0.7458(4) 0.106(3) Uani 1 1 d D . . H6E H 0.4966 0.5927 0.7568 0.159 Uiso 1 1 calc R . . H6F H 0.3768 0.5713 0.7479 0.159 Uiso 1 1 calc R . . H6G H 0.4148 0.6791 0.7745 0.159 Uiso 1 1 calc R . . C7 C 0.3506(10) 0.7422(9) 0.5906(4) 0.150(5) Uani 1 1 d D . . H7A H 0.2995 0.7964 0.5817 0.180 Uiso 1 1 calc R . . H7B H 0.4193 0.7722 0.5836 0.180 Uiso 1 1 calc R . . C8 C 0.3360(12) 0.6608(10) 0.5468(5) 0.164(6) Uani 1 1 d D . . H8A H 0.3438 0.6879 0.5051 0.245 Uiso 1 1 calc R . . H8B H 0.2671 0.6320 0.5517 0.245 Uiso 1 1 calc R . . H8C H 0.3871 0.6071 0.5539 0.245 Uiso 1 1 calc R . . C9 C 0.3075(5) 0.8091(5) 0.6930(4) 0.084(2) Uani 1 1 d D . . H9A H 0.2430 0.8345 0.6745 0.101 Uiso 1 1 calc R . . H9B H 0.2924 0.7895 0.7359 0.101 Uiso 1 1 calc R . . C10 C 0.3844(6) 0.8942(6) 0.6931(5) 0.096(3) Uani 1 1 d D . . H10A H 0.3570 0.9525 0.7163 0.144 Uiso 1 1 calc R . . H10B H 0.3985 0.9154 0.6508 0.144 Uiso 1 1 calc R . . H10C H 0.4480 0.8704 0.7124 0.144 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 0.0451(2) 0.03501(19) 0.0432(2) 0.00148(16) -0.00048(17) 0.00599(18) S1 0.1039(14) 0.0427(8) 0.0774(12) -0.0081(8) -0.0464(12) 0.0203(10) S2 0.0707(9) 0.0301(7) 0.0797(10) 0.0009(8) 0.0317(8) 0.0008(8) S3 0.0394(7) 0.0664(9) 0.0449(8) -0.0042(7) 0.0028(5) 0.0061(6) S4 0.0426(7) 0.0362(7) 0.0824(11) 0.0021(6) -0.0024(8) 0.0057(7) O1 0.196(7) 0.032(3) 0.151(5) -0.007(3) -0.105(5) 0.020(4) O2 0.050(2) 0.050(2) 0.059(3) -0.010(2) 0.000(2) 0.0076(18) O3 0.044(2) 0.094(4) 0.057(2) -0.026(2) -0.0130(19) 0.010(2) O4 0.059(2) 0.033(2) 0.063(2) 0.0019(18) -0.019(2) -0.0097(19) C1 0.057(4) 0.031(3) 0.071(4) 0.001(3) -0.010(3) 0.004(3) C2 0.054(3) 0.033(3) 0.046(3) 0.004(3) -0.001(3) 0.009(3) C3 0.038(3) 0.041(3) 0.045(3) -0.001(3) -0.003(2) 0.002(2) C4 0.049(3) 0.030(2) 0.036(3) 0.003(2) 0.001(2) -0.001(2) C1A 0.041(3) 0.036(3) 0.057(4) 0.002(3) -0.012(3) -0.002(2) C2A 0.057(4) 0.038(3) 0.062(4) 0.000(3) -0.017(3) -0.002(3) C3A 0.058(4) 0.038(3) 0.087(5) 0.007(3) -0.011(3) 0.009(3) C4A 0.044(3) 0.069(4) 0.071(5) 0.018(4) -0.013(3) 0.010(3) C5A 0.074(4) 0.075(5) 0.058(4) -0.002(4) -0.024(4) 0.022(4) C6A 0.083(5) 0.043(3) 0.073(5) -0.012(3) -0.026(4) 0.018(3) C1B 0.040(3) 0.035(3) 0.045(3) 0.009(2) -0.002(2) 0.008(2) C2B 0.050(3) 0.041(3) 0.049(3) 0.006(3) 0.001(3) 0.003(3) C3B 0.061(4) 0.067(4) 0.051(4) 0.018(3) 0.007(3) 0.015(3) C4B 0.063(4) 0.071(5) 0.092(6) 0.029(4) 0.005(4) -0.017(4) C5B 0.076(5) 0.063(4) 0.103(6) 0.008(4) -0.013(5) -0.025(4) C6B 0.064(4) 0.046(4) 0.071(4) -0.003(3) -0.007(3) -0.002(3) C1C 0.041(3) 0.033(3) 0.052(3) -0.002(2) 0.003(2) -0.004(2) C2C 0.041(3) 0.053(3) 0.047(3) -0.008(2) 0.004(3) -0.002(3) C3C 0.078(5) 0.059(4) 0.049(4) -0.008(3) -0.003(3) 0.000(3) C4C 0.085(5) 0.061(4) 0.067(5) -0.015(4) 0.027(4) 0.006(4) C5C 0.056(4) 0.054(4) 0.070(4) -0.011(3) 0.019(3) 0.006(3) C6C 0.040(3) 0.051(4) 0.066(4) -0.005(3) 0.004(3) 0.003(3) C1D 0.034(2) 0.031(2) 0.040(3) 0.006(2) 0.005(2) -0.0026(19) C2D 0.034(3) 0.037(3) 0.047(3) 0.003(2) -0.002(2) -0.004(2) C3D 0.047(3) 0.038(3) 0.057(3) 0.003(3) 0.006(3) 0.004(2) C4D 0.070(4) 0.026(3) 0.075(4) -0.007(3) 0.016(3) -0.008(3) C5D 0.056(3) 0.040(3) 0.068(4) -0.008(3) -0.004(3) -0.011(3) C6D 0.043(3) 0.042(3) 0.053(3) 0.001(3) -0.006(2) -0.005(2) O5 0.089(4) 0.081(4) 0.136(5) -0.027(4) -0.012(4) -0.004(3) N1 0.060(3) 0.056(3) 0.067(3) -0.008(3) 0.002(2) 0.006(3) C5 0.077(5) 0.069(5) 0.142(8) 0.019(6) 0.001(6) 0.018(4) C6 0.083(6) 0.120(8) 0.116(7) 0.065(6) -0.003(5) 0.002(5) C7 0.168(11) 0.149(13) 0.134(10) 0.018(9) -0.013(9) 0.031(9) C8 0.236(16) 0.134(10) 0.120(9) -0.070(8) -0.011(9) 0.006(10) C9 0.071(5) 0.059(4) 0.123(7) 0.000(4) 0.023(5) 0.016(3) C10 0.075(5) 0.061(5) 0.151(8) -0.025(5) 0.005(6) -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 In1 S4 2.4654(15) . ? In1 S1 2.4696(16) . ? In1 S3 2.4751(14) . ? In1 S2 2.4812(15) . ? S1 C1 1.700(6) . ? S2 C2 1.756(6) . ? S3 C3 1.757(5) . ? S4 C4 1.769(5) . ? O1 C1 1.198(8) . ? O2 C2 1.205(6) . ? O3 C3 1.228(6) . ? O4 C4 1.216(6) . ? C1 C1A 1.508(8) . ? C2 C1B 1.506(8) . ? C3 C1C 1.486(8) . ? C4 C1D 1.497(7) . ? C1A C6A 1.354(8) . ? C1A C2A 1.380(8) . ? C2A C3A 1.402(8) . ? C3A C4A 1.336(9) . ? C4A C5A 1.387(10) . ? C5A C6A 1.400(9) . ? C1B C2B 1.383(8) . ? C1B C6B 1.401(8) . ? C2B C3B 1.388(8) . ? C3B C4B 1.365(10) . ? C4B C5B 1.365(11) . ? C5B C6B 1.386(10) . ? C1C C2C 1.394(8) . ? C1C C6C 1.395(8) . ? C2C C3C 1.383(8) . ? C3C C4C 1.352(10) . ? C4C C5C 1.371(10) . ? C5C C6C 1.362(9) . ? C1D C2D 1.381(7) . ? C1D C6D 1.388(7) . ? C2D C3D 1.389(8) . ? C3D C4D 1.384(8) . ? C4D C5D 1.368(9) . ? C5D C6D 1.392(8) . ? N1 C5 1.467(8) . ? N1 C9 1.502(7) . ? N1 C7 1.504(10) . ? C5 C6 1.480(10) . ? C7 C8 1.425(12) . ? C9 C10 1.482(9) . ? 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 In1 S1 117.99(6) . . ? S4 In1 S3 114.65(6) . . ? S1 In1 S3 104.70(6) . . ? S4 In1 S2 103.81(5) . . ? S1 In1 S2 104.29(7) . . ? S3 In1 S2 110.97(5) . . ? C1 S1 In1 102.7(2) . . ? C2 S2 In1 95.7(2) . . ? C3 S3 In1 93.62(19) . . ? C4 S4 In1 94.67(18) . . ? O1 C1 C1A 121.2(6) . . ? O1 C1 S1 123.0(5) . . ? C1A C1 S1 115.8(4) . . ? O2 C2 C1B 121.4(5) . . ? O2 C2 S2 123.4(5) . . ? C1B C2 S2 115.2(4) . . ? O3 C3 C1C 120.9(4) . . ? O3 C3 S3 121.9(4) . . ? C1C C3 S3 117.1(4) . . ? O4 C4 C1D 121.3(5) . . ? O4 C4 S4 121.8(4) . . ? C1D C4 S4 116.9(4) . . ? C6A C1A C2A 119.0(5) . . ? C6A C1A C1 119.2(5) . . ? C2A C1A C1 121.8(5) . . ? C1A C2A C3A 119.1(6) . . ? C4A C3A C2A 121.3(6) . . ? C3A C4A C5A 120.7(6) . . ? C4A C5A C6A 117.5(6) . . ? C1A C6A C5A 122.4(6) . . ? C2B C1B C6B 119.3(5) . . ? C2B C1B C2 123.1(5) . . ? C6B C1B C2 117.6(5) . . ? C1B C2B C3B 120.7(6) . . ? C4B C3B C2B 119.7(6) . . ? C3B C4B C5B 120.1(7) . . ? C4B C5B C6B 121.6(7) . . ? C5B C6B C1B 118.5(6) . . ? C2C C1C C6C 118.4(5) . . ? C2C C1C C3 122.9(5) . . ? C6C C1C C3 118.7(5) . . ? C3C C2C C1C 120.2(6) . . ? C4C C3C C2C 120.0(7) . . ? C3C C4C C5C 120.5(6) . . ? C6C C5C C4C 120.7(6) . . ? C5C C6C C1C 120.1(6) . . ? C2D C1D C6D 119.0(5) . . ? C2D C1D C4 118.3(5) . . ? C6D C1D C4 122.7(5) . . ? C1D C2D C3D 120.5(5) . . ? C4D C3D C2D 119.9(5) . . ? C5D C4D C3D 120.1(5) . . ? C4D C5D C6D 120.1(5) . . ? C1D C6D C5D 120.4(5) . . ? C5 N1 C9 115.1(6) . . ? C5 N1 C7 112.5(6) . . ? C9 N1 C7 108.2(6) . . ? N1 C5 C6 116.3(7) . . ? C8 C7 N1 117.1(10) . . ? C10 C9 N1 113.9(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.791 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.078