# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'M. Lappert' 'Peter B Hitchcock' 'Andrey V Protchenko' 'Patrick G. H. Uiterweerd' _publ_contact_author_name 'Prof M Lappert ' _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis and structures of halides and pseudohalides of bis[2,6-bis(dimethylamino)phenyl]tin(IV) ; _publ_requested_category FM # Attachment 'mfl_30july2008.cif' data_(2)-may798 _database_code_depnum_ccdc_archive 'CCDC 697226' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H15 Cl N2 Sn' _chemical_formula_sum 'C10 H15 Cl N2 Sn' _chemical_formula_weight 317.38 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' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 '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(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 8.135(1) _cell_length_b 9.190(1) _cell_length_c 15.934(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.12(2) _cell_angle_gamma 90.00 _cell_volume 1191.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.3 _cell_measurement_theta_max 8.5 _cell_measurement_wavelength 0.71073 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 2.335 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 1 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7 _diffrn_standards_decay_corr_max 1.073 _diffrn_standards_decay_corr_min 0.996 _diffrn_reflns_number 5499 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 34.97 _diffrn_reflns_theta_full 34.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5220 _reflns_number_observed 4105 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The diffraction data showed systematic absences of h0l for l odd, but the 0k0 reflections showed weak but significant intensity for the 030,050, and 070 reflections. The structure was initially solved in space group Pc but, since it clearly corresponded to spacegroup P2(1)/c, it was changed to the latter space group for the final refinement. There were no differences in the molecular geometry between the two different refinements.(For comparison the final wR2 for all data in Pc was 0.136) Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+4.7162P] 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 SHELXL _refine_ls_extinction_coef 0.0041(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5220 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_obs 0.0598 _refine_ls_wR_factor_all 0.1442 _refine_ls_wR_factor_obs 0.1352 _refine_ls_goodness_of_fit_all 1.150 _refine_ls_goodness_of_fit_obs 1.218 _refine_ls_restrained_S_all 1.150 _refine_ls_restrained_S_obs 1.218 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sn Sn 0.06321(4) 0.20329(3) 0.01735(2) 0.02328(9) Uani 1 d . . Cl Cl 0.32311(15) 0.10480(13) 0.08090(7) 0.0298(2) Uani 1 d . . N1 N 0.1471(5) 0.1697(4) -0.1240(2) 0.0244(7) Uani 1 d . . N2 N 0.2384(5) 0.5982(4) 0.0458(2) 0.0244(7) Uani 1 d . . C1 C 0.1885(5) 0.3843(4) -0.0445(3) 0.0205(7) Uani 1 d . . C2 C 0.2014(5) 0.3218(5) -0.1231(3) 0.0220(7) Uani 1 d . . C3 C 0.2673(6) 0.3901(6) -0.1921(3) 0.0290(9) Uani 1 d . . H3 H 0.2754 0.3426 -0.2448 0.035 Uiso 1 calc R . C4 C 0.3212(6) 0.5332(6) -0.1797(3) 0.0335(10) Uani 1 d . . H4 H 0.3640 0.5859 -0.2257 0.040 Uiso 1 calc R . C5 C 0.3134(6) 0.5997(5) -0.1017(3) 0.0283(9) Uani 1 d . . H5 H 0.3536 0.6962 -0.0949 0.034 Uiso 1 calc R . C6 C 0.2473(5) 0.5270(5) -0.0328(3) 0.0220(7) Uani 1 d . . C7 C 0.2835(6) 0.0673(5) -0.1382(3) 0.0302(9) Uani 1 d . . H7A H 0.2414 -0.0326 -0.1383 0.045 Uiso 1 calc R . H7B H 0.3667 0.0782 -0.0933 0.045 Uiso 1 calc R . H7C H 0.3331 0.0884 -0.1924 0.045 Uiso 1 calc R . C8 C 0.0112(6) 0.1425(6) -0.1851(3) 0.0341(10) Uani 1 d . . H8A H -0.0202 0.0396 -0.1832 0.051 Uiso 1 calc R . H8B H 0.0474 0.1669 -0.2417 0.051 Uiso 1 calc R . H8C H -0.0835 0.2030 -0.1710 0.051 Uiso 1 calc R . C9 C 0.2074(6) 0.5040(5) 0.1167(3) 0.0286(9) Uani 1 d . . H9A H 0.2033 0.5625 0.1681 0.043 Uiso 1 calc R . H9B H 0.2957 0.4320 0.1222 0.043 Uiso 1 calc R . H9C H 0.1021 0.4540 0.1079 0.043 Uiso 1 calc R . C10 C 0.3621(6) 0.7111(5) 0.0622(4) 0.0320(9) Uani 1 d . . H10A H 0.3452 0.7532 0.1178 0.048 Uiso 1 calc R . H10B H 0.3516 0.7874 0.0195 0.048 Uiso 1 calc R . H10C H 0.4722 0.6681 0.0602 0.048 Uiso 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 Sn 0.02186(14) 0.02232(13) 0.02582(14) 0.00029(11) 0.00471(9) -0.00309(11) Cl 0.0307(5) 0.0274(5) 0.0312(5) 0.0022(4) -0.0015(4) 0.0043(4) N1 0.0207(15) 0.027(2) 0.026(2) -0.0045(13) -0.0001(12) -0.0003(13) N2 0.025(2) 0.0171(14) 0.031(2) 0.0003(13) -0.0003(13) -0.0045(13) C1 0.0150(14) 0.021(2) 0.025(2) 0.0018(14) 0.0012(12) 0.0001(13) C2 0.019(2) 0.024(2) 0.022(2) 0.0015(13) 0.0000(13) 0.0001(13) C3 0.028(2) 0.037(2) 0.023(2) 0.004(2) 0.0030(15) 0.001(2) C4 0.030(2) 0.041(3) 0.030(2) 0.014(2) 0.006(2) 0.001(2) C5 0.026(2) 0.026(2) 0.033(2) 0.009(2) 0.003(2) -0.001(2) C6 0.017(2) 0.022(2) 0.027(2) 0.0036(14) -0.0005(13) -0.0008(13) C7 0.028(2) 0.027(2) 0.036(2) -0.006(2) 0.005(2) 0.006(2) C8 0.028(2) 0.040(3) 0.034(2) -0.008(2) -0.005(2) -0.004(2) C9 0.038(2) 0.023(2) 0.025(2) -0.001(2) -0.001(2) 0.002(2) C10 0.023(2) 0.024(2) 0.049(3) -0.006(2) 0.000(2) -0.005(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 Sn C1 2.194(4) . ? Sn N1 2.386(4) . ? Sn Cl 2.4962(12) . ? N1 C2 1.467(6) . ? N1 C7 1.476(6) . ? N1 C8 1.480(6) . ? N2 C6 1.416(6) . ? N2 C9 1.450(6) . ? N2 C10 1.465(6) . ? C1 C2 1.383(6) . ? C1 C6 1.407(6) . ? C2 C3 1.384(6) . ? C3 C4 1.399(8) . ? C4 C5 1.388(7) . ? C5 C6 1.401(6) . ? 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 Sn N1 61.99(14) . . ? C1 Sn Cl 93.43(11) . . ? N1 Sn Cl 94.61(10) . . ? C2 N1 C7 112.4(4) . . ? C2 N1 C8 112.8(4) . . ? C7 N1 C8 110.2(4) . . ? C2 N1 Sn 87.6(2) . . ? C7 N1 Sn 117.2(3) . . ? C8 N1 Sn 114.8(3) . . ? C6 N2 C9 115.3(3) . . ? C6 N2 C10 116.0(4) . . ? C9 N2 C10 114.4(4) . . ? C2 C1 C6 118.3(4) . . ? C2 C1 Sn 97.8(3) . . ? C6 C1 Sn 143.8(3) . . ? C1 C2 C3 124.7(4) . . ? C1 C2 N1 112.1(4) . . ? C3 C2 N1 123.1(4) . . ? C2 C3 C4 116.1(4) . . ? C5 C4 C3 121.4(4) . . ? C4 C5 C6 121.1(4) . . ? C5 C6 C1 118.4(4) . . ? C5 C6 N2 120.0(4) . . ? C1 C6 N2 121.6(4) . . ? _refine_diff_density_max 3.227 _refine_diff_density_min -1.893 _refine_diff_density_rms 0.188 #===END data_(4)-mar2900 _database_code_depnum_ccdc_archive 'CCDC 697227' _audit_creation_date 2000-03-17T15:08:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H30 Cl2 N4 Sn' _chemical_formula_sum 'C20 H30 Cl2 N4 Sn' _chemical_formula_weight 516.07 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.2558(4) _cell_length_b 17.2642(4) _cell_length_c 7.9120(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2220.45(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10750 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.798 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18152 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5153 _reflns_number_gt 4572 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0300P)^2^+1.4495P] 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_number_reflns 5153 _refine_ls_number_parameters 244 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.067 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(3) _refine_diff_density_max 0.444 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sn Sn 0.250947(10) 0.411603(9) 0.26433(7) 0.01861(5) Uani 1 1 d . . . Cl1 Cl 0.23272(5) 0.53126(5) 0.11161(10) 0.02945(15) Uani 1 1 d . . . Cl2 Cl 0.21403(5) 0.33840(5) 0.01957(10) 0.03200(16) Uani 1 1 d . . . N1 N 0.25198(14) 0.28323(16) 0.4306(4) 0.0261(6) Uani 1 1 d . . . N2 N 0.04995(16) 0.48919(18) 0.4137(4) 0.0328(6) Uani 1 1 d . . . N3 N 0.31644(13) 0.50928(13) 0.5053(3) 0.0218(5) Uani 1 1 d . . . N4 N 0.43194(15) 0.31300(14) 0.1381(3) 0.0249(5) Uani 1 1 d . . . C1 C 0.15155(17) 0.38362(18) 0.4302(4) 0.0232(6) Uani 1 1 d . . . C2 C 0.17250(19) 0.31091(18) 0.4895(4) 0.0262(6) Uani 1 1 d . . . C3 C 0.1206(2) 0.2678(2) 0.5934(4) 0.0385(8) Uani 1 1 d . . . H3 H 0.1376 0.2195 0.6392 0.046 Uiso 1 1 calc R . . C4 C 0.0436(2) 0.2975(2) 0.6275(5) 0.0426(9) Uani 1 1 d . . . H4 H 0.0061 0.2683 0.6937 0.051 Uiso 1 1 calc R . . C5 C 0.0205(2) 0.3690(2) 0.5672(4) 0.0379(8) Uani 1 1 d . . . H5 H -0.0333 0.3875 0.5914 0.045 Uiso 1 1 calc R . . C6 C 0.07346(19) 0.41531(18) 0.4716(4) 0.0272(7) Uani 1 1 d . . . C7 C 0.2459(2) 0.2098(2) 0.3346(6) 0.0368(8) Uani 1 1 d . . . H7A H 0.3009 0.1936 0.2985 0.055 Uiso 1 1 calc R . . H7B H 0.211 0.2176 0.2351 0.055 Uiso 1 1 calc R . . H7C H 0.2218 0.1697 0.4068 0.055 Uiso 1 1 calc R . . C8 C 0.3117(2) 0.2739(2) 0.5681(5) 0.0399(9) Uani 1 1 d . . . H8A H 0.3639 0.255 0.522 0.06 Uiso 1 1 calc R . . H8B H 0.2905 0.2365 0.6505 0.06 Uiso 1 1 calc R . . H8C H 0.3205 0.3239 0.6238 0.06 Uiso 1 1 calc R . . C9 C 0.1047(2) 0.5526(2) 0.4560(5) 0.0344(7) Uani 1 1 d . . . H9A H 0.0824 0.601 0.4106 0.052 Uiso 1 1 calc R . . H9B H 0.159 0.5429 0.407 0.052 Uiso 1 1 calc R . . H9C H 0.1095 0.5566 0.5792 0.052 Uiso 1 1 calc R . . C10 C -0.0358(2) 0.5115(3) 0.4416(5) 0.0517(12) Uani 1 1 d . . . H10A H -0.045 0.5638 0.3974 0.078 Uiso 1 1 calc R . . H10B H -0.0478 0.5106 0.563 0.078 Uiso 1 1 calc R . . H10C H -0.0721 0.4749 0.3831 0.078 Uiso 1 1 calc R . . C11 C 0.37873(16) 0.41444(15) 0.3240(4) 0.0183(5) Uani 1 1 d . . . C12 C 0.38877(16) 0.46397(16) 0.4611(4) 0.0200(5) Uani 1 1 d . . . C13 C 0.46230(17) 0.46734(17) 0.5513(4) 0.0252(6) Uani 1 1 d . . . H13 H 0.4687 0.5018 0.644 0.03 Uiso 1 1 calc R . . C14 C 0.52547(18) 0.41917(17) 0.5020(4) 0.0270(6) Uani 1 1 d . . . H14 H 0.5761 0.4206 0.562 0.032 Uiso 1 1 calc R . . C15 C 0.51679(17) 0.36852(17) 0.3663(4) 0.0220(6) Uani 1 1 d . . . H15 H 0.5612 0.3356 0.3357 0.026 Uiso 1 1 calc R . . C16 C 0.44366(15) 0.36563(15) 0.2749(4) 0.0203(5) Uani 1 1 d . . . C17 C 0.2921(2) 0.5003(2) 0.6842(4) 0.0310(7) Uani 1 1 d . . . H17A H 0.2431 0.5317 0.7066 0.046 Uiso 1 1 calc R . . H17B H 0.3371 0.5175 0.7573 0.046 Uiso 1 1 calc R . . H17C H 0.2798 0.4457 0.7072 0.046 Uiso 1 1 calc R . . C18 C 0.3304(2) 0.59189(16) 0.4671(5) 0.0289(7) Uani 1 1 d . . . H18A H 0.2813 0.6218 0.4973 0.043 Uiso 1 1 calc R . . H18B H 0.3416 0.598 0.3461 0.043 Uiso 1 1 calc R . . H18C H 0.3775 0.6108 0.5324 0.043 Uiso 1 1 calc R . . C19 C 0.4897(2) 0.24780(17) 0.1305(6) 0.0368(8) Uani 1 1 d . . . H19A H 0.4763 0.215 0.0331 0.055 Uiso 1 1 calc R . . H19B H 0.4854 0.2172 0.2345 0.055 Uiso 1 1 calc R . . H19C H 0.5459 0.2676 0.1187 0.055 Uiso 1 1 calc R . . C20 C 0.4212(2) 0.3484(2) -0.0264(4) 0.0323(7) Uani 1 1 d . . . H20A H 0.4133 0.3079 -0.1117 0.048 Uiso 1 1 calc R . . H20B H 0.4701 0.379 -0.0546 0.048 Uiso 1 1 calc R . . H20C H 0.3729 0.3823 -0.0243 0.048 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 Sn 0.01553(8) 0.02427(9) 0.01604(8) 0.00155(10) -0.00053(6) -0.00196(6) Cl1 0.0302(3) 0.0340(4) 0.0242(4) 0.0094(3) -0.0016(3) 0.0002(3) Cl2 0.0307(4) 0.0434(4) 0.0220(3) -0.0061(3) -0.0050(3) -0.0061(3) N1 0.0307(14) 0.0229(13) 0.0247(13) 0.0013(10) -0.0055(10) -0.0049(10) N2 0.0199(11) 0.0516(18) 0.0270(14) 0.0018(13) 0.0032(10) 0.0060(12) N3 0.0218(10) 0.0259(12) 0.0178(11) -0.0023(10) 0.0002(10) -0.0021(9) N4 0.0263(12) 0.0245(12) 0.0239(13) -0.0065(10) -0.0008(10) 0.0017(10) C1 0.0247(13) 0.0307(15) 0.0144(12) 0.0011(11) 0.0004(11) -0.0095(12) C2 0.0328(15) 0.0287(15) 0.0169(14) -0.0031(11) -0.0009(12) -0.0126(13) C3 0.054(2) 0.0348(17) 0.0263(17) 0.0021(15) 0.0033(16) -0.0207(16) C4 0.0462(19) 0.053(2) 0.0286(17) -0.0059(17) 0.0159(16) -0.0268(17) C5 0.0323(16) 0.055(2) 0.0261(16) -0.0097(16) 0.0118(13) -0.0156(16) C6 0.0231(14) 0.0422(18) 0.0163(13) -0.0049(12) 0.0031(12) -0.0091(12) C7 0.046(2) 0.0242(16) 0.040(2) -0.0035(15) 0.0005(15) -0.0034(14) C8 0.0454(19) 0.0381(19) 0.0363(19) 0.0121(15) -0.0190(16) -0.0065(15) C9 0.0325(16) 0.0386(18) 0.0321(17) 0.0001(15) 0.0002(14) 0.0101(14) C10 0.0267(17) 0.093(3) 0.036(2) 0.008(2) 0.0082(15) 0.0141(19) C11 0.0170(12) 0.0197(13) 0.0182(12) 0.0025(9) -0.0007(10) -0.0051(9) C12 0.0201(12) 0.0208(13) 0.0192(12) -0.0004(10) -0.0004(10) -0.0013(10) C13 0.0250(13) 0.0282(15) 0.0223(14) -0.0040(12) -0.0050(12) -0.0049(11) C14 0.0216(14) 0.0325(16) 0.0268(16) 0.0025(13) -0.0070(13) 0.0009(11) C15 0.0176(12) 0.0262(14) 0.0223(14) 0.0014(12) -0.0010(11) 0.0023(11) C16 0.0215(11) 0.0207(11) 0.0185(12) 0.0021(13) -0.0019(12) -0.0026(9) C17 0.0311(16) 0.0417(19) 0.0202(15) -0.0007(14) 0.0026(13) 0.0042(14) C18 0.0308(16) 0.0245(15) 0.0314(17) -0.0023(12) 0.0006(14) 0.0014(12) C19 0.0433(18) 0.0277(17) 0.039(2) -0.0113(15) -0.0019(16) 0.0050(14) C20 0.0287(15) 0.047(2) 0.0213(15) -0.0057(14) -0.0016(12) 0.0017(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn C11 2.131(3) . ? Sn C1 2.137(3) . ? Sn Cl2 2.3890(9) . ? Sn Cl1 2.4115(8) . ? Sn N1 2.577(3) . ? N1 C2 1.454(4) . ? N1 C8 1.467(4) . ? N1 C7 1.480(5) . ? N2 C6 1.408(4) . ? N2 C9 1.449(5) . ? N2 C10 1.463(4) . ? N3 C12 1.455(3) . ? N3 C18 1.475(4) . ? N3 C17 1.478(4) . ? N4 C16 1.426(4) . ? N4 C20 1.449(4) . ? N4 C19 1.467(4) . ? C1 C2 1.383(4) . ? C1 C6 1.421(4) . ? C2 C3 1.394(4) . ? C3 C4 1.379(6) . ? C4 C5 1.376(6) . ? C5 C6 1.397(4) . ? C11 C12 1.391(4) . ? C11 C16 1.405(4) . ? C12 C13 1.393(4) . ? C13 C14 1.378(4) . ? C14 C15 1.392(4) . ? C15 C16 1.392(4) . ? 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 C11 Sn C1 127.31(11) . . ? C11 Sn Cl2 115.89(8) . . ? C1 Sn Cl2 100.85(8) . . ? C11 Sn Cl1 102.19(7) . . ? C1 Sn Cl1 114.11(9) . . ? Cl2 Sn Cl1 90.93(3) . . ? C11 Sn N1 84.28(9) . . ? C1 Sn N1 59.81(10) . . ? Cl2 Sn N1 87.73(7) . . ? Cl1 Sn N1 173.30(5) . . ? C2 N1 C8 112.7(3) . . ? C2 N1 C7 112.7(2) . . ? C8 N1 C7 109.3(3) . . ? C2 N1 Sn 82.84(17) . . ? C8 N1 Sn 118.5(2) . . ? C7 N1 Sn 118.3(3) . . ? C6 N2 C9 116.2(3) . . ? C6 N2 C10 116.6(3) . . ? C9 N2 C10 110.6(3) . . ? C12 N3 C18 110.3(2) . . ? C12 N3 C17 113.0(2) . . ? C18 N3 C17 109.8(2) . . ? C16 N4 C20 115.4(2) . . ? C16 N4 C19 115.8(2) . . ? C20 N4 C19 111.3(3) . . ? C2 C1 C6 119.4(3) . . ? C2 C1 Sn 103.1(2) . . ? C6 C1 Sn 136.9(2) . . ? C1 C2 C3 122.4(3) . . ? C1 C2 N1 114.1(3) . . ? C3 C2 N1 123.5(3) . . ? C4 C3 C2 117.7(3) . . ? C5 C4 C3 121.0(3) . . ? C4 C5 C6 122.1(3) . . ? C5 C6 N2 121.8(3) . . ? C5 C6 C1 117.1(3) . . ? N2 C6 C1 121.1(3) . . ? C12 C11 C16 119.7(3) . . ? C12 C11 Sn 107.54(19) . . ? C16 C11 Sn 131.1(2) . . ? C11 C12 C13 121.7(3) . . ? C11 C12 N3 115.0(2) . . ? C13 C12 N3 123.2(3) . . ? C14 C13 C12 118.0(3) . . ? C13 C14 C15 121.5(3) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C11 118.5(3) . . ? C15 C16 N4 122.1(2) . . ? C11 C16 N4 119.4(2) . . ? #===END data_(6)-oct1899 _database_code_depnum_ccdc_archive 'CCDC 697228' _audit_creation_date 1999-10-19T09:59:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H30 I2 N4 Sn' _chemical_formula_sum 'C20 H30 I2 N4 Sn' _chemical_formula_weight 698.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4333(2) _cell_length_b 15.0037(2) _cell_length_c 20.1333(3) _cell_angle_alpha 90 _cell_angle_beta 90.824(1) _cell_angle_gamma 90 _cell_volume 4963.56(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28119 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3635 _exptl_absorpt_correction_T_max 0.4234 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 44805 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 14287 _reflns_number_gt 12199 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0120P)^2^+9.5660P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00049(4) _refine_ls_number_reflns 14287 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.039 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.939 _refine_diff_density_min -1.615 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sn Sn 0.316188(11) 0.175446(12) 0.240555(9) 0.02192(5) Uani 1 1 d . . . I1 I 0.348032(13) 0.103868(15) 0.116114(10) 0.03819(6) Uani 1 1 d . . . I2 I 0.305596(15) 0.010685(14) 0.297245(12) 0.04259(6) Uani 1 1 d . . . N1 N 0.30802(15) 0.34090(17) 0.17479(12) 0.0299(5) Uani 1 1 d . . . N2 N 0.11210(16) 0.15009(19) 0.28179(13) 0.0352(6) Uani 1 1 d . . . N3 N 0.29943(14) 0.24684(16) 0.36703(11) 0.0266(5) Uani 1 1 d . . . N4 N 0.52255(15) 0.22964(17) 0.21507(13) 0.0311(5) Uani 1 1 d . . . C1 C 0.20673(16) 0.24959(19) 0.22632(13) 0.0245(5) Uani 1 1 d . . . C2 C 0.22569(17) 0.33175(19) 0.19826(14) 0.0271(5) Uani 1 1 d . . . C3 C 0.1682(2) 0.3999(2) 0.19536(16) 0.0377(7) Uani 1 1 d . . . H3 H 0.181 0.4558 0.1761 0.045 Uiso 1 1 calc R . . C4 C 0.0926(2) 0.3845(3) 0.22089(19) 0.0459(8) Uani 1 1 d . . . H4 H 0.0533 0.4309 0.2198 0.055 Uiso 1 1 calc R . . C5 C 0.0719(2) 0.3027(3) 0.24842(17) 0.0411(8) Uani 1 1 d . . . H5 H 0.0187 0.2938 0.2651 0.049 Uiso 1 1 calc R . . C6 C 0.12868(17) 0.2336(2) 0.25172(14) 0.0303(6) Uani 1 1 d . . . C7 C 0.3104(2) 0.3414(3) 0.10155(16) 0.0452(8) Uani 1 1 d . . . H7A H 0.3669 0.3476 0.0872 0.068 Uiso 1 1 calc R . . H7B H 0.2782 0.3915 0.0844 0.068 Uiso 1 1 calc R . . H7C H 0.2878 0.2854 0.0843 0.068 Uiso 1 1 calc R . . C8 C 0.3502(2) 0.4194(2) 0.20160(19) 0.0436(8) Uani 1 1 d . . . H8A H 0.4054 0.422 0.184 0.065 Uiso 1 1 calc R . . H8B H 0.3529 0.4155 0.2502 0.065 Uiso 1 1 calc R . . H8C H 0.3204 0.4734 0.1885 0.065 Uiso 1 1 calc R . . C9 C 0.0446(3) 0.1481(3) 0.3280(2) 0.0591(11) Uani 1 1 d . . . H9A H 0.0384 0.0877 0.3457 0.089 Uiso 1 1 calc R . . H9B H -0.0057 0.1658 0.3048 0.089 Uiso 1 1 calc R . . H9C H 0.0556 0.1896 0.3647 0.089 Uiso 1 1 calc R . . C10 C 0.1049(2) 0.0764(2) 0.23439(19) 0.0463(8) Uani 1 1 d . . . H10A H 0.0935 0.021 0.2584 0.07 Uiso 1 1 calc R . . H10B H 0.156 0.0701 0.2103 0.07 Uiso 1 1 calc R . . H10C H 0.0605 0.0887 0.2028 0.07 Uiso 1 1 calc R . . C11 C 0.41105(16) 0.24517(17) 0.29177(13) 0.0224(5) Uani 1 1 d . . . C12 C 0.37715(16) 0.28348(18) 0.34806(13) 0.0247(5) Uani 1 1 d . . . C13 C 0.41575(19) 0.3536(2) 0.38131(15) 0.0323(6) Uani 1 1 d . . . H13 H 0.3929 0.3789 0.4201 0.039 Uiso 1 1 calc R . . C14 C 0.4881(2) 0.3855(2) 0.35645(16) 0.0346(7) Uani 1 1 d . . . H14 H 0.5135 0.4354 0.377 0.042 Uiso 1 1 calc R . . C15 C 0.52435(18) 0.3458(2) 0.30191(15) 0.0317(6) Uani 1 1 d . . . H15 H 0.5746 0.3683 0.2863 0.038 Uiso 1 1 calc R . . C16 C 0.48780(16) 0.27322(19) 0.26985(14) 0.0265(5) Uani 1 1 d . . . C17 C 0.23786(19) 0.3144(2) 0.38169(17) 0.0389(7) Uani 1 1 d . . . H17A H 0.187 0.285 0.394 0.058 Uiso 1 1 calc R . . H17B H 0.2283 0.3515 0.3423 0.058 Uiso 1 1 calc R . . H17C H 0.2571 0.3518 0.4186 0.058 Uiso 1 1 calc R . . C18 C 0.3089(2) 0.1857(2) 0.42388(16) 0.0403(8) Uani 1 1 d . . . H18A H 0.2555 0.1618 0.4358 0.06 Uiso 1 1 calc R . . H18B H 0.3323 0.2181 0.4619 0.06 Uiso 1 1 calc R . . H18C H 0.3451 0.1366 0.4118 0.06 Uiso 1 1 calc R . . C19 C 0.5918(2) 0.2742(3) 0.18478(18) 0.0479(9) Uani 1 1 d . . . H19A H 0.6113 0.2383 0.1476 0.072 Uiso 1 1 calc R . . H19B H 0.6356 0.281 0.2179 0.072 Uiso 1 1 calc R . . H19C H 0.575 0.333 0.1686 0.072 Uiso 1 1 calc R . . C20 C 0.5377(2) 0.1348(2) 0.22404(18) 0.0404(7) Uani 1 1 d . . . H20A H 0.5618 0.1104 0.1837 0.061 Uiso 1 1 calc R . . H20B H 0.4863 0.1042 0.2327 0.061 Uiso 1 1 calc R . . H20C H 0.5752 0.126 0.2617 0.061 Uiso 1 1 calc R . . Sn1B Sn 0.177787(11) -0.206246(12) 0.481418(9) 0.02251(5) Uani 1 1 d . . . I1B I 0.130873(15) -0.170546(17) 0.352629(11) 0.04461(6) Uani 1 1 d . . . I2B I 0.161459(15) -0.032390(14) 0.521066(14) 0.04643(7) Uani 1 1 d . . . N1B N 0.20982(18) -0.37443(18) 0.43012(16) 0.0420(7) Uani 1 1 d . . . N2B N 0.37877(16) -0.14049(19) 0.52261(13) 0.0356(6) Uani 1 1 d . . . N3B N 0.20674(15) -0.25750(19) 0.61252(12) 0.0330(5) Uani 1 1 d . . . N4B N -0.02566(15) -0.28168(17) 0.46433(13) 0.0301(5) Uani 1 1 d . . . C1B C 0.29796(17) -0.26074(19) 0.47462(13) 0.0259(5) Uani 1 1 d . . . C2B C 0.29076(19) -0.3475(2) 0.45134(16) 0.0336(6) Uani 1 1 d . . . C3B C 0.3575(2) -0.4049(2) 0.4513(2) 0.0493(10) Uani 1 1 d . . . H3B H 0.3523 -0.4643 0.4355 0.059 Uiso 1 1 calc R . . C4B C 0.4311(2) -0.3732(3) 0.4748(2) 0.0522(10) Uani 1 1 d . . . H4B H 0.4771 -0.4116 0.4756 0.063 Uiso 1 1 calc R . . C5B C 0.4394(2) -0.2867(3) 0.49728(19) 0.0439(8) Uani 1 1 d . . . H5B H 0.4911 -0.2664 0.5124 0.053 Uiso 1 1 calc R . . C6B C 0.37311(18) -0.2286(2) 0.49817(14) 0.0312(6) Uani 1 1 d . . . C7B C 0.2068(3) -0.3961(3) 0.3589(2) 0.0695(13) Uani 1 1 d . . . H7B1 H 0.1514 -0.414 0.3462 0.104 Uiso 1 1 calc R . . H7B2 H 0.2445 -0.4451 0.3499 0.104 Uiso 1 1 calc R . . H7B3 H 0.2226 -0.3436 0.3331 0.104 Uiso 1 1 calc R . . C8B C 0.1779(3) -0.4492(2) 0.4696(3) 0.0620(13) Uani 1 1 d . . . H8B1 H 0.1232 -0.4647 0.4534 0.093 Uiso 1 1 calc R . . H8B2 H 0.1755 -0.4316 0.5164 0.093 Uiso 1 1 calc R . . H8B3 H 0.2139 -0.5009 0.4652 0.093 Uiso 1 1 calc R . . C9B C 0.4474(3) -0.1219(3) 0.5674(2) 0.0626(12) Uani 1 1 d . . . H9B1 H 0.4455 -0.0594 0.5814 0.094 Uiso 1 1 calc R . . H9B2 H 0.4985 -0.1333 0.5444 0.094 Uiso 1 1 calc R . . H9B3 H 0.4441 -0.1606 0.6065 0.094 Uiso 1 1 calc R . . C10B C 0.3733(2) -0.0729(2) 0.47094(18) 0.0433(8) Uani 1 1 d . . . H10D H 0.3776 -0.0136 0.4911 0.065 Uiso 1 1 calc R . . H10E H 0.321 -0.0783 0.4473 0.065 Uiso 1 1 calc R . . H10F H 0.4177 -0.0812 0.4396 0.065 Uiso 1 1 calc R . . C11B C 0.09146(16) -0.27660(18) 0.53980(13) 0.0239(5) Uani 1 1 d . . . C12B C 0.12982(17) -0.3017(2) 0.59833(14) 0.0282(6) Uani 1 1 d . . . C13B C 0.0969(2) -0.3670(2) 0.63961(16) 0.0378(7) Uani 1 1 d . . . H13B H 0.1238 -0.3845 0.6796 0.045 Uiso 1 1 calc R . . C14B C 0.0235(2) -0.4055(2) 0.62006(17) 0.0389(7) Uani 1 1 d . . . H14B H 0.001 -0.4517 0.6463 0.047 Uiso 1 1 calc R . . C15B C -0.01758(19) -0.3779(2) 0.56311(16) 0.0332(6) Uani 1 1 d . . . H15B H -0.0684 -0.4045 0.5517 0.04 Uiso 1 1 calc R . . C16B C 0.01445(17) -0.31170(18) 0.52212(14) 0.0254(5) Uani 1 1 d . . . C17B C 0.2730(2) -0.3187(3) 0.6314(2) 0.0539(10) Uani 1 1 d . . . H17D H 0.3229 -0.2845 0.6401 0.081 Uiso 1 1 calc R . . H17E H 0.2823 -0.3609 0.5951 0.081 Uiso 1 1 calc R . . H17F H 0.2581 -0.3515 0.6715 0.081 Uiso 1 1 calc R . . C18B C 0.1979(2) -0.1883(3) 0.66352(17) 0.0472(9) Uani 1 1 d . . . H18D H 0.2507 -0.1597 0.6719 0.071 Uiso 1 1 calc R . . H18E H 0.1785 -0.2154 0.7047 0.071 Uiso 1 1 calc R . . H18F H 0.1586 -0.1435 0.648 0.071 Uiso 1 1 calc R . . C19B C -0.0942(2) -0.3356(3) 0.43998(19) 0.0473(9) Uani 1 1 d . . . H19D H -0.1172 -0.3084 0.3996 0.071 Uiso 1 1 calc R . . H19E H -0.136 -0.3385 0.4741 0.071 Uiso 1 1 calc R . . H19F H -0.0751 -0.3959 0.4299 0.071 Uiso 1 1 calc R . . C20B C -0.0478(2) -0.1873(2) 0.46441(18) 0.0388(7) Uani 1 1 d . . . H20D H -0.0754 -0.1723 0.4224 0.058 Uiso 1 1 calc R . . H20E H 0.0014 -0.1509 0.4695 0.058 Uiso 1 1 calc R . . H20F H -0.0845 -0.1753 0.5014 0.058 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 Sn 0.02076(8) 0.01981(9) 0.02519(9) 0.00005(7) 0.00027(6) 0.00115(6) I1 0.04083(11) 0.04355(12) 0.03026(10) -0.00919(8) 0.00336(8) 0.00500(9) I2 0.05878(14) 0.02247(10) 0.04675(12) 0.00885(8) 0.00853(10) 0.00289(9) N1 0.0321(12) 0.0292(13) 0.0285(12) 0.0096(10) -0.0006(10) 0.0008(10) N2 0.0292(12) 0.0417(15) 0.0349(13) -0.0047(11) 0.0061(10) -0.0091(11) N3 0.0249(11) 0.0306(12) 0.0243(11) -0.0008(9) 0.0039(9) 0.0029(9) N4 0.0273(12) 0.0354(14) 0.0307(12) 0.0006(10) 0.0054(10) -0.0037(10) C1 0.0241(12) 0.0273(13) 0.0222(12) -0.0021(10) -0.0028(10) 0.0048(10) C2 0.0284(13) 0.0284(14) 0.0243(12) 0.0023(11) -0.0037(10) 0.0047(11) C3 0.0451(18) 0.0327(16) 0.0352(16) 0.0045(13) -0.0041(14) 0.0144(14) C4 0.0410(18) 0.044(2) 0.052(2) -0.0022(17) -0.0047(16) 0.0213(15) C5 0.0259(14) 0.057(2) 0.0404(17) -0.0067(16) -0.0003(13) 0.0095(14) C6 0.0238(13) 0.0400(17) 0.0270(13) -0.0080(12) -0.0031(11) 0.0011(11) C7 0.053(2) 0.053(2) 0.0302(15) 0.0153(15) 0.0051(15) 0.0091(17) C8 0.0458(19) 0.0298(17) 0.055(2) 0.0143(15) -0.0075(16) -0.0060(14) C9 0.052(2) 0.065(3) 0.060(2) -0.005(2) 0.026(2) -0.014(2) C10 0.0444(19) 0.044(2) 0.051(2) -0.0105(16) 0.0035(16) -0.0137(16) C11 0.0245(12) 0.0189(12) 0.0236(11) 0.0038(10) -0.0021(10) 0.0008(9) C12 0.0240(12) 0.0254(13) 0.0247(12) 0.0038(10) -0.0015(10) 0.0018(10) C13 0.0380(16) 0.0303(15) 0.0287(14) -0.0057(12) -0.0016(12) 0.0019(12) C14 0.0402(16) 0.0296(15) 0.0338(15) -0.0026(12) -0.0063(13) -0.0075(13) C15 0.0280(14) 0.0329(16) 0.0340(15) 0.0048(12) -0.0048(12) -0.0070(12) C16 0.0235(12) 0.0298(14) 0.0260(12) 0.0048(11) -0.0010(10) -0.0002(10) C17 0.0318(15) 0.0448(19) 0.0403(17) -0.0113(14) 0.0059(13) 0.0072(13) C18 0.0451(18) 0.049(2) 0.0273(14) 0.0112(14) 0.0027(13) -0.0053(15) C19 0.0406(18) 0.062(2) 0.0414(18) -0.0085(17) 0.0159(15) -0.0181(17) C20 0.0324(16) 0.0423(19) 0.0468(18) -0.0040(15) 0.0061(14) 0.0077(14) Sn1B 0.02353(9) 0.01894(9) 0.02511(9) 0.00034(7) 0.00179(7) -0.00209(6) I1B 0.04716(13) 0.05841(15) 0.02811(10) 0.01173(9) -0.00473(9) -0.01393(11) I2B 0.05070(13) 0.02258(10) 0.06583(16) -0.01266(10) -0.00505(11) 0.00070(9) N1B 0.0438(16) 0.0283(14) 0.0544(17) -0.0143(13) 0.0126(13) -0.0081(12) N2B 0.0334(13) 0.0381(15) 0.0352(13) 0.0042(11) -0.0049(11) -0.0065(11) N3B 0.0227(11) 0.0470(16) 0.0291(12) 0.0053(11) -0.0032(10) -0.0002(10) N4B 0.0276(12) 0.0315(13) 0.0313(12) -0.0006(10) -0.0033(10) -0.0048(10) C1B 0.0266(13) 0.0272(14) 0.0242(12) 0.0032(10) 0.0073(10) 0.0012(10) C2B 0.0373(16) 0.0281(15) 0.0357(15) 0.0010(12) 0.0122(13) 0.0018(12) C3B 0.060(2) 0.0307(17) 0.058(2) 0.0056(16) 0.0254(19) 0.0159(16) C4B 0.0400(19) 0.057(2) 0.060(2) 0.0164(19) 0.0146(17) 0.0223(17) C5B 0.0293(15) 0.053(2) 0.0493(19) 0.0183(17) 0.0041(14) 0.0066(14) C6B 0.0278(14) 0.0386(17) 0.0274(13) 0.0094(12) 0.0044(11) 0.0013(12) C7B 0.071(3) 0.070(3) 0.067(3) -0.040(2) 0.004(2) -0.009(2) C8B 0.063(2) 0.0220(17) 0.102(4) -0.0106(19) 0.039(2) -0.0108(16) C9B 0.049(2) 0.075(3) 0.063(3) 0.006(2) -0.026(2) -0.014(2) C10B 0.0474(19) 0.0372(18) 0.0453(19) 0.0090(15) -0.0025(16) -0.0099(15) C11B 0.0269(13) 0.0207(12) 0.0244(12) 0.0017(10) 0.0040(10) -0.0008(10) C12B 0.0277(13) 0.0298(14) 0.0272(13) 0.0038(11) 0.0047(11) 0.0032(11) C13B 0.0410(17) 0.0390(18) 0.0334(15) 0.0121(13) 0.0035(13) 0.0031(14) C14B 0.0455(18) 0.0303(16) 0.0413(17) 0.0118(13) 0.0090(14) -0.0033(13) C15B 0.0338(15) 0.0257(14) 0.0403(16) -0.0010(12) 0.0062(13) -0.0066(12) C16B 0.0258(13) 0.0229(13) 0.0277(13) -0.0027(10) 0.0028(10) 0.0005(10) C17B 0.0314(17) 0.078(3) 0.052(2) 0.029(2) -0.0028(16) 0.0095(17) C18B 0.0443(19) 0.066(2) 0.0309(16) -0.0103(16) -0.0008(14) -0.0127(17) C19B 0.0428(19) 0.054(2) 0.0444(19) -0.0053(17) -0.0107(16) -0.0128(16) C20B 0.0345(16) 0.0365(17) 0.0451(18) 0.0069(14) -0.0041(14) 0.0035(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn C1 2.131(3) . ? Sn C11 2.131(3) . ? Sn I2 2.7294(3) . ? Sn I1 2.7824(3) . ? N1 C2 1.446(4) . ? N1 C8 1.466(4) . ? N1 C7 1.476(4) . ? N2 C6 1.420(4) . ? N2 C9 1.459(4) . ? N2 C10 1.464(4) . ? N3 C12 1.447(3) . ? N3 C17 1.465(4) . ? N3 C18 1.473(4) . ? N4 C16 1.410(4) . ? N4 C20 1.455(4) . ? N4 C19 1.461(4) . ? C1 C2 1.393(4) . ? C1 C6 1.408(4) . ? C2 C3 1.393(4) . ? C3 C4 1.370(5) . ? C4 C5 1.391(5) . ? C5 C6 1.396(4) . ? C11 C12 1.394(4) . ? C11 C16 1.407(4) . ? C12 C13 1.395(4) . ? C13 C14 1.382(4) . ? C14 C15 1.391(4) . ? C15 C16 1.397(4) . ? Sn1B C11B 2.135(3) . ? Sn1B C1B 2.144(3) . ? Sn1B I2B 2.7422(3) . ? Sn1B I1B 2.7472(3) . ? N1B C2B 1.449(4) . ? N1B C7B 1.471(5) . ? N1B C8B 1.475(5) . ? N2B C6B 1.414(4) . ? N2B C10B 1.455(4) . ? N2B C9B 1.461(5) . ? N3B C12B 1.453(4) . ? N3B C18B 1.469(4) . ? N3B C17B 1.470(4) . ? N4B C16B 1.403(4) . ? N4B C20B 1.463(4) . ? N4B C19B 1.465(4) . ? C1B C2B 1.387(4) . ? C1B C6B 1.402(4) . ? C2B C3B 1.395(5) . ? C3B C4B 1.378(6) . ? C4B C5B 1.380(6) . ? C5B C6B 1.395(4) . ? C11B C12B 1.381(4) . ? C11B C16B 1.412(4) . ? C12B C13B 1.398(4) . ? C13B C14B 1.389(5) . ? C14B C15B 1.385(5) . ? C15B C16B 1.399(4) . ? 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 Sn C11 114.77(10) . . ? C1 Sn I2 118.05(8) . . ? C11 Sn I2 107.03(7) . . ? C1 Sn I1 104.46(7) . . ? C11 Sn I1 118.65(7) . . ? I2 Sn I1 92.345(9) . . ? C2 N1 C8 113.3(3) . . ? C2 N1 C7 111.5(3) . . ? C8 N1 C7 110.1(3) . . ? C6 N2 C9 116.2(3) . . ? C6 N2 C10 113.7(3) . . ? C9 N2 C10 110.2(3) . . ? C12 N3 C17 113.9(2) . . ? C12 N3 C18 111.0(2) . . ? C17 N3 C18 109.8(3) . . ? C16 N4 C20 115.3(2) . . ? C16 N4 C19 116.2(3) . . ? C20 N4 C19 111.5(3) . . ? C2 C1 C6 120.6(3) . . ? C2 C1 Sn 108.86(19) . . ? C6 C1 Sn 129.3(2) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 N1 123.7(3) . . ? C1 C2 N1 115.6(2) . . ? C4 C3 C2 118.6(3) . . ? C3 C4 C5 121.8(3) . . ? C4 C5 C6 120.4(3) . . ? C5 C6 C1 117.9(3) . . ? C5 C6 N2 122.9(3) . . ? C1 C6 N2 119.1(3) . . ? C12 C11 C16 120.1(3) . . ? C12 C11 Sn 107.32(18) . . ? C16 C11 Sn 130.4(2) . . ? C11 C12 C13 121.1(3) . . ? C11 C12 N3 115.0(2) . . ? C13 C12 N3 123.8(3) . . ? C14 C13 C12 118.3(3) . . ? C13 C14 C15 121.2(3) . . ? C14 C15 C16 120.8(3) . . ? C15 C16 C11 118.0(3) . . ? C15 C16 N4 123.1(3) . . ? C11 C16 N4 118.8(3) . . ? C11B Sn1B C1B 117.82(10) . . ? C11B Sn1B I2B 103.98(7) . . ? C1B Sn1B I2B 118.39(8) . . ? C11B Sn1B I1B 115.88(8) . . ? C1B Sn1B I1B 105.10(7) . . ? I2B Sn1B I1B 93.553(10) . . ? C2B N1B C7B 111.5(3) . . ? C2B N1B C8B 112.7(3) . . ? C7B N1B C8B 110.5(3) . . ? C6B N2B C10B 113.6(3) . . ? C6B N2B C9B 116.1(3) . . ? C10B N2B C9B 110.4(3) . . ? C12B N3B C18B 111.5(2) . . ? C12B N3B C17B 113.9(3) . . ? C18B N3B C17B 110.0(3) . . ? C16B N4B C20B 115.1(2) . . ? C16B N4B C19B 116.7(3) . . ? C20B N4B C19B 110.2(3) . . ? C2B C1B C6B 120.5(3) . . ? C2B C1B Sn1B 107.8(2) . . ? C6B C1B Sn1B 130.9(2) . . ? C1B C2B C3B 121.1(3) . . ? C1B C2B N1B 115.8(3) . . ? C3B C2B N1B 123.1(3) . . ? C4B C3B C2B 118.2(3) . . ? C3B C4B C5B 121.3(3) . . ? C4B C5B C6B 121.2(3) . . ? C5B C6B C1B 117.7(3) . . ? C5B C6B N2B 122.8(3) . . ? C1B C6B N2B 119.5(3) . . ? C12B C11B C16B 120.7(2) . . ? C12B C11B Sn1B 107.83(19) . . ? C16B C11B Sn1B 130.2(2) . . ? C11B C12B C13B 121.5(3) . . ? C11B C12B N3B 115.4(2) . . ? C13B C12B N3B 123.1(3) . . ? C14B C13B C12B 117.7(3) . . ? C15B C14B C13B 121.4(3) . . ? C14B C15B C16B 121.1(3) . . ? C15B C16B N4B 122.7(3) . . ? C15B C16B C11B 117.4(3) . . ? N4B C16B C11B 119.9(2) . . ? #===END data_(7)-oct2300 _database_code_depnum_ccdc_archive 'CCDC 697229' _audit_creation_date 2000-10-13T15:48:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H48 N8 Si2 Sn' _chemical_formula_sum 'C26 H48 N8 Si2 Sn' _chemical_formula_weight 647.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pn _symmetry_space_group_name_Hall 'P -2yac' _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.5687(6) _cell_length_b 17.0682(12) _cell_length_c 11.0296(7) _cell_angle_alpha 90 _cell_angle_beta 114.313(4) _cell_angle_gamma 90 _cell_volume 1641.60(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31833 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.703 _exptl_absorpt_correction_T_max 0.729 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 8394 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.0493 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 4890 _reflns_number_gt 4719 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0322P)^2^+1.1247P] 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_number_reflns 4890 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.077 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_diff_density_max 0.687 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sn Sn 0.15020(3) 0.222784(12) 0.68707(3) 0.02081(9) Uani 1 1 d . . . Si1 Si 0.10163(16) 0.38811(7) 0.82236(13) 0.0343(3) Uani 1 1 d . . . Si2 Si 0.40465(17) 0.36250(8) 0.80485(14) 0.0368(3) Uani 1 1 d . . . N1 N 0.3150(4) 0.1623(2) 0.8510(4) 0.0299(8) Uani 1 1 d . . . N2 N 0.3440(4) 0.1790(2) 0.9654(4) 0.0314(9) Uani 1 1 d . . . N3 N 0.3788(6) 0.1908(3) 1.0771(4) 0.0480(12) Uani 1 1 d . . . N4 N 0.1618(4) 0.0620(2) 0.6069(4) 0.0297(9) Uani 1 1 d . . . N5 N 0.2613(5) 0.3156(2) 0.4553(4) 0.0319(9) Uani 1 1 d . . . N6 N -0.1558(4) 0.2375(2) 0.4133(4) 0.0255(8) Uani 1 1 d . . . N7 N -0.0081(5) 0.1471(2) 0.8723(4) 0.0313(9) Uani 1 1 d . . . N8 N 0.2143(4) 0.3337(2) 0.7623(4) 0.0294(9) Uani 1 1 d . . . C1 C -0.1077(7) 0.3834(3) 0.7101(7) 0.0572(16) Uani 1 1 d . . . H1A H -0.1235 0.4007 0.6206 0.086 Uiso 1 1 calc R . . H1B H -0.1649 0.4177 0.7448 0.086 Uiso 1 1 calc R . . H1C H -0.1441 0.3294 0.7061 0.086 Uiso 1 1 calc R . . C2 C 0.1481(8) 0.4949(3) 0.8326(6) 0.0543(15) Uani 1 1 d . . . H2A H 0.1353 0.5139 0.7448 0.081 Uiso 1 1 calc R . . H2B H 0.2544 0.5031 0.8964 0.081 Uiso 1 1 calc R . . H2C H 0.079 0.5238 0.8619 0.081 Uiso 1 1 calc R . . C3 C 0.1305(9) 0.3567(4) 0.9931(7) 0.063(2) Uani 1 1 d . . . H3A H 0.2399 0.3589 1.0522 0.094 Uiso 1 1 calc R . . H3B H 0.0932 0.3029 0.99 0.094 Uiso 1 1 calc R . . H3C H 0.0734 0.3917 1.0268 0.094 Uiso 1 1 calc R . . C4 C 0.4186(8) 0.4537(3) 0.7152(6) 0.0549(16) Uani 1 1 d . . . H4A H 0.3567 0.4953 0.7301 0.082 Uiso 1 1 calc R . . H4B H 0.3804 0.4429 0.6197 0.082 Uiso 1 1 calc R . . H4C H 0.5258 0.4706 0.749 0.082 Uiso 1 1 calc R . . C5 C 0.5236(7) 0.2853(3) 0.7738(6) 0.0458(14) Uani 1 1 d . . . H5A H 0.5185 0.2371 0.82 0.069 Uiso 1 1 calc R . . H5B H 0.6302 0.3031 0.8069 0.069 Uiso 1 1 calc R . . H5C H 0.4845 0.2751 0.678 0.069 Uiso 1 1 calc R . . C6 C 0.5046(7) 0.3830(4) 0.9887(6) 0.0612(17) Uani 1 1 d . . . H6A H 0.4481 0.4234 1.0131 0.092 Uiso 1 1 calc R . . H6B H 0.6091 0.4014 1.0101 0.092 Uiso 1 1 calc R . . H6C H 0.5085 0.3349 1.0386 0.092 Uiso 1 1 calc R . . C7 C 0.2061(5) 0.1874(2) 0.5254(4) 0.0263(9) Uani 1 1 d . . . C8 C 0.1881(5) 0.1066(3) 0.5069(4) 0.0271(10) Uani 1 1 d . . . C9 C 0.2055(6) 0.0705(3) 0.4007(5) 0.0334(12) Uani 1 1 d . . . H9 H 0.193 0.0154 0.3883 0.04 Uiso 1 1 calc R . . C10 C 0.2413(6) 0.1157(3) 0.3136(4) 0.0377(12) Uani 1 1 d . . . H10 H 0.2537 0.0915 0.2412 0.045 Uiso 1 1 calc R . . C11 C 0.2591(6) 0.1957(3) 0.3306(5) 0.0348(11) Uani 1 1 d . . . H11 H 0.2841 0.2257 0.2697 0.042 Uiso 1 1 calc R . . C12 C 0.2411(5) 0.2335(3) 0.4355(5) 0.0269(10) Uani 1 1 d . . . C13 C 0.2997(6) 0.0166(3) 0.6891(5) 0.0433(13) Uani 1 1 d . . . H13A H 0.2797 -0.0133 0.7562 0.065 Uiso 1 1 calc R . . H13B H 0.3858 0.0524 0.7335 0.065 Uiso 1 1 calc R . . H13C H 0.3252 -0.0196 0.6323 0.065 Uiso 1 1 calc R . . C14 C 0.0271(6) 0.0103(3) 0.5529(5) 0.0423(13) Uani 1 1 d . . . H14A H 0.0166 -0.0181 0.6259 0.063 Uiso 1 1 calc R . . H14B H 0.0401 -0.0272 0.491 0.063 Uiso 1 1 calc R . . H14C H -0.0651 0.0418 0.5057 0.063 Uiso 1 1 calc R . . C15 C 0.1183(7) 0.3595(3) 0.4119(6) 0.0471(15) Uani 1 1 d . . . H15A H 0.141 0.4155 0.4281 0.071 Uiso 1 1 calc R . . H15B H 0.0598 0.3418 0.4619 0.071 Uiso 1 1 calc R . . H15C H 0.0578 0.3507 0.3167 0.071 Uiso 1 1 calc R . . C16 C 0.3649(8) 0.3517(4) 0.4054(7) 0.0581(16) Uani 1 1 d . . . H16A H 0.3713 0.4081 0.4236 0.087 Uiso 1 1 calc R . . H16B H 0.3263 0.343 0.3093 0.087 Uiso 1 1 calc R . . H16C H 0.467 0.3283 0.4499 0.087 Uiso 1 1 calc R . . C17 C -0.0818(5) 0.1880(2) 0.6417(4) 0.0247(9) Uani 1 1 d . . . C18 C -0.1925(5) 0.1943(2) 0.5089(4) 0.0257(9) Uani 1 1 d . . . C19 C -0.3387(5) 0.1634(3) 0.4738(4) 0.0320(10) Uani 1 1 d . . . H19 H -0.413 0.1674 0.3846 0.038 Uiso 1 1 calc R . . C20 C -0.3765(5) 0.1267(3) 0.5684(5) 0.0360(11) Uani 1 1 d . . . H20 H -0.4759 0.105 0.5435 0.043 Uiso 1 1 calc R . . C21 C -0.2691(6) 0.1216(3) 0.6996(5) 0.0349(11) Uani 1 1 d . . . H21 H -0.2958 0.0974 0.7647 0.042 Uiso 1 1 calc R . . C22 C -0.1232(5) 0.1519(3) 0.7353(4) 0.0299(10) Uani 1 1 d . . . C23 C -0.1612(6) 0.1891(3) 0.3023(5) 0.0336(11) Uani 1 1 d . . . H23A H -0.1358 0.2212 0.2406 0.05 Uiso 1 1 calc R . . H23B H -0.2645 0.1674 0.2558 0.05 Uiso 1 1 calc R . . H23C H -0.087 0.1463 0.3361 0.05 Uiso 1 1 calc R . . C24 C -0.2587(6) 0.3054(3) 0.3610(5) 0.0375(11) Uani 1 1 d . . . H24A H -0.2314 0.3334 0.2962 0.056 Uiso 1 1 calc R . . H24B H -0.2479 0.3407 0.4344 0.056 Uiso 1 1 calc R . . H24C H -0.365 0.2872 0.3176 0.056 Uiso 1 1 calc R . . C25 C -0.0705(7) 0.1710(4) 0.9687(5) 0.0495(14) Uani 1 1 d . . . H25A H -0.1126 0.224 0.9475 0.074 Uiso 1 1 calc R . . H25B H 0.0116 0.1702 1.0587 0.074 Uiso 1 1 calc R . . H25C H -0.1518 0.1345 0.9638 0.074 Uiso 1 1 calc R . . C26 C 0.0565(6) 0.0682(3) 0.9019(6) 0.0401(13) Uani 1 1 d . . . H26A H 0.1337 0.0661 0.994 0.06 Uiso 1 1 calc R . . H26B H 0.1045 0.055 0.8413 0.06 Uiso 1 1 calc R . . H26C H -0.0253 0.0305 0.8902 0.06 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 Sn 0.02198(14) 0.02214(12) 0.01599(13) -0.00083(15) 0.00547(9) -0.00114(15) Si1 0.0462(9) 0.0278(6) 0.0305(7) -0.0052(5) 0.0172(6) 0.0006(6) Si2 0.0355(8) 0.0382(7) 0.0321(7) -0.0069(6) 0.0094(6) -0.0148(6) N1 0.029(2) 0.036(2) 0.019(2) -0.0047(16) 0.0034(15) 0.0014(16) N2 0.027(2) 0.035(2) 0.028(3) 0.0022(17) 0.0072(16) 0.0002(16) N3 0.054(3) 0.066(3) 0.020(2) 0.000(2) 0.011(2) 0.007(3) N4 0.030(2) 0.0244(18) 0.0220(19) 0.0007(15) -0.0023(16) 0.0029(15) N5 0.033(2) 0.037(2) 0.029(2) 0.0052(17) 0.0159(17) -0.0042(17) N6 0.028(2) 0.0268(18) 0.0198(19) 0.0041(14) 0.0081(15) 0.0038(15) N7 0.032(2) 0.041(2) 0.0191(19) 0.0087(15) 0.0084(16) -0.0027(17) N8 0.032(2) 0.0196(17) 0.035(2) -0.0047(15) 0.0110(17) -0.0070(15) C1 0.044(4) 0.049(3) 0.074(4) -0.014(3) 0.020(3) 0.009(3) C2 0.073(4) 0.031(3) 0.055(4) -0.009(2) 0.023(3) -0.002(3) C3 0.087(6) 0.065(4) 0.049(4) 0.011(3) 0.042(4) 0.019(4) C4 0.065(4) 0.046(3) 0.056(4) -0.009(3) 0.026(3) -0.029(3) C5 0.029(3) 0.058(3) 0.047(3) 0.002(2) 0.012(2) -0.004(2) C6 0.048(4) 0.076(4) 0.042(3) -0.015(3) 0.002(3) -0.022(3) C7 0.021(2) 0.032(2) 0.020(2) -0.0005(17) 0.0022(17) 0.0019(18) C8 0.020(2) 0.036(2) 0.020(2) -0.0020(18) 0.0026(18) 0.0047(19) C9 0.036(3) 0.032(2) 0.023(3) -0.011(2) 0.003(2) 0.008(2) C10 0.033(3) 0.059(3) 0.017(2) -0.006(2) 0.0066(19) 0.014(2) C11 0.029(3) 0.057(3) 0.017(2) 0.004(2) 0.0090(19) 0.010(2) C12 0.022(2) 0.039(2) 0.019(2) 0.0031(18) 0.0075(18) 0.0040(18) C13 0.053(3) 0.037(3) 0.027(3) 0.003(2) 0.003(2) 0.020(2) C14 0.049(3) 0.031(2) 0.037(3) -0.007(2) 0.009(2) -0.013(2) C15 0.037(3) 0.035(3) 0.057(4) 0.016(3) 0.007(3) 0.006(2) C16 0.065(4) 0.070(4) 0.057(4) -0.004(3) 0.042(3) -0.023(3) C17 0.026(2) 0.023(2) 0.023(2) 0.0010(16) 0.0071(18) 0.0021(17) C18 0.028(3) 0.0210(19) 0.026(2) -0.0008(17) 0.0092(18) 0.0020(18) C19 0.021(2) 0.039(2) 0.027(2) 0.0032(19) 0.0007(18) -0.0007(19) C20 0.023(3) 0.040(3) 0.040(3) 0.006(2) 0.007(2) -0.005(2) C21 0.031(3) 0.040(2) 0.034(3) 0.009(2) 0.013(2) -0.008(2) C22 0.032(3) 0.031(2) 0.023(2) 0.0059(18) 0.0078(19) -0.0005(19) C23 0.033(3) 0.041(3) 0.022(2) -0.004(2) 0.007(2) 0.001(2) C24 0.035(3) 0.039(3) 0.036(3) 0.013(2) 0.012(2) 0.009(2) C25 0.046(3) 0.074(4) 0.027(3) 0.002(3) 0.013(2) -0.003(3) C26 0.036(3) 0.044(3) 0.032(3) 0.015(2) 0.006(2) 0.000(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn N8 2.057(3) . ? Sn N1 2.116(4) . ? Sn C17 2.148(4) . ? Sn C7 2.148(5) . ? Si1 N8 1.747(4) . ? Si1 C3 1.866(7) . ? Si1 C2 1.869(5) . ? Si1 C1 1.873(6) . ? Si2 N8 1.753(4) . ? Si2 C5 1.863(6) . ? Si2 C4 1.879(6) . ? Si2 C6 1.885(6) . ? N1 N2 1.209(5) . ? N2 N3 1.154(6) . ? N4 C8 1.445(6) . ? N4 C14 1.470(6) . ? N4 C13 1.476(6) . ? N5 C12 1.419(6) . ? N5 C16 1.454(7) . ? N5 C15 1.457(7) . ? N6 C18 1.443(6) . ? N6 C23 1.459(6) . ? N6 C24 1.477(6) . ? N7 C22 1.461(6) . ? N7 C26 1.462(7) . ? N7 C25 1.474(7) . ? C7 C8 1.394(6) . ? C7 C12 1.410(7) . ? C8 C9 1.394(7) . ? C9 C10 1.380(8) . ? C10 C11 1.379(8) . ? C11 C12 1.396(7) . ? C17 C22 1.393(6) . ? C17 C18 1.415(6) . ? C18 C19 1.393(7) . ? C19 C20 1.386(7) . ? C20 C21 1.390(7) . ? C21 C22 1.384(7) . ? 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 N8 Sn N1 96.39(15) . . ? N8 Sn C17 117.15(16) . . ? N1 Sn C17 113.52(16) . . ? N8 Sn C7 117.29(16) . . ? N1 Sn C7 102.67(15) . . ? C17 Sn C7 108.40(16) . . ? N8 Si1 C3 111.9(3) . . ? N8 Si1 C2 111.9(3) . . ? C3 Si1 C2 106.7(3) . . ? N8 Si1 C1 112.7(2) . . ? C3 Si1 C1 109.2(4) . . ? C2 Si1 C1 104.1(3) . . ? N8 Si2 C5 113.5(2) . . ? N8 Si2 C4 112.5(2) . . ? C5 Si2 C4 108.0(3) . . ? N8 Si2 C6 110.6(3) . . ? C5 Si2 C6 104.6(3) . . ? C4 Si2 C6 107.3(3) . . ? N2 N1 Sn 123.1(3) . . ? N3 N2 N1 175.3(5) . . ? C8 N4 C14 114.0(4) . . ? C8 N4 C13 110.7(4) . . ? C14 N4 C13 110.3(4) . . ? C12 N5 C16 115.5(4) . . ? C12 N5 C15 114.0(4) . . ? C16 N5 C15 110.7(5) . . ? C18 N6 C23 112.9(4) . . ? C18 N6 C24 111.3(4) . . ? C23 N6 C24 109.2(4) . . ? C22 N7 C26 110.6(4) . . ? C22 N7 C25 111.9(4) . . ? C26 N7 C25 110.7(4) . . ? Si1 N8 Si2 119.0(2) . . ? Si1 N8 Sn 120.9(2) . . ? Si2 N8 Sn 118.1(2) . . ? C8 C7 C12 120.0(4) . . ? C8 C7 Sn 110.0(3) . . ? C12 C7 Sn 129.7(3) . . ? C7 C8 C9 120.7(4) . . ? C7 C8 N4 117.4(4) . . ? C9 C8 N4 121.8(4) . . ? C10 C9 C8 119.1(4) . . ? C11 C10 C9 120.8(4) . . ? C10 C11 C12 121.3(5) . . ? C11 C12 C7 118.1(4) . . ? C11 C12 N5 121.9(4) . . ? C7 C12 N5 120.0(4) . . ? C22 C17 C18 118.7(4) . . ? C22 C17 Sn 122.2(3) . . ? C18 C17 Sn 118.8(3) . . ? C19 C18 C17 119.8(4) . . ? C19 C18 N6 120.6(4) . . ? C17 C18 N6 119.4(4) . . ? C20 C19 C18 120.4(4) . . ? C19 C20 C21 120.1(4) . . ? C22 C21 C20 119.9(4) . . ? C21 C22 C17 121.1(4) . . ? C21 C22 N7 121.1(4) . . ? C17 C22 N7 117.9(4) . . ? #===END data_(8)-jul2300 _database_code_depnum_ccdc_archive 'CCDC 697230' _audit_creation_date 2000-07-18T15:08:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H30 N10 Sn' _chemical_formula_sum 'C20 H30 N10 Sn' _chemical_formula_weight 529.23 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1) _symmetry_space_group_name_Hall 'P 4w' _symmetry_Int_Tables_number 76 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 9.1568(2) _cell_length_b 9.1568(2) _cell_length_c 29.1683(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2445.67(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9035 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.657 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 7198 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.964 _reflns_number_total 4277 _reflns_number_gt 4103 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0000P)^2^+3.5857P] 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_number_reflns 4277 _refine_ls_number_parameters 281 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(4) _refine_diff_density_max 0.472 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sn Sn 0.00391(4) 0.49081(3) 0.20256(5) 0.02387(10) Uani 1 1 d . . . N1 N 0.0776(4) 0.2709(4) 0.21038(19) 0.0400(12) Uani 1 1 d . . . N2 N 0.2045(5) 0.2443(4) 0.21312(15) 0.0350(10) Uani 1 1 d . . . N3 N 0.3244(5) 0.2123(5) 0.21670(18) 0.0473(12) Uani 1 1 d . . . N4 N 0.2090(4) 0.5459(5) 0.17357(15) 0.0374(9) Uani 1 1 d . . . N5 N 0.3018(5) 0.6139(5) 0.19417(16) 0.0366(10) Uani 1 1 d . . . N6 N 0.3927(5) 0.6779(6) 0.2120(2) 0.0608(15) Uani 1 1 d . . . N7 N -0.2468(4) 0.3720(4) 0.22004(14) 0.0285(8) Uani 1 1 d . . . N8 N -0.0499(4) 0.5992(4) 0.08598(15) 0.0325(9) Uani 1 1 d . . . N9 N -0.0593(4) 0.7706(4) 0.20433(17) 0.0309(8) Uani 1 1 d . . . N10 N 0.0132(5) 0.4180(5) 0.32396(17) 0.0429(11) Uani 1 1 d . . . C1 C -0.1589(5) 0.4761(4) 0.15092(15) 0.0252(9) Uani 1 1 d . . . C2 C -0.2804(5) 0.4203(4) 0.17366(16) 0.0253(9) Uani 1 1 d . . . C3 C -0.4183(5) 0.4226(5) 0.15408(17) 0.0311(10) Uani 1 1 d . . . H3 H -0.5004 0.3837 0.1698 0.037 Uiso 1 1 calc R . . C4 C -0.4324(5) 0.4831(5) 0.11101(18) 0.0347(10) Uani 1 1 d . . . H4 H -0.5262 0.487 0.0971 0.042 Uiso 1 1 calc R . . C5 C -0.3117(5) 0.5391(5) 0.08726(18) 0.0347(10) Uani 1 1 d . . . H5 H -0.3241 0.5791 0.0575 0.042 Uiso 1 1 calc R . . C6 C -0.1729(5) 0.5361(5) 0.10735(16) 0.0297(9) Uani 1 1 d . . . C7 C -0.3411(5) 0.4373(6) 0.25539(19) 0.0400(12) Uani 1 1 d . . . H7A H -0.3125 0.4003 0.2856 0.06 Uiso 1 1 calc R . . H7B H -0.4431 0.4112 0.2493 0.06 Uiso 1 1 calc R . . H7C H -0.3305 0.5437 0.2548 0.06 Uiso 1 1 calc R . . C8 C -0.2536(5) 0.2106(5) 0.2231(2) 0.0384(11) Uani 1 1 d . . . H8A H -0.2312 0.1798 0.2545 0.058 Uiso 1 1 calc R . . H8B H -0.1822 0.1678 0.202 0.058 Uiso 1 1 calc R . . H8C H -0.3519 0.1774 0.2148 0.058 Uiso 1 1 calc R . . C9 C -0.0784(7) 0.6990(7) 0.0480(2) 0.0539(16) Uani 1 1 d . . . H9A H 0.0144 0.7358 0.0359 0.081 Uiso 1 1 calc R . . H9B H -0.1377 0.781 0.0589 0.081 Uiso 1 1 calc R . . H9C H -0.131 0.647 0.0237 0.081 Uiso 1 1 calc R . . C10 C 0.0664(7) 0.4932(6) 0.0740(2) 0.0458(13) Uani 1 1 d . . . H10A H 0.1478 0.5448 0.0594 0.069 Uiso 1 1 calc R . . H10B H 0.0272 0.4201 0.0528 0.069 Uiso 1 1 calc R . . H10C H 0.1011 0.4448 0.1019 0.069 Uiso 1 1 calc R . . C11 C -0.0166(4) 0.6055(4) 0.26570(16) 0.0256(9) Uani 1 1 d . . . C12 C -0.0586(5) 0.7460(5) 0.25339(17) 0.0296(9) Uani 1 1 d . . . C13 C -0.1054(6) 0.8467(6) 0.2857(2) 0.0463(13) Uani 1 1 d . . . H13 H -0.1307 0.9434 0.2771 0.056 Uiso 1 1 calc R . . C14 C -0.1144(6) 0.8020(7) 0.3311(2) 0.0497(14) Uani 1 1 d . . . H14 H -0.1497 0.8678 0.3537 0.06 Uiso 1 1 calc R . . C15 C -0.0726(6) 0.6637(7) 0.34359(19) 0.0455(13) Uani 1 1 d . . . H15 H -0.08 0.6361 0.3749 0.055 Uiso 1 1 calc R . . C16 C -0.0202(5) 0.5631(5) 0.31243(19) 0.0326(11) Uani 1 1 d . . . C17 C -0.2054(6) 0.8112(5) 0.18651(19) 0.0405(12) Uani 1 1 d . . . H17A H -0.1996 0.8266 0.1533 0.061 Uiso 1 1 calc R . . H17B H -0.2384 0.9013 0.2014 0.061 Uiso 1 1 calc R . . H17C H -0.2749 0.7325 0.193 0.061 Uiso 1 1 calc R . . C18 C 0.0496(6) 0.8769(5) 0.1894(2) 0.0442(13) Uani 1 1 d . . . H18A H 0.0436 0.8889 0.156 0.066 Uiso 1 1 calc R . . H18B H 0.1473 0.8423 0.1977 0.066 Uiso 1 1 calc R . . H18C H 0.0309 0.9709 0.2043 0.066 Uiso 1 1 calc R . . C19 C -0.0412(10) 0.3677(9) 0.3678(3) 0.078(2) Uani 1 1 d . . . H19A H -0.0122 0.2657 0.3725 0.118 Uiso 1 1 calc R . . H19B H -0.1479 0.375 0.3683 0.118 Uiso 1 1 calc R . . H19C H -0.0002 0.4283 0.3923 0.118 Uiso 1 1 calc R . . C20 C 0.1641(6) 0.3761(7) 0.3171(2) 0.0550(15) Uani 1 1 d . . . H20A H 0.1772 0.2737 0.326 0.082 Uiso 1 1 calc R . . H20B H 0.2274 0.438 0.336 0.082 Uiso 1 1 calc R . . H20C H 0.19 0.3882 0.2847 0.082 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 Sn 0.02367(14) 0.02297(14) 0.02496(16) -0.0022(2) 0.00046(13) 0.00314(10) N1 0.030(2) 0.0259(17) 0.064(4) -0.003(2) -0.004(2) 0.0037(15) N2 0.039(2) 0.0258(17) 0.040(3) 0.0015(17) 0.0050(19) 0.0030(15) N3 0.034(2) 0.048(2) 0.060(3) 0.012(2) 0.008(2) 0.0117(18) N4 0.033(2) 0.047(2) 0.032(2) -0.0084(19) 0.0032(18) -0.0049(17) N5 0.031(2) 0.039(2) 0.040(3) -0.004(2) 0.0051(19) 0.0035(17) N6 0.040(3) 0.070(3) 0.073(4) -0.032(3) -0.006(3) 0.002(2) N7 0.0314(19) 0.0220(17) 0.032(2) 0.0041(15) 0.0055(17) 0.0021(15) N8 0.035(2) 0.036(2) 0.027(2) 0.0058(18) 0.0013(17) -0.0041(17) N9 0.035(2) 0.0262(15) 0.032(2) -0.002(2) -0.007(2) 0.0010(14) N10 0.051(3) 0.042(3) 0.036(3) 0.016(2) 0.000(2) 0.008(2) C1 0.029(2) 0.0243(19) 0.022(2) -0.0043(17) -0.0001(17) 0.0067(16) C2 0.033(2) 0.0203(19) 0.023(2) -0.0063(17) 0.0006(19) 0.0048(16) C3 0.031(2) 0.033(2) 0.029(3) -0.0040(19) 0.0048(19) -0.0031(18) C4 0.029(2) 0.042(2) 0.033(3) -0.005(2) -0.005(2) 0.0002(19) C5 0.040(2) 0.042(2) 0.023(2) -0.001(2) -0.001(2) -0.003(2) C6 0.032(2) 0.032(2) 0.025(2) -0.0075(18) 0.0013(19) -0.0047(18) C7 0.037(2) 0.052(3) 0.031(3) 0.001(2) 0.010(2) 0.007(2) C8 0.039(2) 0.028(2) 0.049(3) 0.006(2) 0.007(2) -0.0015(19) C9 0.049(3) 0.074(4) 0.039(3) 0.025(3) 0.003(3) -0.008(3) C10 0.047(3) 0.048(3) 0.043(4) -0.012(3) 0.010(3) -0.003(2) C11 0.0259(19) 0.024(2) 0.027(2) -0.0016(17) -0.0035(17) 0.0046(16) C12 0.032(2) 0.026(2) 0.031(3) -0.0031(19) 0.0014(19) 0.0012(17) C13 0.055(3) 0.044(3) 0.040(3) -0.011(2) -0.002(3) 0.018(2) C14 0.051(3) 0.056(3) 0.043(3) -0.022(3) 0.000(3) 0.014(3) C15 0.045(3) 0.066(4) 0.025(3) -0.005(3) 0.001(2) 0.002(3) C16 0.030(2) 0.031(2) 0.036(3) 0.001(2) -0.001(2) 0.0045(19) C17 0.048(3) 0.032(2) 0.042(3) -0.001(2) -0.015(2) 0.006(2) C18 0.053(3) 0.031(2) 0.049(4) 0.007(2) 0.000(3) -0.001(2) C19 0.094(6) 0.083(5) 0.058(5) 0.030(4) 0.015(4) 0.015(4) C20 0.053(3) 0.056(3) 0.056(4) 0.009(3) 0.002(3) 0.015(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn N4 2.121(4) . ? Sn C1 2.123(5) . ? Sn C11 2.129(5) . ? Sn N1 2.136(4) . ? Sn N7 2.591(4) . ? Sn N9 2.627(3) . ? N1 N2 1.189(6) . ? N2 N3 1.141(6) . ? N4 N5 1.213(6) . ? N5 N6 1.143(6) . ? N7 C2 1.456(6) . ? N7 C7 1.472(6) . ? N7 C8 1.482(6) . ? N8 C6 1.411(6) . ? N8 C9 1.460(7) . ? N8 C10 1.483(7) . ? N9 C12 1.448(7) . ? N9 C18 1.460(6) . ? N9 C17 1.483(6) . ? N10 C16 1.404(7) . ? N10 C19 1.448(8) . ? N10 C20 1.448(7) . ? C1 C6 1.390(6) . ? C1 C2 1.393(6) . ? C2 C3 1.386(6) . ? C3 C4 1.379(7) . ? C4 C5 1.401(7) . ? C5 C6 1.400(6) . ? C11 C12 1.390(6) . ? C11 C16 1.418(7) . ? C12 C13 1.387(7) . ? C13 C14 1.388(8) . ? C14 C15 1.373(8) . ? C15 C16 1.380(7) . ? 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 N4 Sn C1 110.73(19) . . ? N4 Sn C11 107.81(17) . . ? C1 Sn C11 125.68(15) . . ? N4 Sn N1 89.25(17) . . ? C1 Sn N1 103.76(17) . . ? C11 Sn N1 113.6(2) . . ? N4 Sn N7 164.38(16) . . ? C1 Sn N7 59.41(15) . . ? C11 Sn N7 87.63(15) . . ? N1 Sn N7 82.14(14) . . ? N4 Sn N9 88.34(15) . . ? C1 Sn N9 85.48(15) . . ? C11 Sn N9 58.82(16) . . ? N1 Sn N9 170.71(19) . . ? N7 Sn N9 102.14(13) . . ? N2 N1 Sn 120.6(3) . . ? N3 N2 N1 176.6(5) . . ? N3 N2 Sn 144.3(4) . . ? N5 N4 Sn 123.0(4) . . ? N6 N5 N4 177.2(6) . . ? N6 N5 Sn 145.9(4) . . ? C2 N7 C7 113.8(4) . . ? C2 N7 C8 110.5(4) . . ? C7 N7 C8 109.8(4) . . ? C2 N7 Sn 82.9(2) . . ? C7 N7 Sn 119.2(3) . . ? C8 N7 Sn 117.9(3) . . ? C6 N8 C9 116.7(4) . . ? C6 N8 C10 114.2(4) . . ? C9 N8 C10 111.0(5) . . ? C12 N9 C18 113.3(4) . . ? C12 N9 C17 112.9(4) . . ? C18 N9 C17 110.1(4) . . ? C12 N9 Sn 82.4(2) . . ? C18 N9 Sn 119.6(3) . . ? C17 N9 Sn 115.9(3) . . ? C16 N10 C19 115.9(5) . . ? C16 N10 C20 115.2(4) . . ? C19 N10 C20 111.5(5) . . ? C6 C1 C2 120.4(4) . . ? C6 C1 Sn 133.5(3) . . ? C2 C1 Sn 104.3(3) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 N7 125.5(4) . . ? C1 C2 N7 112.6(4) . . ? C3 C2 Sn 164.5(3) . . ? C1 C2 Sn 47.0(2) . . ? N7 C2 Sn 66.1(2) . . ? C4 C3 C2 117.8(4) . . ? C3 C4 C5 121.6(4) . . ? C6 C5 C4 120.1(5) . . ? C1 C6 C5 118.3(4) . . ? C1 C6 N8 119.5(4) . . ? C5 C6 N8 122.1(5) . . ? C12 C11 C16 119.7(4) . . ? C12 C11 Sn 104.9(3) . . ? C16 C11 Sn 134.3(3) . . ? C13 C12 C11 121.6(5) . . ? C13 C12 N9 124.6(4) . . ? C11 C12 N9 113.6(4) . . ? C13 C12 Sn 165.7(4) . . ? C11 C12 Sn 46.7(2) . . ? N9 C12 Sn 67.1(2) . . ? C12 C13 C14 118.1(5) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 122.6(5) . . ? C15 C16 N10 123.3(5) . . ? C15 C16 C11 117.3(5) . . ? N10 C16 C11 119.0(4) . . ? #===END data_(10)-oct3800 _database_code_depnum_ccdc_archive 'CCDC 697231' _audit_creation_date 2000-10-31T16:35:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H30 N6 S2 Sn' _chemical_formula_sum 'C22 H30 N6 S2 Sn' _chemical_formula_weight 561.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7728(7) _cell_length_b 10.5566(5) _cell_length_c 13.2285(10) _cell_angle_alpha 83.528(4) _cell_angle_beta 83.428(3) _cell_angle_gamma 71.525(10) _cell_volume 1281.67(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10568 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.18 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.750 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 10193 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0648 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 27.95 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 6078 _reflns_number_gt 5083 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0288P)^2^+1.0784P] 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_number_reflns 6078 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.579 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sn Sn 0.10908(2) -0.28066(2) 0.256289(17) 0.03125(8) Uani 1 1 d . . . S1 S -0.35097(11) 0.00008(10) 0.37727(11) 0.0627(3) Uani 1 1 d . . . S2 S -0.29897(16) -0.3722(2) 0.14195(11) 0.0994(6) Uani 1 1 d . . . N1 N -0.0643(3) -0.1302(3) 0.3244(3) 0.0501(8) Uani 1 1 d . . . N2 N -0.0609(4) -0.3492(3) 0.2196(3) 0.0546(9) Uani 1 1 d . . . N3 N 0.1382(4) -0.2092(3) -0.0366(2) 0.0576(9) Uani 1 1 d . . . N4 N 0.2511(3) -0.1455(3) 0.2965(2) 0.0388(7) Uani 1 1 d . . . N5 N 0.2657(3) -0.5282(3) 0.1931(2) 0.0347(6) Uani 1 1 d . . . N6 N 0.1505(3) -0.3366(3) 0.5173(2) 0.0393(7) Uani 1 1 d . . . C1 C -0.1849(4) -0.0770(3) 0.3453(3) 0.0387(8) Uani 1 1 d . . . C2 C -0.1607(4) -0.3577(4) 0.1870(3) 0.0455(9) Uani 1 1 d . . . C3 C 0.1928(4) -0.1712(3) 0.1320(3) 0.0349(7) Uani 1 1 d . . . C4 C 0.1937(4) -0.1448(3) 0.0238(3) 0.0425(8) Uani 1 1 d . . . C5 C 0.2568(5) -0.0449(4) -0.0180(3) 0.0618(12) Uani 1 1 d . . . H5 H 0.2556 -0.0204 -0.0893 0.074 Uiso 1 1 calc R . . C6 C 0.3194(6) 0.0179(4) 0.0394(4) 0.0701(14) Uani 1 1 d . . . H6 H 0.36 0.0844 0.007 0.084 Uiso 1 1 calc R . . C7 C 0.3253(5) -0.0127(4) 0.1431(4) 0.0573(11) Uani 1 1 d . . . H7 H 0.3721 0.0285 0.1825 0.069 Uiso 1 1 calc R . . C8 C 0.2602(4) -0.1059(3) 0.1871(3) 0.0392(8) Uani 1 1 d . . . C9 C 0.1273(8) -0.1644(6) -0.1447(4) 0.096(2) Uani 1 1 d . . . H9A H 0.0846 -0.2205 -0.1769 0.144 Uiso 1 1 calc R . . H9B H 0.2241 -0.1717 -0.178 0.144 Uiso 1 1 calc R . . H9C H 0.0659 -0.0709 -0.1518 0.144 Uiso 1 1 calc R . . C10 C 0.0723(8) -0.3040(6) -0.0030(4) 0.108(3) Uani 1 1 d . . . H10A H 0.0417 -0.3346 -0.0614 0.163 Uiso 1 1 calc R . . H10B H -0.0125 -0.2656 0.0438 0.163 Uiso 1 1 calc R . . H10C H 0.1403 -0.3802 0.0328 0.163 Uiso 1 1 calc R . . C11 C 0.1876(5) -0.0309(4) 0.3595(4) 0.0616(12) Uani 1 1 d . . . H11A H 0.184 -0.0637 0.4318 0.092 Uiso 1 1 calc R . . H11B H 0.0893 0.0177 0.3409 0.092 Uiso 1 1 calc R . . H11C H 0.2472 0.0293 0.3478 0.092 Uiso 1 1 calc R . . C12 C 0.3948(4) -0.2260(4) 0.3313(3) 0.0494(10) Uani 1 1 d . . . H12A H 0.3845 -0.2511 0.4048 0.074 Uiso 1 1 calc R . . H12B H 0.4618 -0.1728 0.3177 0.074 Uiso 1 1 calc R . . H12C H 0.4327 -0.3072 0.2945 0.074 Uiso 1 1 calc R . . C13 C 0.2099(3) -0.4433(3) 0.3578(2) 0.0276(6) Uani 1 1 d . . . C14 C 0.2844(3) -0.5512(3) 0.3017(2) 0.0305(7) Uani 1 1 d . . . C15 C 0.3702(4) -0.6707(3) 0.3479(3) 0.0447(9) Uani 1 1 d . . . H15 H 0.4194 -0.7447 0.3091 0.054 Uiso 1 1 calc R . . C16 C 0.3817(4) -0.6786(4) 0.4514(3) 0.0505(10) Uani 1 1 d . . . H16 H 0.439 -0.7597 0.4841 0.061 Uiso 1 1 calc R . . C17 C 0.3116(4) -0.5708(4) 0.5088(3) 0.0429(8) Uani 1 1 d . . . H17 H 0.3231 -0.5786 0.5798 0.051 Uiso 1 1 calc R . . C18 C 0.2240(4) -0.4508(3) 0.4634(2) 0.0337(7) Uani 1 1 d . . . C19 C 0.4014(5) -0.5351(5) 0.1313(3) 0.0633(12) Uani 1 1 d . . . H19A H 0.3835 -0.5192 0.0588 0.095 Uiso 1 1 calc R . . H19B H 0.4714 -0.624 0.1437 0.095 Uiso 1 1 calc R . . H19C H 0.4403 -0.4667 0.1498 0.095 Uiso 1 1 calc R . . C20 C 0.1977(5) -0.6207(4) 0.1599(3) 0.0477(9) Uani 1 1 d . . . H20A H 0.1866 -0.6024 0.0865 0.072 Uiso 1 1 calc R . . H20B H 0.1024 -0.608 0.1972 0.072 Uiso 1 1 calc R . . H20C H 0.2589 -0.7132 0.1738 0.072 Uiso 1 1 calc R . . C21 C 0.2132(5) -0.3274(5) 0.6105(3) 0.0625(12) Uani 1 1 d . . . H21A H 0.155 -0.2458 0.6424 0.094 Uiso 1 1 calc R . . H21B H 0.3124 -0.3244 0.5934 0.094 Uiso 1 1 calc R . . H21C H 0.2142 -0.4058 0.658 0.094 Uiso 1 1 calc R . . C22 C -0.0039(4) -0.3171(4) 0.5372(3) 0.0518(10) Uani 1 1 d . . . H22A H -0.0491 -0.2371 0.5746 0.078 Uiso 1 1 calc R . . H22B H -0.0193 -0.3955 0.5781 0.078 Uiso 1 1 calc R . . H22C H -0.0475 -0.3054 0.4723 0.078 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 Sn 0.02981(13) 0.03257(12) 0.02999(13) 0.00094(8) -0.00416(9) -0.00828(9) S1 0.0371(5) 0.0482(5) 0.0935(9) -0.0133(6) 0.0041(5) -0.0007(4) S2 0.0675(9) 0.2094(18) 0.0555(8) -0.0278(10) -0.0021(6) -0.0860(11) N1 0.0373(17) 0.0484(17) 0.055(2) -0.0056(15) -0.0004(15) -0.0002(14) N2 0.0402(18) 0.064(2) 0.066(2) -0.0059(17) -0.0146(17) -0.0207(16) N3 0.089(3) 0.058(2) 0.0298(17) 0.0056(15) -0.0161(17) -0.0272(19) N4 0.0468(17) 0.0349(14) 0.0379(16) -0.0068(12) -0.0069(13) -0.0144(13) N5 0.0385(15) 0.0429(15) 0.0291(14) -0.0081(12) -0.0015(12) -0.0204(12) N6 0.0496(18) 0.0433(15) 0.0303(15) -0.0138(12) 0.0056(13) -0.0212(13) C1 0.042(2) 0.0295(16) 0.041(2) -0.0002(14) -0.0041(16) -0.0077(14) C2 0.043(2) 0.058(2) 0.038(2) -0.0077(17) 0.0009(16) -0.0194(18) C3 0.0410(19) 0.0260(14) 0.0347(18) 0.0017(13) -0.0024(14) -0.0076(13) C4 0.052(2) 0.0342(17) 0.0353(19) 0.0031(14) -0.0046(16) -0.0071(16) C5 0.086(3) 0.054(2) 0.044(2) 0.0159(19) 0.000(2) -0.030(2) C6 0.092(4) 0.056(3) 0.069(3) 0.018(2) -0.004(3) -0.043(3) C7 0.073(3) 0.044(2) 0.063(3) 0.0036(19) -0.008(2) -0.033(2) C8 0.043(2) 0.0288(15) 0.046(2) -0.0013(14) -0.0038(16) -0.0108(14) C9 0.171(6) 0.096(4) 0.036(3) 0.014(3) -0.030(3) -0.062(4) C10 0.196(7) 0.129(5) 0.048(3) 0.020(3) -0.043(4) -0.117(5) C11 0.078(3) 0.053(2) 0.060(3) -0.028(2) -0.001(2) -0.023(2) C12 0.047(2) 0.058(2) 0.053(2) 0.0020(19) -0.0191(19) -0.0277(19) C13 0.0271(15) 0.0312(15) 0.0260(15) -0.0040(12) -0.0015(12) -0.0106(12) C14 0.0295(16) 0.0342(15) 0.0289(16) -0.0041(13) -0.0026(13) -0.0109(13) C15 0.046(2) 0.0368(17) 0.046(2) -0.0082(16) -0.0117(17) -0.0008(15) C16 0.052(2) 0.0400(19) 0.052(2) 0.0019(17) -0.0205(19) -0.0001(17) C17 0.046(2) 0.053(2) 0.0299(18) 0.0031(15) -0.0125(16) -0.0144(17) C18 0.0371(18) 0.0382(16) 0.0289(17) -0.0044(13) -0.0034(14) -0.0151(14) C19 0.051(3) 0.096(3) 0.049(3) -0.023(2) 0.014(2) -0.031(2) C20 0.067(3) 0.048(2) 0.037(2) -0.0119(16) -0.0084(18) -0.0269(19) C21 0.084(3) 0.078(3) 0.039(2) -0.023(2) -0.002(2) -0.037(3) C22 0.056(2) 0.050(2) 0.051(2) -0.0208(18) 0.0142(19) -0.0196(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn C13 2.105(3) . ? Sn N1 2.115(3) . ? Sn N2 2.131(3) . ? Sn C3 2.138(3) . ? Sn N4 2.416(3) . ? S1 C1 1.600(4) . ? S2 C2 1.594(4) . ? N1 C1 1.150(5) . ? N2 C2 1.143(5) . ? N3 C4 1.361(5) . ? N3 C10 1.363(6) . ? N3 C9 1.459(5) . ? N4 C8 1.460(5) . ? N4 C11 1.476(5) . ? N4 C12 1.487(4) . ? N5 C14 1.453(4) . ? N5 C19 1.462(5) . ? N5 C20 1.470(4) . ? N6 C18 1.417(4) . ? N6 C22 1.453(5) . ? N6 C21 1.463(5) . ? C3 C8 1.397(5) . ? C3 C4 1.427(5) . ? C4 C5 1.414(5) . ? C5 C6 1.367(6) . ? C6 C7 1.377(6) . ? C7 C8 1.375(5) . ? C13 C14 1.386(4) . ? C13 C18 1.411(4) . ? C14 C15 1.393(4) . ? C15 C16 1.377(5) . ? C16 C17 1.387(5) . ? C17 C18 1.399(5) . ? 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 C13 Sn N1 114.71(12) . . ? C13 Sn N2 98.91(12) . . ? N1 Sn N2 83.09(14) . . ? C13 Sn C3 132.40(12) . . ? N1 Sn C3 102.98(12) . . ? N2 Sn C3 114.02(13) . . ? C13 Sn N4 93.28(10) . . ? N1 Sn N4 83.18(12) . . ? N2 Sn N4 164.53(11) . . ? C3 Sn N4 62.53(11) . . ? C1 N1 Sn 153.4(3) . . ? C2 N2 Sn 164.0(3) . . ? C4 N3 C10 125.3(4) . . ? C4 N3 C9 119.8(4) . . ? C10 N3 C9 114.3(4) . . ? C8 N4 C11 113.3(3) . . ? C8 N4 C12 111.7(3) . . ? C11 N4 C12 109.3(3) . . ? C8 N4 Sn 85.86(18) . . ? C11 N4 Sn 121.5(3) . . ? C12 N4 Sn 113.4(2) . . ? C14 N5 C19 112.4(3) . . ? C14 N5 C20 111.6(3) . . ? C19 N5 C20 110.6(3) . . ? C18 N6 C22 113.0(3) . . ? C18 N6 C21 115.4(3) . . ? C22 N6 C21 110.7(3) . . ? N1 C1 S1 177.8(4) . . ? N2 C2 S2 179.0(4) . . ? C8 C3 C4 119.5(3) . . ? C8 C3 Sn 99.0(2) . . ? C4 C3 Sn 141.4(3) . . ? N3 C4 C5 121.3(4) . . ? N3 C4 C3 123.5(3) . . ? C5 C4 C3 115.2(4) . . ? C6 C5 C4 123.1(4) . . ? C5 C6 C7 121.6(4) . . ? C8 C7 C6 117.0(4) . . ? C7 C8 C3 123.5(4) . . ? C7 C8 N4 124.0(3) . . ? C3 C8 N4 112.5(3) . . ? C14 C13 C18 120.1(3) . . ? C14 C13 Sn 108.5(2) . . ? C18 C13 Sn 130.9(2) . . ? C13 C14 C15 121.4(3) . . ? C13 C14 N5 114.6(3) . . ? C15 C14 N5 124.0(3) . . ? C16 C15 C14 118.3(3) . . ? C15 C16 C17 121.5(3) . . ? C16 C17 C18 120.8(3) . . ? C17 C18 C13 117.9(3) . . ? C17 C18 N6 123.7(3) . . ? C13 C18 N6 118.5(3) . . ? #===END