# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Alan H. Cowley' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; 'Kalyan V. Vasudevan' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_email cowley@mail.utexas.edu _publ_contact_author_fax 512-471-6822 _publ_contact_author_phone 512-471-7710 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Alan H. Cowley' _publ_contact_letter ; Please consider this CIF submission for publication in ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; Article Title ; data_kv076b _database_code_depnum_ccdc_archive 'CCDC 812611' #TrackingRef 'kvkv076b.cif' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H72 N4 Pd2 Br4' _chemical_formula_sum 'C62 H72 Br4 Cl0 N4 Pd2' _chemical_formula_weight 1405.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.605(5) _cell_length_b 15.173(5) _cell_length_c 23.927(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 7117(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 2.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .992 _exptl_absorpt_correction_T_max .997 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26799 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.55 _reflns_number_total 8177 _reflns_number_gt 5069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of what appeared to be methylene chloride was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.1068P)^2^+0.9300P] 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_extinction_coef ? _refine_ls_number_reflns 8177 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0786(3) 0.0841(4) 0.0886(2) 0.0361(12) Uani 1 1 d . . . C2 C 1.0765(2) 0.0174(4) 0.0448(2) 0.0387(13) Uani 1 1 d . . . C3 C 1.0107(3) 0.0264(4) 0.0214(2) 0.0360(12) Uani 1 1 d . . . C4 C 0.9673(3) 0.0884(4) 0.0458(2) 0.0377(12) Uani 1 1 d . . . C5 C 1.0105(3) 0.1296(4) 0.0894(2) 0.0365(12) Uani 1 1 d . . . C6 C 0.9023(3) 0.0990(4) 0.0234(2) 0.0402(13) Uani 1 1 d . . . H6 H 0.8733 0.1417 0.0380 0.048 Uiso 1 1 calc R . . C7 C 0.8799(3) 0.0452(4) -0.0216(2) 0.0425(14) Uani 1 1 d . . . H7 H 0.8359 0.0518 -0.0357 0.051 Uiso 1 1 calc R . . C8 C 1.1880(3) 0.0667(4) 0.1288(2) 0.0402(13) Uani 1 1 d . . . C9 C 1.1936(3) -0.0046(4) 0.1643(2) 0.0439(14) Uani 1 1 d . . . C10 C 1.2586(3) -0.0444(5) 0.1676(3) 0.0629(19) Uani 1 1 d . . . H10 H 1.2651 -0.0922 0.1914 0.075 Uiso 1 1 calc R . . C11 C 1.3123(3) -0.0137(6) 0.1363(4) 0.074(2) Uani 1 1 d . . . H11 H 1.3545 -0.0414 0.1385 0.089 Uiso 1 1 calc R . . C12 C 1.3037(3) 0.0588(5) 0.1012(3) 0.070(2) Uani 1 1 d . . . H12 H 1.3403 0.0792 0.0802 0.084 Uiso 1 1 calc R . . C13 C 1.2407(3) 0.1012(4) 0.0975(3) 0.0508(16) Uani 1 1 d . . . C14 C 1.1353(4) -0.0398(5) 0.1990(3) 0.065(2) Uani 1 1 d . . . H14 H 1.0944 -0.0059 0.1892 0.078 Uiso 1 1 calc R . . C15 C 1.1487(6) -0.0259(8) 0.2598(4) 0.121(4) Uani 1 1 d . . . H15A H 1.1072 -0.0340 0.2804 0.181 Uiso 1 1 calc R . . H15B H 1.1654 0.0329 0.2656 0.181 Uiso 1 1 calc R . . H15C H 1.1821 -0.0676 0.2724 0.181 Uiso 1 1 calc R . . C16 C 1.1199(5) -0.1365(6) 0.1874(4) 0.104(3) Uani 1 1 d . . . H16A H 1.1058 -0.1433 0.1492 0.155 Uiso 1 1 calc R . . H16B H 1.0841 -0.1562 0.2117 0.155 Uiso 1 1 calc R . . H16C H 1.1602 -0.1711 0.1940 0.155 Uiso 1 1 calc R . . C17 C 1.2328(4) 0.1801(5) 0.0604(4) 0.073(2) Uani 1 1 d . . . H17 H 1.1872 0.2049 0.0664 0.087 Uiso 1 1 calc R . . C18 C 1.2399(9) 0.1576(9) -0.0009(5) 0.168(7) Uani 1 1 d . . . H18A H 1.2872 0.1490 -0.0097 0.252 Uiso 1 1 calc R . . H18B H 1.2220 0.2049 -0.0231 0.252 Uiso 1 1 calc R . . H18C H 1.2151 0.1045 -0.0088 0.252 Uiso 1 1 calc R . . C19 C 1.2855(6) 0.2520(7) 0.0727(5) 0.122(4) Uani 1 1 d . . . H19A H 1.2796 0.2728 0.1103 0.183 Uiso 1 1 calc R . . H19B H 1.2793 0.3000 0.0471 0.183 Uiso 1 1 calc R . . H19C H 1.3306 0.2282 0.0685 0.183 Uiso 1 1 calc R . . C20 C 0.9347(3) 0.2314(4) 0.1311(2) 0.0372(13) Uani 1 1 d . . . C21 C 0.8836(3) 0.1837(4) 0.1601(3) 0.0474(15) Uani 1 1 d . . . C22 C 0.8203(3) 0.2218(5) 0.1637(3) 0.0611(19) Uani 1 1 d . . . H22 H 0.7853 0.1917 0.1817 0.073 Uiso 1 1 calc R . . C23 C 0.8076(3) 0.3038(6) 0.1411(3) 0.069(2) Uani 1 1 d . . . H23 H 0.7647 0.3292 0.1447 0.083 Uiso 1 1 calc R . . C24 C 0.8594(4) 0.3487(5) 0.1128(3) 0.067(2) Uani 1 1 d . . . H24 H 0.8502 0.4036 0.0973 0.080 Uiso 1 1 calc R . . C25 C 0.9235(3) 0.3135(4) 0.1074(3) 0.0431(14) Uani 1 1 d . . . C26 C 0.8989(3) 0.0970(4) 0.1909(3) 0.0574(17) Uani 1 1 d . . . H26 H 0.9387 0.0704 0.1728 0.069 Uiso 1 1 calc R . . C27 C 0.8410(5) 0.0311(5) 0.1869(4) 0.096(3) Uani 1 1 d . . . H27A H 0.8000 0.0571 0.2013 0.144 Uiso 1 1 calc R . . H27B H 0.8521 -0.0204 0.2083 0.144 Uiso 1 1 calc R . . H27C H 0.8343 0.0148 0.1485 0.144 Uiso 1 1 calc R . . C28 C 0.9181(6) 0.1151(6) 0.2504(4) 0.103(3) Uani 1 1 d . . . H28A H 0.9573 0.1531 0.2514 0.154 Uiso 1 1 calc R . . H28B H 0.9288 0.0605 0.2688 0.154 Uiso 1 1 calc R . . H28C H 0.8807 0.1431 0.2692 0.154 Uiso 1 1 calc R . . C29 C 0.9807(4) 0.3604(4) 0.0750(3) 0.0535(16) Uani 1 1 d . . . H29 H 1.0242 0.3366 0.0884 0.064 Uiso 1 1 calc R . . C30 C 0.9759(5) 0.3409(6) 0.0133(3) 0.083(2) Uani 1 1 d . . . H30A H 0.9309 0.3547 0.0002 0.124 Uiso 1 1 calc R . . H30B H 0.9851 0.2796 0.0069 0.124 Uiso 1 1 calc R . . H30C H 1.0087 0.3760 -0.0065 0.124 Uiso 1 1 calc R . . C31 C 0.9816(4) 0.4600(5) 0.0854(4) 0.082(2) Uani 1 1 d . . . H31A H 0.9407 0.4858 0.0706 0.124 Uiso 1 1 calc R . . H31B H 1.0205 0.4855 0.0673 0.124 Uiso 1 1 calc R . . H31C H 0.9840 0.4711 0.1248 0.124 Uiso 1 1 calc R . . N1 N 1.1218(2) 0.1104(3) 0.12565(17) 0.0346(10) Uani 1 1 d . . . N2 N 1.0014(2) 0.1918(3) 0.12536(18) 0.0355(10) Uani 1 1 d . . . Br1 Br 1.19032(3) 0.22715(4) 0.22613(3) 0.0519(2) Uani 1 1 d . . . Br2 Br 1.04165(3) 0.34143(5) 0.21953(3) 0.0579(2) Uani 1 1 d . . . Pd1 Pd 1.08758(2) 0.21491(3) 0.173011(17) 0.03710(16) Uani 1 1 d . . . 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 C1 0.033(3) 0.042(3) 0.033(3) -0.001(2) -0.004(2) 0.003(2) C2 0.030(3) 0.060(4) 0.026(3) 0.001(3) -0.001(2) 0.005(3) C3 0.032(3) 0.048(3) 0.028(3) -0.002(2) -0.005(2) 0.007(2) C4 0.035(3) 0.050(3) 0.028(3) -0.005(3) -0.001(2) 0.000(3) C5 0.033(3) 0.048(3) 0.029(3) -0.002(3) 0.004(2) -0.001(2) C6 0.033(3) 0.048(3) 0.039(3) -0.004(3) -0.004(2) 0.009(2) C7 0.034(3) 0.063(4) 0.031(3) -0.007(3) -0.005(2) 0.006(3) C8 0.038(3) 0.053(3) 0.030(3) -0.008(3) -0.004(2) 0.000(3) C9 0.039(3) 0.059(4) 0.034(3) 0.004(3) -0.002(2) 0.002(3) C10 0.061(4) 0.078(5) 0.050(4) 0.018(4) -0.012(3) 0.016(4) C11 0.032(3) 0.102(6) 0.089(6) -0.006(5) -0.007(4) 0.015(4) C12 0.044(4) 0.083(5) 0.082(6) -0.012(5) 0.013(4) -0.008(4) C13 0.035(3) 0.064(4) 0.053(4) -0.003(3) 0.008(3) -0.005(3) C14 0.060(4) 0.085(5) 0.050(4) 0.031(4) 0.006(3) 0.004(4) C15 0.157(10) 0.147(9) 0.059(6) 0.008(6) 0.018(6) -0.070(8) C16 0.103(7) 0.113(8) 0.094(7) -0.024(6) 0.039(6) -0.053(6) C17 0.059(4) 0.070(5) 0.089(6) 0.015(4) 0.020(4) -0.004(4) C18 0.277(19) 0.155(12) 0.071(7) 0.029(8) -0.032(10) -0.091(11) C19 0.168(12) 0.095(7) 0.104(9) 0.005(6) 0.032(8) -0.030(7) C20 0.036(3) 0.051(4) 0.024(3) -0.009(2) 0.002(2) 0.000(3) C21 0.046(3) 0.054(4) 0.042(4) -0.010(3) 0.011(3) -0.005(3) C22 0.051(4) 0.065(5) 0.067(5) -0.011(4) 0.031(3) -0.006(3) C23 0.040(4) 0.087(6) 0.081(6) -0.014(5) 0.010(4) 0.005(4) C24 0.059(4) 0.062(4) 0.079(5) 0.001(4) -0.006(4) 0.014(4) C25 0.040(3) 0.051(4) 0.038(3) -0.001(3) -0.001(2) 0.008(3) C26 0.067(4) 0.050(4) 0.056(4) 0.004(3) 0.024(3) 0.004(3) C27 0.128(7) 0.060(5) 0.101(7) 0.000(5) 0.011(6) -0.033(5) C28 0.155(9) 0.081(6) 0.072(6) 0.015(5) -0.026(6) -0.005(6) C29 0.064(4) 0.050(4) 0.046(4) 0.010(3) 0.003(3) 0.002(3) C30 0.106(6) 0.095(6) 0.047(5) 0.021(4) 0.012(4) -0.009(5) C31 0.087(6) 0.068(5) 0.092(7) 0.017(5) 0.003(5) -0.006(4) N1 0.032(2) 0.051(3) 0.021(2) 0.001(2) -0.0023(17) 0.001(2) N2 0.034(2) 0.041(3) 0.031(2) 0.000(2) 0.0011(19) 0.001(2) Br1 0.0464(4) 0.0663(5) 0.0430(4) -0.0084(3) -0.0131(3) -0.0044(3) Br2 0.0546(4) 0.0640(5) 0.0552(4) -0.0232(3) 0.0005(3) 0.0002(3) Pd1 0.0356(2) 0.0489(3) 0.0268(2) -0.00427(18) -0.00038(17) -0.00333(18) _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 C1 N1 1.288(7) . ? C1 C2 1.459(8) . ? C1 C5 1.503(7) . ? C2 C7 1.393(8) 5_755 ? C2 C3 1.414(7) . ? C3 C3 1.366(10) 5_755 ? C3 C4 1.396(7) . ? C4 C6 1.391(7) . ? C4 C5 1.482(7) . ? C5 N2 1.289(7) . ? C6 C7 1.422(8) . ? C6 H6 0.9300 . ? C7 C2 1.393(8) 5_755 ? C7 H7 0.9300 . ? C8 C9 1.380(8) . ? C8 C13 1.380(8) . ? C8 N1 1.460(7) . ? C9 C10 1.411(8) . ? C9 C14 1.511(8) . ? C10 C11 1.374(10) . ? C10 H10 0.9300 . ? C11 C12 1.394(11) . ? C11 H11 0.9300 . ? C12 C13 1.394(9) . ? C12 H12 0.9300 . ? C13 C17 1.499(10) . ? C14 C15 1.494(11) . ? C14 C16 1.524(11) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.512(15) . ? C17 C19 1.530(12) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C25 1.387(8) . ? C20 C21 1.416(8) . ? C20 N2 1.446(7) . ? C21 C22 1.372(9) . ? C21 C26 1.537(9) . ? C22 C23 1.380(11) . ? C22 H22 0.9300 . ? C23 C24 1.397(10) . ? C23 H23 0.9300 . ? C24 C25 1.371(9) . ? C24 H24 0.9300 . ? C25 C29 1.537(9) . ? C26 C28 1.498(12) . ? C26 C27 1.517(10) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.509(10) . ? C29 C31 1.532(10) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 Pd1 2.061(4) . ? N2 Pd1 2.068(4) . ? Br1 Pd1 2.3889(8) . ? Br2 Pd1 2.3949(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 136.7(5) . . ? N1 C1 C5 115.7(5) . . ? C2 C1 C5 107.6(4) . . ? C7 C2 C3 118.0(5) 5_755 . ? C7 C2 C1 137.9(5) 5_755 . ? C3 C2 C1 104.1(4) . . ? C3 C3 C4 121.5(6) 5_755 . ? C3 C3 C2 121.3(6) 5_755 . ? C4 C3 C2 117.1(5) . . ? C6 C4 C3 118.3(5) . . ? C6 C4 C5 138.2(5) . . ? C3 C4 C5 103.3(4) . . ? N2 C5 C4 134.4(5) . . ? N2 C5 C1 117.9(5) . . ? C4 C5 C1 107.8(5) . . ? C4 C6 C7 120.6(5) . . ? C4 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 120.2(5) 5_755 . ? C2 C7 H7 119.9 5_755 . ? C6 C7 H7 119.9 . . ? C9 C8 C13 124.8(5) . . ? C9 C8 N1 117.4(5) . . ? C13 C8 N1 117.8(5) . . ? C8 C9 C10 116.3(5) . . ? C8 C9 C14 123.6(5) . . ? C10 C9 C14 120.0(6) . . ? C11 C10 C9 121.0(6) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 120.2(6) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.7(7) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C8 C13 C12 116.9(6) . . ? C8 C13 C17 123.2(6) . . ? C12 C13 C17 119.9(6) . . ? C15 C14 C9 110.6(6) . . ? C15 C14 C16 110.4(7) . . ? C9 C14 C16 113.0(6) . . ? C15 C14 H14 107.6 . . ? C9 C14 H14 107.6 . . ? C16 C14 H14 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 112.6(8) . . ? C13 C17 C19 112.7(8) . . ? C18 C17 C19 106.6(8) . . ? C13 C17 H17 108.3 . . ? C18 C17 H17 108.3 . . ? C19 C17 H17 108.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 123.2(5) . . ? C25 C20 N2 118.6(5) . . ? C21 C20 N2 118.2(5) . . ? C22 C21 C20 117.0(6) . . ? C22 C21 C26 120.4(6) . . ? C20 C21 C26 122.3(6) . . ? C21 C22 C23 121.3(6) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 119.9(6) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 121.5(7) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C20 117.1(6) . . ? C24 C25 C29 122.4(6) . . ? C20 C25 C29 120.4(5) . . ? C28 C26 C27 111.6(7) . . ? C28 C26 C21 110.4(6) . . ? C27 C26 C21 112.8(6) . . ? C28 C26 H26 107.2 . . ? C27 C26 H26 107.2 . . ? C21 C26 H26 107.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C31 110.6(6) . . ? C30 C29 C25 111.0(6) . . ? C31 C29 C25 112.5(6) . . ? C30 C29 H29 107.5 . . ? C31 C29 H29 107.5 . . ? C25 C29 H29 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 N1 C8 118.6(4) . . ? C1 N1 Pd1 113.7(3) . . ? C8 N1 Pd1 127.7(3) . . ? C5 N2 C20 119.5(4) . . ? C5 N2 Pd1 112.3(3) . . ? C20 N2 Pd1 128.1(3) . . ? N1 Pd1 N2 80.32(17) . . ? N1 Pd1 Br1 94.48(11) . . ? N2 Pd1 Br1 174.41(13) . . ? N1 Pd1 Br2 174.02(12) . . ? N2 Pd1 Br2 94.89(13) . . ? Br1 Pd1 Br2 90.42(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C7 -3.2(13) . . . 5_755 ? C5 C1 C2 C7 178.9(7) . . . 5_755 ? N1 C1 C2 C3 179.0(6) . . . . ? C5 C1 C2 C3 1.1(6) . . . . ? C7 C2 C3 C3 2.2(10) 5_755 . . 5_755 ? C1 C2 C3 C3 -179.5(7) . . . 5_755 ? C7 C2 C3 C4 178.9(5) 5_755 . . . ? C1 C2 C3 C4 -2.8(7) . . . . ? C3 C3 C4 C6 -3.7(10) 5_755 . . . ? C2 C3 C4 C6 179.6(5) . . . . ? C3 C3 C4 C5 179.9(7) 5_755 . . . ? C2 C3 C4 C5 3.2(7) . . . . ? C6 C4 C5 N2 3.1(12) . . . . ? C3 C4 C5 N2 178.4(6) . . . . ? C6 C4 C5 C1 -177.5(7) . . . . ? C3 C4 C5 C1 -2.2(6) . . . . ? N1 C1 C5 N2 1.8(8) . . . . ? C2 C1 C5 N2 -179.8(5) . . . . ? N1 C1 C5 C4 -177.8(5) . . . . ? C2 C1 C5 C4 0.7(6) . . . . ? C3 C4 C6 C7 2.8(9) . . . . ? C5 C4 C6 C7 177.6(6) . . . . ? C4 C6 C7 C2 -1.7(9) . . . 5_755 ? C13 C8 C9 C10 -0.7(9) . . . . ? N1 C8 C9 C10 -178.5(5) . . . . ? C13 C8 C9 C14 178.6(6) . . . . ? N1 C8 C9 C14 0.9(9) . . . . ? C8 C9 C10 C11 -0.9(10) . . . . ? C14 C9 C10 C11 179.7(7) . . . . ? C9 C10 C11 C12 1.2(12) . . . . ? C10 C11 C12 C13 0.1(12) . . . . ? C9 C8 C13 C12 1.9(10) . . . . ? N1 C8 C13 C12 179.6(5) . . . . ? C9 C8 C13 C17 -178.5(6) . . . . ? N1 C8 C13 C17 -0.8(9) . . . . ? C11 C12 C13 C8 -1.5(10) . . . . ? C11 C12 C13 C17 178.9(7) . . . . ? C8 C9 C14 C15 -113.3(8) . . . . ? C10 C9 C14 C15 66.0(10) . . . . ? C8 C9 C14 C16 122.4(8) . . . . ? C10 C9 C14 C16 -58.3(9) . . . . ? C8 C13 C17 C18 -112.7(10) . . . . ? C12 C13 C17 C18 66.9(11) . . . . ? C8 C13 C17 C19 126.6(8) . . . . ? C12 C13 C17 C19 -53.8(10) . . . . ? C25 C20 C21 C22 0.8(9) . . . . ? N2 C20 C21 C22 -178.4(5) . . . . ? C25 C20 C21 C26 -173.9(6) . . . . ? N2 C20 C21 C26 6.9(8) . . . . ? C20 C21 C22 C23 -1.4(10) . . . . ? C26 C21 C22 C23 173.3(7) . . . . ? C21 C22 C23 C24 1.5(12) . . . . ? C22 C23 C24 C25 -0.8(12) . . . . ? C23 C24 C25 C20 0.2(10) . . . . ? C23 C24 C25 C29 178.2(7) . . . . ? C21 C20 C25 C24 -0.1(9) . . . . ? N2 C20 C25 C24 179.1(5) . . . . ? C21 C20 C25 C29 -178.2(5) . . . . ? N2 C20 C25 C29 1.0(8) . . . . ? C22 C21 C26 C28 -83.8(9) . . . . ? C20 C21 C26 C28 90.6(8) . . . . ? C22 C21 C26 C27 41.9(9) . . . . ? C20 C21 C26 C27 -143.7(7) . . . . ? C24 C25 C29 C30 -84.2(8) . . . . ? C20 C25 C29 C30 93.8(7) . . . . ? C24 C25 C29 C31 40.4(9) . . . . ? C20 C25 C29 C31 -141.6(6) . . . . ? C2 C1 N1 C8 -0.2(10) . . . . ? C5 C1 N1 C8 177.5(4) . . . . ? C2 C1 N1 Pd1 178.2(6) . . . . ? C5 C1 N1 Pd1 -4.0(6) . . . . ? C9 C8 N1 C1 -91.0(6) . . . . ? C13 C8 N1 C1 91.1(7) . . . . ? C9 C8 N1 Pd1 90.8(6) . . . . ? C13 C8 N1 Pd1 -87.1(6) . . . . ? C4 C5 N2 C20 5.3(9) . . . . ? C1 C5 N2 C20 -174.1(5) . . . . ? C4 C5 N2 Pd1 -179.2(5) . . . . ? C1 C5 N2 Pd1 1.4(6) . . . . ? C25 C20 N2 C5 -103.0(6) . . . . ? C21 C20 N2 C5 76.3(7) . . . . ? C25 C20 N2 Pd1 82.3(6) . . . . ? C21 C20 N2 Pd1 -98.5(5) . . . . ? C1 N1 Pd1 N2 3.7(4) . . . . ? C8 N1 Pd1 N2 -178.0(5) . . . . ? C1 N1 Pd1 Br1 -178.4(4) . . . . ? C8 N1 Pd1 Br1 -0.1(4) . . . . ? C1 N1 Pd1 Br2 -33.3(14) . . . . ? C8 N1 Pd1 Br2 145.0(10) . . . . ? C5 N2 Pd1 N1 -2.6(4) . . . . ? C20 N2 Pd1 N1 172.4(5) . . . . ? C5 N2 Pd1 Br1 -24.6(15) . . . . ? C20 N2 Pd1 Br1 150.4(10) . . . . ? C5 N2 Pd1 Br2 173.8(4) . . . . ? C20 N2 Pd1 Br2 -11.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.508 _refine_diff_density_min -1.527 _refine_diff_density_rms 0.131 # Attachment 'kvkv083sq.cif' data_kvkv083sq _database_code_depnum_ccdc_archive 'CCDC 812612' #TrackingRef 'kvkv083sq.cif' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H72 Cl4 N4 Pd2, 2 (C H2 Cl2)' _chemical_formula_sum 'C64 H76 Cl8 N4 Pd2' _chemical_formula_weight 1397.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M pbca _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.460(5) _cell_length_b 15.257(5) _cell_length_c 23.428(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 6956(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25734 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7958 _reflns_number_gt 4583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A disordered molecule of dichloromethane solvent was removed using SQUEEZE. This process has resulted in a number of associated A alerts. ; _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^)+(0.0763P)^2^+0.0000P] 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_extinction_coef ? _refine_ls_number_reflns 7958 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.57979(19) 0.0843(3) 0.58991(16) 0.0221(9) Uani 1 1 d . . . C2 C 0.57738(19) 0.0170(3) 0.54499(16) 0.0232(9) Uani 1 1 d . . . C3 C 0.5107(2) 0.0266(3) 0.52170(16) 0.0226(9) Uani 1 1 d . . . C4 C 0.4682(2) 0.0907(3) 0.54543(16) 0.0229(9) Uani 1 1 d . . . C5 C 0.5115(2) 0.1306(3) 0.58985(15) 0.0201(9) Uani 1 1 d . . . C6 C 0.4022(2) 0.1007(3) 0.52321(17) 0.0258(10) Uani 1 1 d . . . H6 H 0.3729 0.1430 0.5381 0.031 Uiso 1 1 calc R . . C7 C 0.3796(2) 0.0458(3) 0.47755(17) 0.0263(10) Uani 1 1 d . . . H7 H 0.3355 0.0525 0.4629 0.032 Uiso 1 1 calc R . . C8 C 0.68791(19) 0.0631(3) 0.63190(16) 0.0229(9) Uani 1 1 d . . . C9 C 0.7450(2) 0.0945(3) 0.60227(19) 0.0375(12) Uani 1 1 d . . . C10 C 0.8062(2) 0.0477(4) 0.6084(3) 0.0557(16) Uani 1 1 d . . . H10 H 0.8453 0.0670 0.5893 0.067 Uiso 1 1 calc R . . C11 C 0.8104(3) -0.0251(4) 0.6413(3) 0.0548(16) Uani 1 1 d . . . H11 H 0.8518 -0.0551 0.6443 0.066 Uiso 1 1 calc R . . C12 C 0.7540(3) -0.0545(3) 0.6701(2) 0.0478(14) Uani 1 1 d . . . H12 H 0.7577 -0.1045 0.6926 0.057 Uiso 1 1 calc R . . C13 C 0.6906(2) -0.0109(3) 0.66659(18) 0.0314(11) Uani 1 1 d . . . C14 C 0.7397(3) 0.1768(4) 0.5650(3) 0.0650(17) Uani 1 1 d . . . H14 H 0.6955 0.2051 0.5730 0.078 Uiso 1 1 calc R . . C15 C 0.7416(5) 0.1536(6) 0.5031(3) 0.121(3) Uani 1 1 d . . . H15A H 0.7870 0.1345 0.4930 0.182 Uiso 1 1 calc R . . H15B H 0.7296 0.2040 0.4807 0.182 Uiso 1 1 calc R . . H15C H 0.7094 0.1072 0.4957 0.182 Uiso 1 1 calc R . . C16 C 0.7981(4) 0.2428(5) 0.5802(4) 0.109(3) Uani 1 1 d . . . H16A H 0.7968 0.2552 0.6203 0.164 Uiso 1 1 calc R . . H16B H 0.7916 0.2961 0.5591 0.164 Uiso 1 1 calc R . . H16C H 0.8418 0.2176 0.5705 0.164 Uiso 1 1 calc R . . C17 C 0.6283(3) -0.0407(4) 0.7010(2) 0.0583(16) Uani 1 1 d . . . H17 H 0.5878 -0.0130 0.6839 0.070 Uiso 1 1 calc R . . C18 C 0.6331(5) -0.0084(5) 0.7626(3) 0.107(3) Uani 1 1 d . . . H18A H 0.6749 -0.0293 0.7795 0.161 Uiso 1 1 calc R . . H18B H 0.5945 -0.0301 0.7839 0.161 Uiso 1 1 calc R . . H18C H 0.6327 0.0545 0.7631 0.161 Uiso 1 1 calc R . . C19 C 0.6171(4) -0.1406(4) 0.6981(3) 0.085(2) Uani 1 1 d . . . H19A H 0.6169 -0.1590 0.6589 0.127 Uiso 1 1 calc R . . H19B H 0.5739 -0.1551 0.7154 0.127 Uiso 1 1 calc R . . H19C H 0.6535 -0.1698 0.7181 0.127 Uiso 1 1 calc R . . C20 C 0.4365(2) 0.2320(3) 0.63374(17) 0.0242(10) Uani 1 1 d . . . C21 C 0.4252(2) 0.3140(3) 0.61007(19) 0.0288(10) Uani 1 1 d . . . C22 C 0.3605(2) 0.3497(4) 0.6163(2) 0.0454(13) Uani 1 1 d . . . H22 H 0.3512 0.4046 0.6008 0.054 Uiso 1 1 calc R . . C23 C 0.3087(3) 0.3048(4) 0.6452(2) 0.0533(15) Uani 1 1 d . . . H23 H 0.2651 0.3292 0.6486 0.064 Uiso 1 1 calc R . . C24 C 0.3225(3) 0.2241(4) 0.6689(2) 0.0470(14) Uani 1 1 d . . . H24 H 0.2878 0.1952 0.6887 0.056 Uiso 1 1 calc R . . C25 C 0.3862(3) 0.1845(3) 0.66413(19) 0.0361(11) Uani 1 1 d . . . C26 C 0.4821(2) 0.3610(3) 0.5773(2) 0.0404(12) Uani 1 1 d . . . H26 H 0.5258 0.3356 0.5899 0.048 Uiso 1 1 calc R . . C27 C 0.4754(3) 0.3421(4) 0.5127(2) 0.0642(17) Uani 1 1 d . . . H27A H 0.4804 0.2803 0.5061 0.096 Uiso 1 1 calc R . . H27B H 0.5106 0.3732 0.4924 0.096 Uiso 1 1 calc R . . H27C H 0.4311 0.3609 0.4996 0.096 Uiso 1 1 calc R . . C28 C 0.4853(3) 0.4596(3) 0.5900(2) 0.0577(15) Uani 1 1 d . . . H28A H 0.4416 0.4859 0.5816 0.087 Uiso 1 1 calc R . . H28B H 0.5201 0.4862 0.5667 0.087 Uiso 1 1 calc R . . H28C H 0.4962 0.4685 0.6295 0.087 Uiso 1 1 calc R . . C29 C 0.4015(3) 0.0983(4) 0.6937(2) 0.0540(15) Uani 1 1 d . . . H29 H 0.4396 0.0702 0.6734 0.065 Uiso 1 1 calc R . . C30 C 0.4248(4) 0.1154(5) 0.7555(3) 0.087(2) Uani 1 1 d . . . H30A H 0.4600 0.1594 0.7557 0.131 Uiso 1 1 calc R . . H30B H 0.4425 0.0622 0.7717 0.131 Uiso 1 1 calc R . . H30C H 0.3864 0.1352 0.7777 0.131 Uiso 1 1 calc R . . C31 C 0.3394(4) 0.0347(4) 0.6924(3) 0.096(2) Uani 1 1 d . . . H31A H 0.3023 0.0590 0.7143 0.145 Uiso 1 1 calc R . . H31B H 0.3527 -0.0207 0.7085 0.145 Uiso 1 1 calc R . . H31C H 0.3248 0.0263 0.6537 0.145 Uiso 1 1 calc R . . N1 N 0.62380(16) 0.1095(2) 0.62710(13) 0.0209(8) Uani 1 1 d . . . N2 N 0.50379(16) 0.1922(2) 0.62701(13) 0.0220(8) Uani 1 1 d . . . Cl1 Cl 0.69040(6) 0.22675(8) 0.72399(5) 0.0365(3) Uani 1 1 d . . . Cl2 Cl 0.54742(6) 0.33516(8) 0.71811(5) 0.0394(3) Uani 1 1 d . . . Pd1 Pd 0.590759(15) 0.21447(2) 0.674316(13) 0.02246(12) Uani 1 1 d . . . 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 C1 0.019(2) 0.027(2) 0.020(2) 0.0007(19) -0.0006(17) 0.0056(18) C2 0.023(2) 0.028(2) 0.019(2) -0.0039(19) -0.0060(17) 0.0008(19) C3 0.024(2) 0.026(2) 0.0175(19) 0.0004(17) -0.0028(18) 0.0014(19) C4 0.027(2) 0.022(2) 0.020(2) -0.0064(18) -0.0001(18) 0.0035(19) C5 0.024(2) 0.022(2) 0.0137(19) -0.0003(17) -0.0026(17) -0.0004(19) C6 0.027(2) 0.023(2) 0.028(2) -0.0079(19) 0.0007(19) 0.010(2) C7 0.022(2) 0.026(2) 0.030(2) -0.006(2) -0.0087(19) 0.005(2) C8 0.020(2) 0.028(2) 0.021(2) -0.0040(19) -0.0052(17) 0.0009(19) C9 0.029(3) 0.040(3) 0.043(3) -0.006(2) 0.005(2) -0.007(2) C10 0.023(3) 0.057(4) 0.087(4) -0.012(3) 0.014(3) -0.001(3) C11 0.025(3) 0.055(4) 0.084(4) -0.008(3) -0.001(3) 0.012(3) C12 0.057(3) 0.035(3) 0.052(3) 0.004(3) -0.022(3) 0.020(3) C13 0.034(3) 0.035(3) 0.025(2) 0.003(2) -0.0029(19) 0.005(2) C14 0.054(4) 0.057(4) 0.084(5) 0.021(4) 0.032(3) -0.009(3) C15 0.176(9) 0.122(7) 0.066(5) 0.039(5) -0.005(5) -0.052(7) C16 0.120(7) 0.057(4) 0.150(8) -0.006(5) 0.075(6) -0.036(4) C17 0.052(3) 0.061(4) 0.061(4) 0.033(3) 0.020(3) 0.020(3) C18 0.187(8) 0.075(5) 0.060(4) 0.008(4) 0.059(5) -0.012(6) C19 0.085(5) 0.071(5) 0.099(5) 0.015(4) 0.032(4) -0.027(4) C20 0.024(2) 0.030(3) 0.019(2) -0.0085(19) 0.0006(18) -0.0012(19) C21 0.023(2) 0.034(3) 0.029(2) -0.004(2) 0.0005(19) 0.005(2) C22 0.036(3) 0.044(3) 0.056(3) -0.006(3) -0.002(3) 0.013(3) C23 0.025(3) 0.062(4) 0.072(4) -0.023(3) 0.007(3) 0.008(3) C24 0.033(3) 0.052(4) 0.056(3) -0.012(3) 0.025(2) -0.006(3) C25 0.040(3) 0.034(3) 0.034(3) -0.012(2) 0.008(2) -0.004(2) C26 0.040(3) 0.035(3) 0.047(3) 0.021(2) 0.002(2) 0.003(2) C27 0.076(4) 0.075(5) 0.041(3) 0.005(3) 0.011(3) -0.009(4) C28 0.068(4) 0.034(3) 0.071(4) 0.014(3) 0.011(3) -0.004(3) C29 0.061(4) 0.038(3) 0.062(4) 0.009(3) 0.038(3) -0.003(3) C30 0.123(6) 0.070(5) 0.068(5) 0.029(4) -0.016(4) -0.020(4) C31 0.128(6) 0.061(5) 0.100(5) 0.010(4) 0.004(5) -0.050(5) N1 0.0203(17) 0.027(2) 0.0155(16) -0.0019(15) 0.0024(14) 0.0010(16) N2 0.0220(18) 0.025(2) 0.0186(16) 0.0015(15) 0.0027(14) -0.0015(15) Cl1 0.0354(6) 0.0380(7) 0.0360(6) -0.0045(5) -0.0111(5) -0.0055(5) Cl2 0.0398(7) 0.0370(7) 0.0414(7) -0.0182(6) 0.0001(5) 0.0007(6) Pd1 0.02482(19) 0.02397(19) 0.01858(17) -0.00324(14) -0.00008(14) -0.00269(15) _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 C1 N1 1.281(5) . ? C1 C2 1.471(6) . ? C1 C5 1.506(5) . ? C2 C7 1.378(6) 5_656 ? C2 C3 1.416(5) . ? C3 C3 1.365(8) 5_656 ? C3 C4 1.397(5) . ? C4 C6 1.394(5) . ? C4 C5 1.470(5) . ? C5 N2 1.290(5) . ? C6 C7 1.428(5) . ? C6 H6 0.9300 . ? C7 C2 1.378(6) 5_656 ? C7 H7 0.9300 . ? C8 C13 1.392(6) . ? C8 C9 1.396(6) . ? C8 N1 1.439(5) . ? C9 C10 1.396(7) . ? C9 C14 1.533(7) . ? C10 C11 1.355(8) . ? C10 H10 0.9300 . ? C11 C12 1.363(7) . ? C11 H11 0.9300 . ? C12 C13 1.404(6) . ? C12 H12 0.9300 . ? C13 C17 1.526(6) . ? C14 C15 1.493(9) . ? C14 C16 1.558(9) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.527(8) . ? C17 C19 1.540(8) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.386(6) . ? C20 C25 1.412(6) . ? C20 N2 1.451(5) . ? C21 C22 1.380(6) . ? C21 C26 1.525(6) . ? C22 C23 1.395(7) . ? C22 H22 0.9300 . ? C23 C24 1.377(8) . ? C23 H23 0.9300 . ? C24 C25 1.383(7) . ? C24 H24 0.9300 . ? C25 C29 1.516(7) . ? C26 C28 1.536(7) . ? C26 C27 1.546(7) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.540(8) . ? C29 C31 1.549(8) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 Pd1 2.050(3) . ? N2 Pd1 2.051(3) . ? Cl1 Pd1 2.2692(12) . ? Cl2 Pd1 2.2703(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 135.9(4) . . ? N1 C1 C5 116.8(4) . . ? C2 C1 C5 107.4(3) . . ? C7 C2 C3 118.7(4) 5_656 . ? C7 C2 C1 137.8(4) 5_656 . ? C3 C2 C1 103.5(3) . . ? C3 C3 C4 122.2(5) 5_656 . ? C3 C3 C2 120.3(5) 5_656 . ? C4 C3 C2 117.5(4) . . ? C6 C4 C3 118.2(4) . . ? C6 C4 C5 138.3(4) . . ? C3 C4 C5 103.5(3) . . ? N2 C5 C4 135.5(4) . . ? N2 C5 C1 116.3(3) . . ? C4 C5 C1 108.2(3) . . ? C4 C6 C7 120.0(4) . . ? C4 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 120.5(4) 5_656 . ? C2 C7 H7 119.7 5_656 . ? C6 C7 H7 119.7 . . ? C13 C8 C9 122.6(4) . . ? C13 C8 N1 118.5(4) . . ? C9 C8 N1 118.8(4) . . ? C8 C9 C10 116.9(5) . . ? C8 C9 C14 120.7(4) . . ? C10 C9 C14 122.4(4) . . ? C11 C10 C9 121.9(5) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C10 C11 C12 120.2(5) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 121.5(5) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 116.8(4) . . ? C8 C13 C17 121.3(4) . . ? C12 C13 C17 121.8(4) . . ? C15 C14 C9 110.9(5) . . ? C15 C14 C16 111.0(5) . . ? C9 C14 C16 110.4(6) . . ? C15 C14 H14 108.1 . . ? C9 C14 H14 108.1 . . ? C16 C14 H14 108.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 110.8(5) . . ? C13 C17 C19 112.6(5) . . ? C18 C17 C19 111.7(5) . . ? C13 C17 H17 107.2 . . ? C18 C17 H17 107.2 . . ? C19 C17 H17 107.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 123.7(4) . . ? C21 C20 N2 118.5(4) . . ? C25 C20 N2 117.7(4) . . ? C22 C21 C20 117.3(4) . . ? C22 C21 C26 122.0(4) . . ? C20 C21 C26 120.6(4) . . ? C21 C22 C23 121.1(5) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 119.6(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 122.2(5) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C20 116.0(5) . . ? C24 C25 C29 121.2(4) . . ? C20 C25 C29 122.7(4) . . ? C21 C26 C28 113.1(4) . . ? C21 C26 C27 110.1(4) . . ? C28 C26 C27 112.0(4) . . ? C21 C26 H26 107.1 . . ? C28 C26 H26 107.1 . . ? C27 C26 H26 107.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 C30 109.9(5) . . ? C25 C29 C31 112.4(5) . . ? C30 C29 C31 110.7(5) . . ? C25 C29 H29 107.9 . . ? C30 C29 H29 107.9 . . ? C31 C29 H29 107.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 N1 C8 119.0(3) . . ? C1 N1 Pd1 113.1(3) . . ? C8 N1 Pd1 127.9(2) . . ? C5 N2 C20 118.8(3) . . ? C5 N2 Pd1 112.9(3) . . ? C20 N2 Pd1 128.0(2) . . ? N1 Pd1 N2 80.68(13) . . ? N1 Pd1 Cl1 94.20(9) . . ? N2 Pd1 Cl1 174.73(10) . . ? N1 Pd1 Cl2 173.74(9) . . ? N2 Pd1 Cl2 94.11(10) . . ? Cl1 Pd1 Cl2 91.07(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C7 -1.9(9) . . . 5_656 ? C5 C1 C2 C7 179.4(5) . . . 5_656 ? N1 C1 C2 C3 178.7(5) . . . . ? C5 C1 C2 C3 0.0(4) . . . . ? C7 C2 C3 C3 1.0(7) 5_656 . . 5_656 ? C1 C2 C3 C3 -179.5(5) . . . 5_656 ? C7 C2 C3 C4 180.0(4) 5_656 . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C3 C3 C4 C6 -0.7(7) 5_656 . . . ? C2 C3 C4 C6 -179.7(4) . . . . ? C3 C3 C4 C5 179.8(5) 5_656 . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C6 C4 C5 N2 0.8(9) . . . . ? C3 C4 C5 N2 -179.8(4) . . . . ? C6 C4 C5 C1 179.9(5) . . . . ? C3 C4 C5 C1 -0.7(4) . . . . ? N1 C1 C5 N2 0.7(5) . . . . ? C2 C1 C5 N2 179.7(3) . . . . ? N1 C1 C5 C4 -178.6(3) . . . . ? C2 C1 C5 C4 0.5(4) . . . . ? C3 C4 C6 C7 0.2(6) . . . . ? C5 C4 C6 C7 179.6(4) . . . . ? C4 C6 C7 C2 -0.2(6) . . . 5_656 ? C13 C8 C9 C10 0.6(7) . . . . ? N1 C8 C9 C10 179.7(4) . . . . ? C13 C8 C9 C14 -179.5(4) . . . . ? N1 C8 C9 C14 -0.3(6) . . . . ? C8 C9 C10 C11 0.1(8) . . . . ? C14 C9 C10 C11 -179.8(5) . . . . ? C9 C10 C11 C12 -0.4(9) . . . . ? C10 C11 C12 C13 0.1(8) . . . . ? C9 C8 C13 C12 -0.9(6) . . . . ? N1 C8 C13 C12 179.9(4) . . . . ? C9 C8 C13 C17 176.5(5) . . . . ? N1 C8 C13 C17 -2.6(6) . . . . ? C11 C12 C13 C8 0.6(7) . . . . ? C11 C12 C13 C17 -176.9(5) . . . . ? C8 C9 C14 C15 -107.2(6) . . . . ? C10 C9 C14 C15 72.7(7) . . . . ? C8 C9 C14 C16 129.3(5) . . . . ? C10 C9 C14 C16 -50.7(7) . . . . ? C8 C13 C17 C18 -97.7(6) . . . . ? C12 C13 C17 C18 79.6(6) . . . . ? C8 C13 C17 C19 136.4(5) . . . . ? C12 C13 C17 C19 -46.2(7) . . . . ? C25 C20 C21 C22 -0.9(6) . . . . ? N2 C20 C21 C22 178.9(4) . . . . ? C25 C20 C21 C26 -179.4(4) . . . . ? N2 C20 C21 C26 0.5(6) . . . . ? C20 C21 C22 C23 0.1(7) . . . . ? C26 C21 C22 C23 178.5(5) . . . . ? C21 C22 C23 C24 1.0(8) . . . . ? C22 C23 C24 C25 -1.2(8) . . . . ? C23 C24 C25 C20 0.3(7) . . . . ? C23 C24 C25 C29 176.1(5) . . . . ? C21 C20 C25 C24 0.8(7) . . . . ? N2 C20 C25 C24 -179.1(4) . . . . ? C21 C20 C25 C29 -174.9(4) . . . . ? N2 C20 C25 C29 5.2(6) . . . . ? C22 C21 C26 C28 42.2(6) . . . . ? C20 C21 C26 C28 -139.4(5) . . . . ? C22 C21 C26 C27 -84.0(6) . . . . ? C20 C21 C26 C27 94.4(5) . . . . ? C24 C25 C29 C30 -85.6(6) . . . . ? C20 C25 C29 C30 89.9(6) . . . . ? C24 C25 C29 C31 38.3(7) . . . . ? C20 C25 C29 C31 -146.3(5) . . . . ? C2 C1 N1 C8 -3.3(7) . . . . ? C5 C1 N1 C8 175.3(3) . . . . ? C2 C1 N1 Pd1 177.4(4) . . . . ? C5 C1 N1 Pd1 -3.9(4) . . . . ? C13 C8 N1 C1 -86.1(5) . . . . ? C9 C8 N1 C1 94.8(5) . . . . ? C13 C8 N1 Pd1 93.1(4) . . . . ? C9 C8 N1 Pd1 -86.1(4) . . . . ? C4 C5 N2 C20 6.4(7) . . . . ? C1 C5 N2 C20 -172.6(3) . . . . ? C4 C5 N2 Pd1 -178.1(4) . . . . ? C1 C5 N2 Pd1 2.9(4) . . . . ? C21 C20 N2 C5 -103.2(5) . . . . ? C25 C20 N2 C5 76.7(5) . . . . ? C21 C20 N2 Pd1 82.0(4) . . . . ? C25 C20 N2 Pd1 -98.1(4) . . . . ? C1 N1 Pd1 N2 4.2(3) . . . . ? C8 N1 Pd1 N2 -175.0(3) . . . . ? C1 N1 Pd1 Cl1 -177.1(3) . . . . ? C8 N1 Pd1 Cl1 3.7(3) . . . . ? C1 N1 Pd1 Cl2 -29.7(10) . . . . ? C8 N1 Pd1 Cl2 151.1(7) . . . . ? C5 N2 Pd1 N1 -3.8(3) . . . . ? C20 N2 Pd1 N1 171.2(3) . . . . ? C5 N2 Pd1 Cl1 -17.8(12) . . . . ? C20 N2 Pd1 Cl1 157.2(8) . . . . ? C5 N2 Pd1 Cl2 172.7(3) . . . . ? C20 N2 Pd1 Cl2 -12.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.697 _refine_diff_density_min -1.849 _refine_diff_density_rms 0.114 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.113 0.210 0.413 213.5 112.8 2 0.613 0.209 0.087 213.5 114.8 3 0.113 0.290 0.913 213.6 113.1 4 0.613 0.290 0.587 213.7 113.9 5 0.387 0.710 0.413 213.7 113.8 6 0.887 0.710 0.087 213.7 114.8 7 0.387 0.790 0.913 213.6 113.2 8 0.887 0.790 0.587 213.6 113.8 _platon_squeeze_details ; ; # Attachment 'kvkv129asq.cif' data_kvkv129asq _database_code_depnum_ccdc_archive 'CCDC 812613' #TrackingRef 'kvkv129asq.cif' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H72 I6 In2 N4, C H2 Cl2' _chemical_formula_sum 'C63 H74 Cl2 I6 In2 N4' _chemical_formula_weight 1949.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n _symmetry_space_group_name_Hall -p2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.370(5) _cell_length_b 22.405(5) _cell_length_c 15.448(5) _cell_angle_alpha 90.000 _cell_angle_beta 95.681(5) _cell_angle_gamma 90.000 _cell_volume 3572(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13664 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.1280 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8143 _reflns_number_gt 4614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The SQUEEZE program was used to remove one disordered dichloromethane molecule. The A alerts pertain to this absence. ; _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^)+(0.0684P)^2^+0.0000P] 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_extinction_coef ? _refine_ls_number_reflns 8143 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3764(7) -0.0954(3) 0.3905(5) 0.0204(16) Uani 1 1 d . . . C2 C 0.4467(6) -0.0776(3) 0.4780(4) 0.0143(15) Uani 1 1 d . . . C3 C 0.4687(7) -0.0159(3) 0.4679(4) 0.0180(16) Uani 1 1 d . . . C4 C 0.4244(6) 0.0109(3) 0.3871(4) 0.0161(15) Uani 1 1 d . . . C5 C 0.3666(6) -0.0399(3) 0.3338(4) 0.0151(15) Uani 1 1 d . . . C6 C 0.4941(7) -0.1049(3) 0.5543(4) 0.0207(16) Uani 1 1 d . . . H6 H 0.4844 -0.1459 0.5606 0.025 Uiso 1 1 calc R . . C7 C 0.5565(6) -0.0717(3) 0.6226(4) 0.0149(15) Uani 1 1 d . . . H7 H 0.5853 -0.0905 0.6747 0.018 Uiso 1 1 calc R . . C8 C 0.3673(6) -0.1990(3) 0.4107(4) 0.0168(16) Uani 1 1 d . . . C9 C 0.4845(7) -0.2292(3) 0.3989(5) 0.0247(18) Uani 1 1 d . . . C10 C 0.5110(8) -0.2790(3) 0.4539(5) 0.034(2) Uani 1 1 d . . . H10 H 0.5873 -0.3001 0.4498 0.041 Uiso 1 1 calc R . . C11 C 0.4304(8) -0.2975(3) 0.5125(5) 0.035(2) Uani 1 1 d . . . H11 H 0.4517 -0.3307 0.5472 0.042 Uiso 1 1 calc R . . C12 C 0.3145(8) -0.2664(3) 0.5206(5) 0.0316(19) Uani 1 1 d . . . H12 H 0.2599 -0.2791 0.5611 0.038 Uiso 1 1 calc R . . C13 C 0.2793(7) -0.2159(3) 0.4680(4) 0.0184(16) Uani 1 1 d . . . C14 C 0.5796(7) -0.2082(3) 0.3374(5) 0.0313(19) Uani 1 1 d . . . H14 H 0.5298 -0.1855 0.2912 0.038 Uiso 1 1 calc R . . C15 C 0.6787(7) -0.1664(4) 0.3809(7) 0.055(3) Uani 1 1 d . . . H15A H 0.6365 -0.1311 0.3992 0.083 Uiso 1 1 calc R . . H15B H 0.7398 -0.1557 0.3407 0.083 Uiso 1 1 calc R . . H15C H 0.7234 -0.1857 0.4307 0.083 Uiso 1 1 calc R . . C16 C 0.6470(9) -0.2580(4) 0.2936(7) 0.055(3) Uani 1 1 d . . . H16A H 0.7036 -0.2413 0.2544 0.082 Uiso 1 1 calc R . . H16B H 0.5834 -0.2828 0.2617 0.082 Uiso 1 1 calc R . . H16C H 0.6966 -0.2815 0.3369 0.082 Uiso 1 1 calc R . . C17 C 0.1557(7) -0.1829(3) 0.4795(5) 0.0301(19) Uani 1 1 d . . . H17 H 0.1476 -0.1502 0.4371 0.036 Uiso 1 1 calc R . . C18 C 0.0410(8) -0.2233(4) 0.4607(6) 0.050(2) Uani 1 1 d . . . H18A H 0.0357 -0.2360 0.4011 0.075 Uiso 1 1 calc R . . H18B H -0.0366 -0.2022 0.4708 0.075 Uiso 1 1 calc R . . H18C H 0.0506 -0.2575 0.4981 0.075 Uiso 1 1 calc R . . C19 C 0.1525(10) -0.1564(4) 0.5684(6) 0.061(3) Uani 1 1 d . . . H19A H 0.1522 -0.1879 0.6106 0.091 Uiso 1 1 calc R . . H19B H 0.0757 -0.1327 0.5698 0.091 Uiso 1 1 calc R . . H19C H 0.2276 -0.1318 0.5818 0.091 Uiso 1 1 calc R . . C20 C 0.3479(7) 0.0075(3) 0.1992(4) 0.0178(16) Uani 1 1 d . . . C21 C 0.2463(7) 0.0464(3) 0.1751(4) 0.0231(17) Uani 1 1 d . . . C22 C 0.2773(8) 0.0966(3) 0.1291(5) 0.0299(19) Uani 1 1 d . . . H22 H 0.2117 0.1235 0.1114 0.036 Uiso 1 1 calc R . . C23 C 0.3987(8) 0.1084(3) 0.1088(5) 0.037(2) Uani 1 1 d . . . H23 H 0.4155 0.1433 0.0794 0.045 Uiso 1 1 calc R . . C24 C 0.4977(8) 0.0685(3) 0.1319(5) 0.034(2) Uani 1 1 d . . . H24 H 0.5807 0.0767 0.1173 0.041 Uiso 1 1 calc R . . C25 C 0.4753(7) 0.0161(3) 0.1765(5) 0.0262(18) Uani 1 1 d . . . C26 C 0.1102(7) 0.0347(3) 0.1977(5) 0.0284(18) Uani 1 1 d . . . H26 H 0.1108 -0.0034 0.2288 0.034 Uiso 1 1 calc R . . C27 C 0.0158(9) 0.0294(5) 0.1185(6) 0.068(3) Uani 1 1 d . . . H27A H 0.0060 0.0675 0.0902 0.102 Uiso 1 1 calc R . . H27B H -0.0665 0.0164 0.1350 0.102 Uiso 1 1 calc R . . H27C H 0.0474 0.0009 0.0793 0.102 Uiso 1 1 calc R . . C28 C 0.0613(9) 0.0818(4) 0.2561(7) 0.064(3) Uani 1 1 d . . . H28A H 0.1189 0.0846 0.3086 0.095 Uiso 1 1 calc R . . H28B H -0.0238 0.0712 0.2702 0.095 Uiso 1 1 calc R . . H28C H 0.0578 0.1196 0.2267 0.095 Uiso 1 1 calc R . . C29 C 0.5876(7) -0.0279(3) 0.1986(5) 0.0282(18) Uani 1 1 d . . . H29 H 0.5534 -0.0632 0.2261 0.034 Uiso 1 1 calc R . . C30 C 0.6935(8) -0.0002(4) 0.2625(6) 0.051(3) Uani 1 1 d . . . H30A H 0.7242 0.0360 0.2382 0.076 Uiso 1 1 calc R . . H30B H 0.7641 -0.0278 0.2730 0.076 Uiso 1 1 calc R . . H30C H 0.6585 0.0086 0.3163 0.076 Uiso 1 1 calc R . . C31 C 0.6450(8) -0.0481(4) 0.1147(6) 0.043(2) Uani 1 1 d . . . H31A H 0.5801 -0.0690 0.0778 0.064 Uiso 1 1 calc R . . H31B H 0.7175 -0.0740 0.1296 0.064 Uiso 1 1 calc R . . H31C H 0.6733 -0.0137 0.0845 0.064 Uiso 1 1 calc R . . N1 N 0.3420(5) -0.1456(2) 0.3574(4) 0.0162(13) Uani 1 1 d . . . N2 N 0.3277(5) -0.0448(2) 0.2538(3) 0.0154(12) Uani 1 1 d . . . In1 In 0.23802(5) -0.14496(2) 0.21395(3) 0.01921(15) Uani 1 1 d . . . I1 I -0.00709(5) -0.12286(2) 0.25104(4) 0.03327(16) Uani 1 1 d . . . I2 I 0.25048(7) -0.26641(2) 0.20312(4) 0.0563(2) Uani 1 1 d . . . I3 I 0.29112(6) -0.11590(3) 0.05080(4) 0.0512(2) Uani 1 1 d . . . 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 C1 0.025(4) 0.016(4) 0.020(4) -0.002(3) 0.003(3) 0.004(3) C2 0.025(4) 0.011(3) 0.006(3) -0.005(3) 0.000(3) -0.003(3) C3 0.027(4) 0.014(4) 0.012(4) 0.002(3) -0.003(3) -0.001(3) C4 0.018(4) 0.013(3) 0.017(4) -0.006(3) 0.001(3) -0.003(3) C5 0.025(4) 0.011(3) 0.011(4) 0.001(3) 0.007(3) 0.002(3) C6 0.031(4) 0.016(3) 0.015(4) 0.000(3) 0.003(3) -0.004(3) C7 0.022(4) 0.012(3) 0.009(3) 0.000(3) -0.006(3) 0.000(3) C8 0.022(4) 0.017(3) 0.009(4) -0.002(3) -0.011(3) -0.001(3) C9 0.023(4) 0.020(4) 0.029(5) -0.011(3) -0.009(3) -0.003(3) C10 0.035(5) 0.021(4) 0.042(5) -0.006(4) -0.023(4) 0.003(3) C11 0.049(6) 0.024(4) 0.029(5) 0.013(4) -0.013(4) 0.008(4) C12 0.045(5) 0.031(4) 0.020(4) 0.004(4) 0.005(4) -0.005(4) C13 0.030(4) 0.014(3) 0.011(4) -0.002(3) -0.001(3) -0.006(3) C14 0.024(4) 0.036(4) 0.033(5) 0.004(4) 0.004(4) -0.001(4) C15 0.023(5) 0.057(6) 0.089(8) -0.007(6) 0.022(5) -0.010(4) C16 0.054(6) 0.048(5) 0.064(7) -0.020(5) 0.022(5) 0.005(5) C17 0.033(5) 0.028(4) 0.031(5) 0.003(4) 0.009(4) 0.001(4) C18 0.044(6) 0.046(5) 0.062(7) 0.010(5) 0.012(5) -0.002(4) C19 0.072(7) 0.062(6) 0.054(7) -0.016(5) 0.030(6) -0.002(5) C20 0.029(4) 0.012(3) 0.012(4) -0.003(3) -0.002(3) -0.004(3) C21 0.034(5) 0.020(4) 0.014(4) -0.007(3) -0.009(3) 0.003(3) C22 0.048(5) 0.020(4) 0.021(4) 0.013(3) -0.001(4) 0.008(4) C23 0.049(6) 0.028(4) 0.037(5) 0.009(4) 0.015(4) -0.005(4) C24 0.037(5) 0.039(5) 0.030(5) 0.005(4) 0.014(4) -0.006(4) C25 0.026(4) 0.033(4) 0.020(4) 0.000(4) 0.002(3) -0.004(3) C26 0.022(4) 0.026(4) 0.035(5) 0.004(4) -0.010(4) 0.003(3) C27 0.040(6) 0.106(9) 0.054(7) 0.000(6) -0.012(5) -0.003(6) C28 0.057(7) 0.057(6) 0.082(8) -0.030(6) 0.033(6) -0.009(5) C29 0.021(4) 0.036(4) 0.029(5) 0.005(4) 0.009(3) 0.004(3) C30 0.031(5) 0.082(7) 0.038(6) -0.021(5) -0.004(4) 0.010(5) C31 0.034(5) 0.050(5) 0.045(6) -0.016(5) 0.005(4) 0.001(4) N1 0.018(3) 0.015(3) 0.016(3) -0.002(3) 0.000(3) 0.001(2) N2 0.016(3) 0.016(3) 0.014(3) -0.002(3) -0.002(3) 0.000(2) In1 0.0214(3) 0.0198(3) 0.0155(3) -0.0024(2) -0.0028(2) -0.0013(2) I1 0.0233(3) 0.0394(3) 0.0376(3) 0.0016(3) 0.0057(2) -0.0007(2) I2 0.0907(5) 0.0231(3) 0.0478(4) -0.0127(3) -0.0305(4) 0.0120(3) I3 0.0732(5) 0.0609(4) 0.0218(3) -0.0154(3) 0.0166(3) -0.0438(3) _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 C1 N1 1.273(8) . ? C1 C5 1.519(9) . ? C1 C2 1.524(9) . ? C2 C6 1.375(9) . ? C2 C3 1.414(8) . ? C3 C3 1.335(12) 3_656 ? C3 C4 1.420(9) . ? C4 C7 1.387(9) 3_656 ? C4 C5 1.495(9) . ? C5 N2 1.267(8) . ? C6 C7 1.396(9) . ? C6 H6 0.9300 . ? C7 C4 1.387(9) 3_656 ? C7 H7 0.9300 . ? C8 C13 1.386(9) . ? C8 C9 1.418(9) . ? C8 N1 1.462(8) . ? C9 C10 1.412(10) . ? C9 C14 1.512(10) . ? C10 C11 1.356(11) . ? C10 H10 0.9300 . ? C11 C12 1.405(11) . ? C11 H11 0.9300 . ? C12 C13 1.418(10) . ? C12 H12 0.9300 . ? C13 C17 1.505(10) . ? C14 C15 1.499(10) . ? C14 C16 1.512(10) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.501(11) . ? C17 C18 1.500(11) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.391(9) . ? C20 C25 1.413(10) . ? C20 N2 1.470(8) . ? C21 C22 1.385(10) . ? C21 C26 1.510(10) . ? C22 C23 1.353(11) . ? C22 H22 0.9300 . ? C23 C24 1.382(11) . ? C23 H23 0.9300 . ? C24 C25 1.391(10) . ? C24 H24 0.9300 . ? C25 C29 1.539(10) . ? C26 C27 1.494(10) . ? C26 C28 1.507(11) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.534(10) . ? C29 C31 1.546(11) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 In1 2.366(5) . ? N2 In1 2.483(5) . ? In1 I1 2.7060(14) . ? In1 I3 2.7118(11) . ? In1 I2 2.7301(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C5 119.5(6) . . ? N1 C1 C2 132.7(6) . . ? C5 C1 C2 107.3(5) . . ? C6 C2 C3 118.8(6) . . ? C6 C2 C1 138.1(6) . . ? C3 C2 C1 103.0(5) . . ? C3 C3 C2 120.8(8) 3_656 . ? C3 C3 C4 121.2(7) 3_656 . ? C2 C3 C4 118.0(6) . . ? C7 C4 C3 118.2(6) 3_656 . ? C7 C4 C5 137.9(6) 3_656 . ? C3 C4 C5 103.8(5) . . ? N2 C5 C4 132.5(6) . . ? N2 C5 C1 119.2(6) . . ? C4 C5 C1 107.8(6) . . ? C2 C6 C7 120.7(6) . . ? C2 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C4 C7 C6 120.1(6) 3_656 . ? C4 C7 H7 119.9 3_656 . ? C6 C7 H7 119.9 . . ? C13 C8 C9 125.3(6) . . ? C13 C8 N1 119.4(6) . . ? C9 C8 N1 115.2(6) . . ? C8 C9 C10 114.7(7) . . ? C8 C9 C14 123.5(6) . . ? C10 C9 C14 121.7(7) . . ? C11 C10 C9 123.2(8) . . ? C11 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? C10 C11 C12 119.8(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 121.2(7) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C8 C13 C12 115.8(7) . . ? C8 C13 C17 124.3(6) . . ? C12 C13 C17 119.9(6) . . ? C15 C14 C16 109.6(7) . . ? C15 C14 C9 112.0(7) . . ? C16 C14 C9 114.2(6) . . ? C15 C14 H14 106.9 . . ? C16 C14 H14 106.9 . . ? C9 C14 H14 106.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 109.1(7) . . ? C19 C17 C13 113.5(7) . . ? C18 C17 C13 110.4(6) . . ? C19 C17 H17 107.9 . . ? C18 C17 H17 107.9 . . ? C13 C17 H17 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 123.3(6) . . ? C21 C20 N2 120.4(6) . . ? C25 C20 N2 116.2(6) . . ? C22 C21 C20 116.0(7) . . ? C22 C21 C26 122.0(6) . . ? C20 C21 C26 122.0(6) . . ? C23 C22 C21 123.1(7) . . ? C23 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 121.2(7) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C20 116.4(7) . . ? C24 C25 C29 119.3(7) . . ? C20 C25 C29 124.3(6) . . ? C27 C26 C28 108.3(7) . . ? C27 C26 C21 112.0(7) . . ? C28 C26 C21 113.2(6) . . ? C27 C26 H26 107.7 . . ? C28 C26 H26 107.7 . . ? C21 C26 H26 107.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C25 111.1(6) . . ? C30 C29 C31 110.4(6) . . ? C25 C29 C31 110.4(6) . . ? C30 C29 H29 108.3 . . ? C25 C29 H29 108.3 . . ? C31 C29 H29 108.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 N1 C8 118.0(6) . . ? C1 N1 In1 117.0(4) . . ? C8 N1 In1 124.9(4) . . ? C5 N2 C20 116.1(5) . . ? C5 N2 In1 113.4(4) . . ? C20 N2 In1 130.5(4) . . ? N1 In1 N2 69.44(17) . . ? N1 In1 I1 98.84(13) . . ? N2 In1 I1 96.81(12) . . ? N1 In1 I3 139.11(13) . . ? N2 In1 I3 84.72(13) . . ? I1 In1 I3 115.74(3) . . ? N1 In1 I2 91.79(12) . . ? N2 In1 I2 153.79(12) . . ? I1 In1 I2 104.27(3) . . ? I3 In1 I2 99.62(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C6 -3.9(14) . . . . ? C5 C1 C2 C6 -174.8(8) . . . . ? N1 C1 C2 C3 172.5(7) . . . . ? C5 C1 C2 C3 1.6(7) . . . . ? C6 C2 C3 C3 -1.7(12) . . . 3_656 ? C1 C2 C3 C3 -179.0(9) . . . 3_656 ? C6 C2 C3 C4 177.1(6) . . . . ? C1 C2 C3 C4 -0.2(8) . . . . ? C3 C3 C4 C7 -2.4(12) 3_656 . . 3_656 ? C2 C3 C4 C7 178.8(6) . . . 3_656 ? C3 C3 C4 C5 177.5(9) 3_656 . . . ? C2 C3 C4 C5 -1.4(8) . . . . ? C7 C4 C5 N2 10.5(14) 3_656 . . . ? C3 C4 C5 N2 -169.3(7) . . . . ? C7 C4 C5 C1 -177.9(8) 3_656 . . . ? C3 C4 C5 C1 2.3(7) . . . . ? N1 C1 C5 N2 -1.8(10) . . . . ? C2 C1 C5 N2 170.5(6) . . . . ? N1 C1 C5 C4 -174.8(6) . . . . ? C2 C1 C5 C4 -2.5(7) . . . . ? C3 C2 C6 C7 3.5(10) . . . . ? C1 C2 C6 C7 179.5(7) . . . . ? C2 C6 C7 C4 -2.3(10) . . . 3_656 ? C13 C8 C9 C10 -2.3(10) . . . . ? N1 C8 C9 C10 176.9(6) . . . . ? C13 C8 C9 C14 -178.2(6) . . . . ? N1 C8 C9 C14 1.1(9) . . . . ? C8 C9 C10 C11 1.1(10) . . . . ? C14 C9 C10 C11 177.1(7) . . . . ? C9 C10 C11 C12 -0.3(12) . . . . ? C10 C11 C12 C13 0.4(11) . . . . ? C9 C8 C13 C12 2.4(10) . . . . ? N1 C8 C13 C12 -176.7(6) . . . . ? C9 C8 C13 C17 179.8(6) . . . . ? N1 C8 C13 C17 0.6(10) . . . . ? C11 C12 C13 C8 -1.4(10) . . . . ? C11 C12 C13 C17 -178.9(7) . . . . ? C8 C9 C14 C15 89.8(9) . . . . ? C10 C9 C14 C15 -85.9(8) . . . . ? C8 C9 C14 C16 -145.0(7) . . . . ? C10 C9 C14 C16 39.4(10) . . . . ? C8 C13 C17 C19 -115.7(8) . . . . ? C12 C13 C17 C19 61.5(9) . . . . ? C8 C13 C17 C18 121.5(7) . . . . ? C12 C13 C17 C18 -61.3(9) . . . . ? C25 C20 C21 C22 -2.3(10) . . . . ? N2 C20 C21 C22 175.4(6) . . . . ? C25 C20 C21 C26 177.8(6) . . . . ? N2 C20 C21 C26 -4.5(10) . . . . ? C20 C21 C22 C23 -0.6(11) . . . . ? C26 C21 C22 C23 179.3(7) . . . . ? C21 C22 C23 C24 2.0(13) . . . . ? C22 C23 C24 C25 -0.5(13) . . . . ? C23 C24 C25 C20 -2.1(11) . . . . ? C23 C24 C25 C29 178.3(7) . . . . ? C21 C20 C25 C24 3.6(11) . . . . ? N2 C20 C25 C24 -174.2(6) . . . . ? C21 C20 C25 C29 -176.8(6) . . . . ? N2 C20 C25 C29 5.4(10) . . . . ? C22 C21 C26 C27 60.5(9) . . . . ? C20 C21 C26 C27 -119.6(8) . . . . ? C22 C21 C26 C28 -62.4(10) . . . . ? C20 C21 C26 C28 117.5(8) . . . . ? C24 C25 C29 C30 65.1(9) . . . . ? C20 C25 C29 C30 -114.5(8) . . . . ? C24 C25 C29 C31 -57.7(9) . . . . ? C20 C25 C29 C31 122.7(8) . . . . ? C5 C1 N1 C8 172.7(6) . . . . ? C2 C1 N1 C8 2.7(11) . . . . ? C5 C1 N1 In1 -8.4(8) . . . . ? C2 C1 N1 In1 -178.4(6) . . . . ? C13 C8 N1 C1 84.7(8) . . . . ? C9 C8 N1 C1 -94.6(7) . . . . ? C13 C8 N1 In1 -94.1(6) . . . . ? C9 C8 N1 In1 86.6(6) . . . . ? C4 C5 N2 C20 4.0(10) . . . . ? C1 C5 N2 C20 -166.8(6) . . . . ? C4 C5 N2 In1 -178.9(6) . . . . ? C1 C5 N2 In1 10.3(7) . . . . ? C21 C20 N2 C5 -100.7(7) . . . . ? C25 C20 N2 C5 77.1(8) . . . . ? C21 C20 N2 In1 82.7(7) . . . . ? C25 C20 N2 In1 -99.4(6) . . . . ? C1 N1 In1 N2 9.6(5) . . . . ? C8 N1 In1 N2 -171.6(5) . . . . ? C1 N1 In1 I1 -84.4(5) . . . . ? C8 N1 In1 I1 94.4(5) . . . . ? C1 N1 In1 I3 63.9(5) . . . . ? C8 N1 In1 I3 -117.3(5) . . . . ? C1 N1 In1 I2 170.9(5) . . . . ? C8 N1 In1 I2 -10.3(5) . . . . ? C5 N2 In1 N1 -10.3(4) . . . . ? C20 N2 In1 N1 166.3(6) . . . . ? C5 N2 In1 I1 86.6(4) . . . . ? C20 N2 In1 I1 -96.8(5) . . . . ? C5 N2 In1 I3 -158.0(5) . . . . ? C20 N2 In1 I3 18.6(5) . . . . ? C5 N2 In1 I2 -57.0(6) . . . . ? C20 N2 In1 I2 119.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.267 _refine_diff_density_min -1.084 _refine_diff_density_rms 0.256 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 127.8 74.4 2 0.100 0.686 0.266 37.6 7.3 3 0.069 0.317 0.136 10.1 2.0 4 0.187 0.111 0.347 7.0 1.2 5 0.500 0.500 0.500 127.8 75.0 6 0.401 0.186 0.233 37.6 6.1 7 0.315 0.610 0.151 6.9 1.4 8 0.431 0.817 0.364 10.1 2.0 9 0.600 0.814 0.766 37.6 7.1 10 0.569 0.183 0.636 10.1 2.1 11 0.687 0.389 0.847 7.1 1.2 12 0.901 0.314 0.733 37.5 6.0 13 0.815 0.889 0.651 7.0 1.1 14 0.931 0.683 0.864 10.1 2.0 _platon_squeeze_details ; ; # Attachment 'kvkv130sq.cif' data_kvkv130sq _database_code_depnum_ccdc_archive 'CCDC 812614' #TrackingRef 'kvkv130sq.cif' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H72 Cl6 In2 N4, 2 (C H2 Cl2)' _chemical_formula_sum 'C64 H76 Cl10 In2 N4' _chemical_formula_weight 1485.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n _symmetry_space_group_name_Hall -p2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.676(5) _cell_length_b 17.250(5) _cell_length_c 18.117(5) _cell_angle_alpha 90.000 _cell_angle_beta 91.994(5) _cell_angle_gamma 90.000 _cell_volume 3647(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14713 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8317 _reflns_number_gt 5519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 2 molecules of disordered dichloromethane were removed using SQUEEZE, resulting in several related A alerts. ; _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^)+(0.0765P)^2^+0.0000P] 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_extinction_coef ? _refine_ls_number_reflns 8317 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6394(3) 0.1043(2) 0.41346(17) 0.0189(7) Uani 1 1 d . . . C2 C 0.6332(3) 0.0528(2) 0.47729(18) 0.0229(8) Uani 1 1 d . . . C3 C 0.5186(3) 0.0258(2) 0.47461(18) 0.0250(8) Uani 1 1 d . . . C4 C 0.4470(3) 0.0519(2) 0.41497(19) 0.0256(8) Uani 1 1 d . . . C5 C 0.5207(3) 0.1054(2) 0.37341(18) 0.0215(8) Uani 1 1 d . . . C6 C 0.3354(3) 0.0252(2) 0.41141(19) 0.0262(8) Uani 1 1 d . . . H6 H 0.2860 0.0417 0.3732 0.031 Uiso 1 1 calc R . . C7 C 0.2948(3) -0.0270(2) 0.46520(18) 0.0253(8) Uani 1 1 d . . . H7 H 0.2193 -0.0441 0.4619 0.030 Uiso 1 1 calc R . . C8 C 0.8375(3) 0.1281(2) 0.41236(17) 0.0199(8) Uani 1 1 d . . . C9 C 0.8825(3) 0.1771(2) 0.46692(18) 0.0263(8) Uani 1 1 d . . . C10 C 0.9938(3) 0.1624(3) 0.4932(2) 0.0390(10) Uani 1 1 d . . . H10 H 1.0258 0.1929 0.5310 0.047 Uiso 1 1 calc R . . C11 C 1.0565(4) 0.1039(3) 0.4644(2) 0.0484(12) Uani 1 1 d . . . H11 H 1.1313 0.0956 0.4821 0.058 Uiso 1 1 calc R . . C12 C 1.0106(3) 0.0564(3) 0.4093(2) 0.0417(11) Uani 1 1 d . . . H12 H 1.0548 0.0165 0.3908 0.050 Uiso 1 1 calc R . . C13 C 0.8988(3) 0.0676(2) 0.3811(2) 0.0304(9) Uani 1 1 d . . . C14 C 0.8163(4) 0.2465(3) 0.4975(2) 0.0383(10) Uani 1 1 d . . . H14 H 0.7406 0.2486 0.4724 0.046 Uiso 1 1 calc R . . C15 C 0.7998(5) 0.2357(3) 0.5811(3) 0.0607(15) Uani 1 1 d . . . H15A H 0.8727 0.2393 0.6070 0.091 Uiso 1 1 calc R . . H15B H 0.7666 0.1858 0.5898 0.091 Uiso 1 1 calc R . . H15C H 0.7498 0.2754 0.5985 0.091 Uiso 1 1 calc R . . C16 C 0.8784(5) 0.3217(3) 0.4831(3) 0.0561(13) Uani 1 1 d . . . H16A H 0.9502 0.3222 0.5106 0.084 Uiso 1 1 calc R . . H16B H 0.8323 0.3645 0.4983 0.084 Uiso 1 1 calc R . . H16C H 0.8921 0.3261 0.4314 0.084 Uiso 1 1 calc R . . C17 C 0.8505(4) 0.0170(3) 0.3196(2) 0.0457(12) Uani 1 1 d . . . H17 H 0.7697 0.0321 0.3137 0.055 Uiso 1 1 calc R . . C18 C 0.8968(12) 0.0289(6) 0.2499(3) 0.237(8) Uani 1 1 d . . . H18A H 0.9746 0.0110 0.2506 0.356 Uiso 1 1 calc R . . H18B H 0.8948 0.0832 0.2382 0.356 Uiso 1 1 calc R . . H18C H 0.8525 0.0008 0.2132 0.356 Uiso 1 1 calc R . . C19 C 0.8487(14) -0.0626(5) 0.3353(4) 0.263(9) Uani 1 1 d . . . H19A H 0.7820 -0.0856 0.3119 0.394 Uiso 1 1 calc R . . H19B H 0.8465 -0.0700 0.3878 0.394 Uiso 1 1 calc R . . H19C H 0.9163 -0.0865 0.3171 0.394 Uiso 1 1 calc R . . C20 C 0.4006(3) 0.1322(2) 0.2722(2) 0.0301(9) Uani 1 1 d . . . C21 C 0.3091(4) 0.1816(3) 0.2839(2) 0.0387(11) Uani 1 1 d . . . C22 C 0.2041(4) 0.1614(4) 0.2454(3) 0.0573(15) Uani 1 1 d . . . H22 H 0.1396 0.1918 0.2522 0.069 Uiso 1 1 calc R . . C23 C 0.1953(5) 0.0994(4) 0.1994(3) 0.0663(17) Uani 1 1 d . . . H23 H 0.1253 0.0869 0.1763 0.080 Uiso 1 1 calc R . . C24 C 0.2887(5) 0.0561(3) 0.1877(3) 0.0650(17) Uani 1 1 d . . . H24 H 0.2821 0.0147 0.1549 0.078 Uiso 1 1 calc R . . C25 C 0.3959(4) 0.0707(3) 0.2226(2) 0.0433(11) Uani 1 1 d . . . C26 C 0.3188(4) 0.2537(3) 0.3314(3) 0.0477(12) Uani 1 1 d . . . H26 H 0.3925 0.2510 0.3589 0.057 Uiso 1 1 calc R . . C27 C 0.2248(5) 0.2602(4) 0.3883(3) 0.085(2) Uani 1 1 d . . . H27A H 0.1517 0.2662 0.3630 0.127 Uiso 1 1 calc R . . H27B H 0.2397 0.3044 0.4194 0.127 Uiso 1 1 calc R . . H27C H 0.2244 0.2141 0.4179 0.127 Uiso 1 1 calc R . . C28 C 0.3232(5) 0.3259(3) 0.2800(3) 0.0644(15) Uani 1 1 d . . . H28A H 0.3909 0.3236 0.2515 0.097 Uiso 1 1 calc R . . H28B H 0.3248 0.3722 0.3094 0.097 Uiso 1 1 calc R . . H28C H 0.2566 0.3265 0.2473 0.097 Uiso 1 1 calc R . . C29 C 0.4974(5) 0.0198(3) 0.2068(3) 0.0525(13) Uani 1 1 d . . . H29 H 0.5658 0.0475 0.2255 0.063 Uiso 1 1 calc R . . C30 C 0.4943(5) -0.0574(3) 0.2482(3) 0.0780(18) Uani 1 1 d . . . H30A H 0.4943 -0.0478 0.3004 0.117 Uiso 1 1 calc R . . H30B H 0.5605 -0.0876 0.2368 0.117 Uiso 1 1 calc R . . H30C H 0.4262 -0.0853 0.2333 0.117 Uiso 1 1 calc R . . C31 C 0.5127(7) 0.0070(4) 0.1234(3) 0.091(2) Uani 1 1 d . . . H31A H 0.4480 -0.0211 0.1030 0.136 Uiso 1 1 calc R . . H31B H 0.5814 -0.0222 0.1162 0.136 Uiso 1 1 calc R . . H31C H 0.5181 0.0563 0.0991 0.136 Uiso 1 1 calc R . . N1 N 0.7219(2) 0.13939(17) 0.38318(14) 0.0192(6) Uani 1 1 d . . . N2 N 0.5073(2) 0.14327(18) 0.31424(15) 0.0235(7) Uani 1 1 d . . . Cl1 Cl 0.61066(11) 0.33003(7) 0.35341(6) 0.0520(3) Uani 1 1 d . . . Cl2 Cl 0.87322(10) 0.24455(9) 0.27179(6) 0.0562(4) Uani 1 1 d . . . Cl3 Cl 0.61239(10) 0.21240(7) 0.16192(5) 0.0449(3) Uani 1 1 d . . . In1 In 0.67369(2) 0.222285(16) 0.286950(13) 0.02576(11) Uani 1 1 d . . . 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 C1 0.0180(18) 0.0157(19) 0.0231(17) 0.0031(15) 0.0042(13) 0.0009(15) C2 0.0185(19) 0.022(2) 0.0278(18) 0.0081(16) 0.0021(14) -0.0004(16) C3 0.0199(19) 0.028(2) 0.0270(18) 0.0098(16) -0.0010(14) -0.0013(17) C4 0.023(2) 0.025(2) 0.0286(19) 0.0132(16) -0.0004(15) 0.0001(17) C5 0.0194(19) 0.022(2) 0.0235(18) 0.0059(15) 0.0038(14) 0.0014(16) C6 0.0190(19) 0.029(2) 0.0306(19) 0.0144(17) -0.0064(15) 0.0011(17) C7 0.0127(18) 0.031(2) 0.0319(19) 0.0131(17) -0.0002(14) -0.0019(16) C8 0.0151(18) 0.023(2) 0.0221(17) 0.0053(15) 0.0013(13) -0.0025(15) C9 0.027(2) 0.027(2) 0.0247(18) 0.0000(16) 0.0027(15) -0.0013(18) C10 0.027(2) 0.047(3) 0.042(2) -0.011(2) -0.0068(17) -0.002(2) C11 0.019(2) 0.058(3) 0.067(3) -0.010(3) -0.007(2) 0.004(2) C12 0.028(2) 0.045(3) 0.053(3) -0.011(2) 0.0052(19) 0.014(2) C13 0.021(2) 0.031(2) 0.040(2) -0.0041(18) 0.0043(16) -0.0020(18) C14 0.036(3) 0.044(3) 0.034(2) -0.015(2) -0.0053(18) 0.007(2) C15 0.065(4) 0.067(4) 0.050(3) -0.026(3) 0.008(3) 0.003(3) C16 0.079(4) 0.033(3) 0.056(3) -0.009(2) -0.009(3) 0.001(3) C17 0.034(2) 0.043(3) 0.060(3) -0.028(2) -0.002(2) 0.010(2) C18 0.52(2) 0.149(9) 0.040(4) -0.024(5) 0.020(7) -0.206(12) C19 0.65(3) 0.058(5) 0.074(5) -0.003(4) -0.086(10) -0.114(10) C20 0.025(2) 0.033(2) 0.032(2) 0.0184(18) -0.0032(16) -0.0049(19) C21 0.032(2) 0.042(3) 0.042(2) 0.025(2) 0.0006(18) 0.004(2) C22 0.029(3) 0.075(4) 0.068(3) 0.045(3) -0.011(2) 0.004(3) C23 0.045(3) 0.070(4) 0.082(4) 0.033(3) -0.033(3) -0.023(3) C24 0.060(4) 0.051(4) 0.080(4) 0.019(3) -0.039(3) -0.024(3) C25 0.045(3) 0.035(3) 0.049(3) 0.014(2) -0.016(2) -0.016(2) C26 0.036(3) 0.061(3) 0.047(3) 0.018(2) 0.011(2) 0.017(2) C27 0.062(4) 0.118(6) 0.077(4) 0.010(4) 0.041(3) 0.024(4) C28 0.071(4) 0.057(4) 0.065(3) 0.018(3) 0.003(3) 0.016(3) C29 0.067(3) 0.032(3) 0.057(3) -0.011(2) -0.023(2) 0.000(3) C30 0.090(5) 0.037(3) 0.105(5) 0.015(3) -0.024(4) 0.005(3) C31 0.136(6) 0.074(5) 0.060(4) -0.017(3) -0.012(4) 0.022(4) N1 0.0205(16) 0.0155(16) 0.0215(14) 0.0000(12) 0.0008(11) -0.0011(13) N2 0.0236(17) 0.0232(18) 0.0237(15) 0.0066(13) 0.0005(12) 0.0034(14) Cl1 0.0782(9) 0.0284(6) 0.0491(6) 0.0012(5) -0.0026(6) 0.0068(6) Cl2 0.0345(6) 0.0908(10) 0.0431(6) 0.0316(6) 0.0000(5) -0.0229(6) Cl3 0.0471(7) 0.0616(8) 0.0254(5) 0.0129(5) -0.0067(4) -0.0166(6) In1 0.02928(18) 0.02532(17) 0.02261(16) 0.00945(11) -0.00004(10) -0.00637(13) _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 C1 N1 1.277(4) . ? C1 C2 1.463(5) . ? C1 C5 1.542(5) . ? C2 C7 1.389(5) 3_656 ? C2 C3 1.417(5) . ? C3 C3 1.361(7) 3_656 ? C3 C4 1.417(5) . ? C4 C6 1.381(5) . ? C4 C5 1.484(5) . ? C5 N2 1.261(4) . ? C6 C7 1.420(5) . ? C6 H6 0.9300 . ? C7 C2 1.389(5) 3_656 ? C7 H7 0.9300 . ? C8 C9 1.390(5) . ? C8 C13 1.395(5) . ? C8 N1 1.446(4) . ? C9 C10 1.392(5) . ? C9 C14 1.539(6) . ? C10 C11 1.362(6) . ? C10 H10 0.9300 . ? C11 C12 1.384(6) . ? C11 H11 0.9300 . ? C12 C13 1.399(5) . ? C12 H12 0.9300 . ? C13 C17 1.509(5) . ? C14 C16 1.513(7) . ? C14 C15 1.546(6) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.402(9) . ? C17 C18 1.407(8) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.387(6) . ? C20 C25 1.391(6) . ? C20 N2 1.450(5) . ? C21 C22 1.432(6) . ? C21 C26 1.515(7) . ? C22 C23 1.358(8) . ? C22 H22 0.9300 . ? C23 C24 1.345(8) . ? C23 H23 0.9300 . ? C24 C25 1.406(6) . ? C24 H24 0.9300 . ? C25 C29 1.510(7) . ? C26 C27 1.536(6) . ? C26 C28 1.557(7) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.530(7) . ? C29 C31 1.544(7) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 In1 2.309(3) . ? N2 In1 2.438(3) . ? Cl1 In1 2.3468(13) . ? Cl2 In1 2.3864(15) . ? Cl3 In1 2.3579(12) . ? 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 N1 C1 C2 133.4(3) . . ? N1 C1 C5 118.1(3) . . ? C2 C1 C5 108.1(3) . . ? C7 C2 C3 117.8(3) 3_656 . ? C7 C2 C1 138.0(3) 3_656 . ? C3 C2 C1 104.2(3) . . ? C3 C3 C4 122.0(4) 3_656 . ? C3 C3 C2 121.0(4) 3_656 . ? C4 C3 C2 117.0(3) . . ? C6 C4 C3 117.4(3) . . ? C6 C4 C5 138.3(3) . . ? C3 C4 C5 104.3(3) . . ? N2 C5 C4 134.1(3) . . ? N2 C5 C1 119.3(3) . . ? C4 C5 C1 106.4(3) . . ? C4 C6 C7 121.1(3) . . ? C4 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.7(3) 3_656 . ? C2 C7 H7 119.7 3_656 . ? C6 C7 H7 119.7 . . ? C9 C8 C13 123.8(3) . . ? C9 C8 N1 120.2(3) . . ? C13 C8 N1 116.0(3) . . ? C8 C9 C10 117.2(4) . . ? C8 C9 C14 123.1(3) . . ? C10 C9 C14 119.6(3) . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 121.0(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 116.1(4) . . ? C8 C13 C17 123.2(3) . . ? C12 C13 C17 120.7(4) . . ? C16 C14 C9 110.8(4) . . ? C16 C14 C15 110.4(4) . . ? C9 C14 C15 109.9(4) . . ? C16 C14 H14 108.6 . . ? C9 C14 H14 108.6 . . ? C15 C14 H14 108.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 109.5(7) . . ? C19 C17 C13 115.1(5) . . ? C18 C17 C13 115.6(5) . . ? C19 C17 H17 105.1 . . ? C18 C17 H17 105.1 . . ? C13 C17 H17 105.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 123.6(4) . . ? C21 C20 N2 119.5(4) . . ? C25 C20 N2 116.9(4) . . ? C20 C21 C22 115.3(5) . . ? C20 C21 C26 123.2(4) . . ? C22 C21 C26 121.5(4) . . ? C23 C22 C21 122.4(5) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C24 C23 C22 119.3(5) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 123.0(6) . . ? C23 C24 H24 118.5 . . ? C25 C24 H24 118.5 . . ? C20 C25 C24 116.2(5) . . ? C20 C25 C29 123.6(4) . . ? C24 C25 C29 120.2(5) . . ? C21 C26 C27 113.6(5) . . ? C21 C26 C28 108.7(4) . . ? C27 C26 C28 112.4(5) . . ? C21 C26 H26 107.3 . . ? C27 C26 H26 107.3 . . ? C28 C26 H26 107.3 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 C30 112.4(4) . . ? C25 C29 C31 112.8(4) . . ? C30 C29 C31 111.1(4) . . ? C25 C29 H29 106.7 . . ? C30 C29 H29 106.7 . . ? C31 C29 H29 106.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 N1 C8 119.2(3) . . ? C1 N1 In1 116.8(2) . . ? C8 N1 In1 124.0(2) . . ? C5 N2 C20 117.2(3) . . ? C5 N2 In1 112.7(2) . . ? C20 N2 In1 130.0(2) . . ? N1 In1 Cl1 100.11(8) . . ? N1 In1 Cl3 137.59(8) . . ? Cl1 In1 Cl3 117.39(4) . . ? N1 In1 Cl2 88.47(7) . . ? Cl1 In1 Cl2 104.86(5) . . ? Cl3 In1 Cl2 99.55(4) . . ? N1 In1 N2 71.07(10) . . ? Cl1 In1 N2 94.15(8) . . ? Cl3 In1 N2 86.39(7) . . ? Cl2 In1 N2 154.33(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C7 8.7(8) . . . 3_656 ? C5 C1 C2 C7 -179.3(4) . . . 3_656 ? N1 C1 C2 C3 -172.1(4) . . . . ? C5 C1 C2 C3 -0.1(4) . . . . ? C7 C2 C3 C3 -2.2(7) 3_656 . . 3_656 ? C1 C2 C3 C3 178.5(5) . . . 3_656 ? C7 C2 C3 C4 -179.2(4) 3_656 . . . ? C1 C2 C3 C4 1.4(5) . . . . ? C3 C3 C4 C6 2.3(7) 3_656 . . . ? C2 C3 C4 C6 179.3(4) . . . . ? C3 C3 C4 C5 -179.1(5) 3_656 . . . ? C2 C3 C4 C5 -2.1(5) . . . . ? C6 C4 C5 N2 -5.6(8) . . . . ? C3 C4 C5 N2 176.3(4) . . . . ? C6 C4 C5 C1 180.0(5) . . . . ? C3 C4 C5 C1 1.9(4) . . . . ? N1 C1 C5 N2 -3.1(5) . . . . ? C2 C1 C5 N2 -176.5(3) . . . . ? N1 C1 C5 C4 172.3(3) . . . . ? C2 C1 C5 C4 -1.1(4) . . . . ? C3 C4 C6 C7 -0.6(6) . . . . ? C5 C4 C6 C7 -178.5(4) . . . . ? C4 C6 C7 C2 -0.3(6) . . . 3_656 ? C13 C8 C9 C10 -2.6(5) . . . . ? N1 C8 C9 C10 179.2(3) . . . . ? C13 C8 C9 C14 176.2(4) . . . . ? N1 C8 C9 C14 -2.1(5) . . . . ? C8 C9 C10 C11 2.2(6) . . . . ? C14 C9 C10 C11 -176.6(4) . . . . ? C9 C10 C11 C12 -1.3(7) . . . . ? C10 C11 C12 C13 0.6(7) . . . . ? C9 C8 C13 C12 1.8(6) . . . . ? N1 C8 C13 C12 -179.9(3) . . . . ? C9 C8 C13 C17 -177.3(4) . . . . ? N1 C8 C13 C17 1.0(5) . . . . ? C11 C12 C13 C8 -0.8(6) . . . . ? C11 C12 C13 C17 178.4(4) . . . . ? C8 C9 C14 C16 -118.8(4) . . . . ? C10 C9 C14 C16 59.9(5) . . . . ? C8 C9 C14 C15 118.9(4) . . . . ? C10 C9 C14 C15 -62.4(5) . . . . ? C8 C13 C17 C19 -122.3(9) . . . . ? C12 C13 C17 C19 58.6(9) . . . . ? C8 C13 C17 C18 108.3(8) . . . . ? C12 C13 C17 C18 -70.8(8) . . . . ? C25 C20 C21 C22 5.0(6) . . . . ? N2 C20 C21 C22 -173.9(3) . . . . ? C25 C20 C21 C26 -172.8(4) . . . . ? N2 C20 C21 C26 8.2(6) . . . . ? C20 C21 C22 C23 -1.5(6) . . . . ? C26 C21 C22 C23 176.4(4) . . . . ? C21 C22 C23 C24 -1.7(7) . . . . ? C22 C23 C24 C25 1.9(8) . . . . ? C21 C20 C25 C24 -5.0(6) . . . . ? N2 C20 C25 C24 174.0(4) . . . . ? C21 C20 C25 C29 176.4(4) . . . . ? N2 C20 C25 C29 -4.7(6) . . . . ? C23 C24 C25 C20 1.3(7) . . . . ? C23 C24 C25 C29 -179.9(5) . . . . ? C20 C21 C26 C27 -130.6(5) . . . . ? C22 C21 C26 C27 51.7(6) . . . . ? C20 C21 C26 C28 103.4(5) . . . . ? C22 C21 C26 C28 -74.4(5) . . . . ? C20 C25 C29 C30 100.4(5) . . . . ? C24 C25 C29 C30 -78.2(5) . . . . ? C20 C25 C29 C31 -133.1(5) . . . . ? C24 C25 C29 C31 48.3(6) . . . . ? C2 C1 N1 C8 2.3(6) . . . . ? C5 C1 N1 C8 -169.2(3) . . . . ? C2 C1 N1 In1 -175.1(3) . . . . ? C5 C1 N1 In1 13.4(4) . . . . ? C9 C8 N1 C1 -90.8(4) . . . . ? C13 C8 N1 C1 90.9(4) . . . . ? C9 C8 N1 In1 86.4(3) . . . . ? C13 C8 N1 In1 -92.0(3) . . . . ? C4 C5 N2 C20 -3.9(6) . . . . ? C1 C5 N2 C20 170.0(3) . . . . ? C4 C5 N2 In1 178.0(3) . . . . ? C1 C5 N2 In1 -8.2(4) . . . . ? C21 C20 N2 C5 92.8(4) . . . . ? C25 C20 N2 C5 -86.2(4) . . . . ? C21 C20 N2 In1 -89.5(4) . . . . ? C25 C20 N2 In1 91.5(4) . . . . ? C1 N1 In1 Cl1 78.3(2) . . . . ? C8 N1 In1 Cl1 -98.9(2) . . . . ? C1 N1 In1 Cl3 -74.4(3) . . . . ? C8 N1 In1 Cl3 108.4(2) . . . . ? C1 N1 In1 Cl2 -176.9(2) . . . . ? C8 N1 In1 Cl2 5.9(2) . . . . ? C1 N1 In1 N2 -12.7(2) . . . . ? C8 N1 In1 N2 170.1(3) . . . . ? C5 N2 In1 N1 10.6(2) . . . . ? C20 N2 In1 N1 -167.2(3) . . . . ? C5 N2 In1 Cl1 -88.7(2) . . . . ? C20 N2 In1 Cl1 93.5(3) . . . . ? C5 N2 In1 Cl3 154.1(3) . . . . ? C20 N2 In1 Cl3 -23.7(3) . . . . ? C5 N2 In1 Cl2 49.5(3) . . . . ? C20 N2 In1 Cl2 -128.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.796 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.132 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 410.1 176.8 2 0.500 0.000 0.500 410.1 176.3 _platon_squeeze_details ; ; # Attachment 'kvkv136sq.cif' data_kvkv136sq _database_code_depnum_ccdc_archive 'CCDC 812615' #TrackingRef 'kvkv136sq.cif' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H72 Br6 In2 N4, C H2 Cl2' _chemical_formula_sum 'C63 H74 Br6 Cl2 In2 N4' _chemical_formula_weight 1667.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n _symmetry_space_group_name_Hall -p2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.178(5) _cell_length_b 21.687(5) _cell_length_c 15.394(5) _cell_angle_alpha 90.000 _cell_angle_beta 92.761(5) _cell_angle_gamma 90.000 _cell_volume 3394(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 4.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.484 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12781 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7768 _reflns_number_gt 4980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of disordered dichloromethane was removed using SQUEEZE. ; _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^)+(0.0421P)^2^+0.0000P] 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_extinction_coef ? _refine_ls_number_reflns 7768 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1185(4) 0.04391(18) 0.6651(2) 0.0167(9) Uani 1 1 d . . . C2 C 0.0656(4) -0.00850(19) 0.6145(2) 0.0188(9) Uani 1 1 d . . . C3 C 0.0298(4) 0.01767(18) 0.5323(2) 0.0182(9) Uani 1 1 d . . . C4 C 0.0539(4) 0.08110(18) 0.5212(2) 0.0186(9) Uani 1 1 d . . . C5 C 0.1138(4) 0.10059(19) 0.6059(2) 0.0180(9) Uani 1 1 d . . . C6 C 0.0140(4) 0.10739(19) 0.4418(2) 0.0216(10) Uani 1 1 d . . . H6 H 0.0262 0.1494 0.4332 0.026 Uiso 1 1 calc R . . C7 C -0.0446(4) 0.07130(19) 0.3738(2) 0.0216(10) Uani 1 1 d . . . H7 H -0.0693 0.0897 0.3209 0.026 Uiso 1 1 calc R . . C8 C 0.1245(4) -0.00071(18) 0.8017(2) 0.0190(10) Uani 1 1 d . . . C9 C 0.2264(4) -0.04115(19) 0.8280(2) 0.0229(10) Uani 1 1 d . . . C10 C 0.1897(5) -0.0935(2) 0.8746(3) 0.0358(12) Uani 1 1 d . . . H10 H 0.2531 -0.1225 0.8915 0.043 Uiso 1 1 calc R . . C11 C 0.0617(6) -0.1023(2) 0.8954(3) 0.0448(14) Uani 1 1 d . . . H11 H 0.0397 -0.1375 0.9260 0.054 Uiso 1 1 calc R . . C12 C -0.0351(5) -0.0603(2) 0.8724(3) 0.0365(12) Uani 1 1 d . . . H12 H -0.1206 -0.0668 0.8891 0.044 Uiso 1 1 calc R . . C13 C -0.0055(4) -0.0078(2) 0.8236(3) 0.0259(10) Uani 1 1 d . . . C14 C 0.3679(4) -0.0301(2) 0.8069(3) 0.0285(11) Uani 1 1 d . . . H14 H 0.3713 0.0089 0.7750 0.034 Uiso 1 1 calc R . . C15 C 0.4186(6) -0.0802(3) 0.7487(4) 0.0563(16) Uani 1 1 d . . . H15A H 0.4251 -0.1183 0.7804 0.084 Uiso 1 1 calc R . . H15B H 0.5038 -0.0689 0.7298 0.084 Uiso 1 1 calc R . . H15C H 0.3589 -0.0853 0.6989 0.084 Uiso 1 1 calc R . . C16 C 0.4558(5) -0.0236(3) 0.8882(3) 0.0596(17) Uani 1 1 d . . . H16A H 0.4216 0.0079 0.9246 0.089 Uiso 1 1 calc R . . H16B H 0.5429 -0.0125 0.8726 0.089 Uiso 1 1 calc R . . H16C H 0.4589 -0.0621 0.9191 0.089 Uiso 1 1 calc R . . C17 C -0.1155(5) 0.0376(2) 0.7988(3) 0.0374(12) Uani 1 1 d . . . H17 H -0.0777 0.0718 0.7667 0.045 Uiso 1 1 calc R . . C18 C -0.1764(5) 0.0637(3) 0.8796(4) 0.0570(16) Uani 1 1 d . . . H18A H -0.2058 0.0305 0.9150 0.086 Uiso 1 1 calc R . . H18B H -0.2499 0.0895 0.8623 0.086 Uiso 1 1 calc R . . H18C H -0.1120 0.0877 0.9122 0.086 Uiso 1 1 calc R . . C19 C -0.2234(5) 0.0077(3) 0.7406(3) 0.0499(15) Uani 1 1 d . . . H19A H -0.1884 -0.0034 0.6860 0.075 Uiso 1 1 calc R . . H19B H -0.2945 0.0363 0.7308 0.075 Uiso 1 1 calc R . . H19C H -0.2551 -0.0286 0.7685 0.075 Uiso 1 1 calc R . . C20 C 0.1262(4) 0.20657(18) 0.5823(2) 0.0208(10) Uani 1 1 d . . . C21 C 0.2214(5) 0.22139(19) 0.5230(3) 0.0248(10) Uani 1 1 d . . . C22 C 0.1943(5) 0.2716(2) 0.4689(3) 0.0318(11) Uani 1 1 d . . . H22 H 0.2551 0.2830 0.4286 0.038 Uiso 1 1 calc R . . C23 C 0.0789(5) 0.3052(2) 0.4735(3) 0.0388(13) Uani 1 1 d . . . H23 H 0.0622 0.3382 0.4361 0.047 Uiso 1 1 calc R . . C24 C -0.0114(5) 0.2894(2) 0.5341(3) 0.0362(12) Uani 1 1 d . . . H24 H -0.0882 0.3124 0.5371 0.043 Uiso 1 1 calc R . . C25 C 0.0098(4) 0.2400(2) 0.5903(3) 0.0259(10) Uani 1 1 d . . . C26 C 0.3488(5) 0.1864(2) 0.5154(3) 0.0324(11) Uani 1 1 d . . . H26 H 0.3490 0.1522 0.5570 0.039 Uiso 1 1 calc R . . C27 C 0.3632(6) 0.1590(3) 0.4246(3) 0.0573(16) Uani 1 1 d . . . H27A H 0.2870 0.1346 0.4088 0.086 Uiso 1 1 calc R . . H27B H 0.4402 0.1334 0.4250 0.086 Uiso 1 1 calc R . . H27C H 0.3715 0.1917 0.3832 0.086 Uiso 1 1 calc R . . C28 C 0.4675(5) 0.2274(3) 0.5395(4) 0.0528(15) Uani 1 1 d . . . H28A H 0.4692 0.2616 0.5001 0.079 Uiso 1 1 calc R . . H28B H 0.5469 0.2038 0.5358 0.079 Uiso 1 1 calc R . . H28C H 0.4609 0.2424 0.5978 0.079 Uiso 1 1 calc R . . C29 C -0.0925(5) 0.2210(2) 0.6541(3) 0.0340(12) Uani 1 1 d . . . H29 H -0.0454 0.2024 0.7045 0.041 Uiso 1 1 calc R . . C30 C -0.1866(5) 0.1725(3) 0.6154(4) 0.0511(15) Uani 1 1 d . . . H30A H -0.2248 0.1871 0.5610 0.077 Uiso 1 1 calc R . . H30B H -0.2550 0.1648 0.6548 0.077 Uiso 1 1 calc R . . H30C H -0.1393 0.1350 0.6059 0.077 Uiso 1 1 calc R . . C31 C -0.1706(6) 0.2752(3) 0.6869(4) 0.0559(16) Uani 1 1 d . . . H31A H -0.1112 0.3060 0.7103 0.084 Uiso 1 1 calc R . . H31B H -0.2265 0.2613 0.7314 0.084 Uiso 1 1 calc R . . H31C H -0.2235 0.2924 0.6396 0.084 Uiso 1 1 calc R . . N1 N 0.1536(3) 0.05097(15) 0.74514(19) 0.0194(8) Uani 1 1 d . . . N2 N 0.1459(3) 0.15287(15) 0.6376(2) 0.0189(8) Uani 1 1 d . . . In1 In 0.24362(3) 0.151045(14) 0.781284(18) 0.02402(10) Uani 1 1 d . . . Br1 Br 0.47429(5) 0.12807(2) 0.74151(3) 0.03325(14) Uani 1 1 d . . . Br2 Br 0.19293(6) 0.12417(3) 0.93429(3) 0.0592(2) Uani 1 1 d . . . Br3 Br 0.22467(8) 0.26609(3) 0.78914(4) 0.0733(2) Uani 1 1 d . . . 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 C1 0.016(2) 0.019(2) 0.015(2) -0.0031(18) 0.0002(16) -0.0005(18) C2 0.017(2) 0.023(2) 0.016(2) 0.0018(18) 0.0033(17) 0.0018(19) C3 0.023(2) 0.018(2) 0.014(2) 0.0002(17) 0.0030(17) -0.0029(18) C4 0.022(2) 0.018(2) 0.016(2) 0.0022(18) -0.0012(17) -0.0002(19) C5 0.017(2) 0.019(2) 0.018(2) -0.0022(19) -0.0013(17) 0.0002(18) C6 0.025(3) 0.017(2) 0.022(2) 0.0051(19) -0.0002(18) -0.0015(19) C7 0.024(3) 0.024(2) 0.016(2) 0.0005(18) -0.0029(18) -0.002(2) C8 0.028(3) 0.017(2) 0.0116(19) 0.0009(17) 0.0010(18) -0.0014(19) C9 0.028(3) 0.023(2) 0.018(2) -0.0020(19) -0.0021(18) -0.007(2) C10 0.043(4) 0.026(3) 0.038(3) 0.013(2) -0.003(2) 0.003(2) C11 0.049(4) 0.045(3) 0.041(3) 0.019(3) 0.006(3) -0.010(3) C12 0.034(3) 0.047(3) 0.028(3) 0.006(2) 0.004(2) -0.015(3) C13 0.027(3) 0.033(3) 0.018(2) -0.001(2) 0.0016(19) -0.006(2) C14 0.027(3) 0.023(2) 0.035(3) 0.004(2) -0.003(2) 0.003(2) C15 0.039(4) 0.059(4) 0.072(4) -0.028(3) 0.010(3) -0.004(3) C16 0.039(4) 0.093(5) 0.046(3) -0.007(3) -0.009(3) -0.010(3) C17 0.022(3) 0.045(3) 0.045(3) -0.002(2) 0.005(2) 0.000(2) C18 0.034(3) 0.065(4) 0.073(4) -0.036(3) 0.004(3) 0.002(3) C19 0.032(3) 0.072(4) 0.046(3) -0.010(3) 0.003(2) 0.010(3) C20 0.029(3) 0.014(2) 0.018(2) 0.0033(18) -0.0094(18) -0.007(2) C21 0.032(3) 0.023(2) 0.019(2) -0.0008(19) -0.0070(19) -0.004(2) C22 0.042(3) 0.026(3) 0.026(2) 0.001(2) -0.005(2) -0.006(2) C23 0.046(4) 0.029(3) 0.040(3) 0.014(2) -0.016(3) 0.002(3) C24 0.039(3) 0.027(3) 0.041(3) 0.003(2) -0.013(2) 0.009(2) C25 0.023(3) 0.026(3) 0.027(2) -0.005(2) -0.0090(19) -0.002(2) C26 0.032(3) 0.031(3) 0.035(3) 0.008(2) 0.012(2) 0.003(2) C27 0.065(4) 0.058(4) 0.050(3) -0.003(3) 0.018(3) 0.007(3) C28 0.036(4) 0.056(4) 0.066(4) 0.010(3) 0.003(3) 0.001(3) C29 0.024(3) 0.042(3) 0.036(3) 0.001(2) -0.002(2) 0.005(2) C30 0.029(3) 0.059(4) 0.066(4) -0.010(3) 0.006(3) -0.006(3) C31 0.047(4) 0.059(4) 0.062(4) -0.020(3) 0.015(3) 0.003(3) N1 0.022(2) 0.0210(19) 0.0152(17) 0.0019(15) -0.0002(15) -0.0002(16) N2 0.021(2) 0.0179(19) 0.0174(17) -0.0021(15) -0.0031(14) -0.0001(16) In1 0.02405(19) 0.02615(18) 0.02142(17) -0.00591(14) -0.00339(12) -0.00051(15) Br1 0.0238(3) 0.0409(3) 0.0352(3) 0.0021(2) 0.0021(2) -0.0012(2) Br2 0.0777(5) 0.0755(4) 0.0258(3) -0.0198(3) 0.0169(3) -0.0464(4) Br3 0.1195(6) 0.0325(3) 0.0630(4) -0.0218(3) -0.0474(4) 0.0261(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.275(4) . ? C1 C2 1.466(5) . ? C1 C5 1.530(5) . ? C2 C7 1.392(6) 3_556 ? C2 C3 1.419(5) . ? C3 C3 1.373(8) 3_556 ? C3 C4 1.409(5) . ? C4 C6 1.392(5) . ? C4 C5 1.473(5) . ? C5 N2 1.271(5) . ? C6 C7 1.416(5) . ? C6 H6 0.9300 . ? C7 C2 1.392(6) 3_556 ? C7 H7 0.9300 . ? C8 C13 1.390(6) . ? C8 C9 1.402(6) . ? C8 N1 1.459(5) . ? C9 C10 1.403(6) . ? C9 C14 1.511(6) . ? C10 C11 1.370(7) . ? C10 H10 0.9300 . ? C11 C12 1.374(7) . ? C11 H11 0.9300 . ? C12 C13 1.405(6) . ? C12 H12 0.9300 . ? C13 C17 1.524(6) . ? C14 C16 1.510(6) . ? C14 C15 1.516(6) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.525(7) . ? C17 C19 1.528(7) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C25 1.400(6) . ? C20 C21 1.400(6) . ? C20 N2 1.451(5) . ? C21 C22 1.391(6) . ? C21 C26 1.512(6) . ? C22 C23 1.386(7) . ? C22 H22 0.9300 . ? C23 C24 1.383(7) . ? C23 H23 0.9300 . ? C24 C25 1.387(6) . ? C24 H24 0.9300 . ? C25 C29 1.522(6) . ? C26 C28 1.531(7) . ? C26 C27 1.532(7) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C31 1.518(7) . ? C29 C30 1.525(7) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 In1 2.411(3) . ? N2 In1 2.381(3) . ? In1 Br2 2.5041(9) . ? In1 Br1 2.5047(12) . ? In1 Br3 2.5058(8) . ? 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 N1 C1 C2 133.3(4) . . ? N1 C1 C5 118.6(3) . . ? C2 C1 C5 107.8(3) . . ? C7 C2 C3 118.2(4) 3_556 . ? C7 C2 C1 138.2(4) 3_556 . ? C3 C2 C1 103.7(3) . . ? C3 C3 C4 122.1(4) 3_556 . ? C3 C3 C2 120.6(5) 3_556 . ? C4 C3 C2 117.4(3) . . ? C6 C4 C3 117.5(4) . . ? C6 C4 C5 138.6(4) . . ? C3 C4 C5 103.9(3) . . ? N2 C5 C4 133.1(4) . . ? N2 C5 C1 119.1(3) . . ? C4 C5 C1 107.3(3) . . ? C4 C6 C7 121.2(4) . . ? C4 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C2 C7 C6 120.5(4) 3_556 . ? C2 C7 H7 119.8 3_556 . ? C6 C7 H7 119.8 . . ? C13 C8 C9 124.1(4) . . ? C13 C8 N1 116.9(4) . . ? C9 C8 N1 119.0(4) . . ? C8 C9 C10 116.2(4) . . ? C8 C9 C14 122.6(4) . . ? C10 C9 C14 121.2(4) . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 121.7(5) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 116.7(4) . . ? C8 C13 C17 124.3(4) . . ? C12 C13 C17 118.9(4) . . ? C16 C14 C9 111.7(4) . . ? C16 C14 C15 110.6(4) . . ? C9 C14 C15 111.6(4) . . ? C16 C14 H14 107.6 . . ? C9 C14 H14 107.6 . . ? C15 C14 H14 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 111.0(4) . . ? C13 C17 C19 111.8(4) . . ? C18 C17 C19 109.0(4) . . ? C13 C17 H17 108.3 . . ? C18 C17 H17 108.3 . . ? C19 C17 H17 108.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 123.6(4) . . ? C25 C20 N2 117.3(4) . . ? C21 C20 N2 119.1(4) . . ? C22 C21 C20 116.6(4) . . ? C22 C21 C26 119.5(4) . . ? C20 C21 C26 123.9(4) . . ? C23 C22 C21 121.6(5) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 119.8(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 121.5(5) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C20 116.9(4) . . ? C24 C25 C29 121.4(4) . . ? C20 C25 C29 121.7(4) . . ? C21 C26 C28 111.1(4) . . ? C21 C26 C27 112.7(4) . . ? C28 C26 C27 109.7(4) . . ? C21 C26 H26 107.7 . . ? C28 C26 H26 107.7 . . ? C27 C26 H26 107.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C25 113.0(4) . . ? C31 C29 C30 109.5(4) . . ? C25 C29 C30 111.7(4) . . ? C31 C29 H29 107.4 . . ? C25 C29 H29 107.4 . . ? C30 C29 H29 107.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 N1 C8 115.4(3) . . ? C1 N1 In1 114.6(3) . . ? C8 N1 In1 129.8(2) . . ? C5 N2 C20 117.7(3) . . ? C5 N2 In1 115.5(3) . . ? C20 N2 In1 126.7(2) . . ? N2 In1 N1 70.34(11) . . ? N2 In1 Br2 141.43(9) . . ? N1 In1 Br2 85.08(7) . . ? N2 In1 Br1 97.51(8) . . ? N1 In1 Br1 96.60(8) . . ? Br2 In1 Br1 114.94(2) . . ? N2 In1 Br3 89.92(8) . . ? N1 In1 Br3 151.44(8) . . ? Br2 In1 Br3 99.58(2) . . ? Br1 In1 Br3 106.56(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C7 -8.8(9) . . . 3_556 ? C5 C1 C2 C7 178.2(5) . . . 3_556 ? N1 C1 C2 C3 171.5(4) . . . . ? C5 C1 C2 C3 -1.5(4) . . . . ? C7 C2 C3 C3 3.1(7) 3_556 . . 3_556 ? C1 C2 C3 C3 -177.1(5) . . . 3_556 ? C7 C2 C3 C4 -178.9(4) 3_556 . . . ? C1 C2 C3 C4 0.8(5) . . . . ? C3 C3 C4 C6 0.4(7) 3_556 . . . ? C2 C3 C4 C6 -177.5(4) . . . . ? C3 C3 C4 C5 178.2(5) 3_556 . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C6 C4 C5 N2 4.0(9) . . . . ? C3 C4 C5 N2 -173.0(4) . . . . ? C6 C4 C5 C1 175.8(5) . . . . ? C3 C4 C5 C1 -1.2(4) . . . . ? N1 C1 C5 N2 0.6(6) . . . . ? C2 C1 C5 N2 174.9(4) . . . . ? N1 C1 C5 C4 -172.5(4) . . . . ? C2 C1 C5 C4 1.7(4) . . . . ? C3 C4 C6 C7 -2.0(6) . . . . ? C5 C4 C6 C7 -178.7(5) . . . . ? C4 C6 C7 C2 1.0(6) . . . 3_556 ? C13 C8 C9 C10 4.0(6) . . . . ? N1 C8 C9 C10 -173.5(3) . . . . ? C13 C8 C9 C14 -176.6(4) . . . . ? N1 C8 C9 C14 5.9(5) . . . . ? C8 C9 C10 C11 -2.5(6) . . . . ? C14 C9 C10 C11 178.2(4) . . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C10 C11 C12 C13 2.2(7) . . . . ? C9 C8 C13 C12 -2.5(6) . . . . ? N1 C8 C13 C12 175.1(3) . . . . ? C9 C8 C13 C17 177.1(4) . . . . ? N1 C8 C13 C17 -5.4(6) . . . . ? C11 C12 C13 C8 -0.7(6) . . . . ? C11 C12 C13 C17 179.7(4) . . . . ? C8 C9 C14 C16 119.2(4) . . . . ? C10 C9 C14 C16 -61.5(6) . . . . ? C8 C9 C14 C15 -116.4(5) . . . . ? C10 C9 C14 C15 62.9(5) . . . . ? C8 C13 C17 C18 -119.9(5) . . . . ? C12 C13 C17 C18 59.7(5) . . . . ? C8 C13 C17 C19 118.1(5) . . . . ? C12 C13 C17 C19 -62.3(5) . . . . ? C25 C20 C21 C22 -1.3(6) . . . . ? N2 C20 C21 C22 177.1(3) . . . . ? C25 C20 C21 C26 178.6(4) . . . . ? N2 C20 C21 C26 -3.1(6) . . . . ? C20 C21 C22 C23 -0.1(6) . . . . ? C26 C21 C22 C23 -179.9(4) . . . . ? C21 C22 C23 C24 1.0(7) . . . . ? C22 C23 C24 C25 -0.7(7) . . . . ? C23 C24 C25 C20 -0.6(6) . . . . ? C23 C24 C25 C29 -177.3(4) . . . . ? C21 C20 C25 C24 1.6(6) . . . . ? N2 C20 C25 C24 -176.8(3) . . . . ? C21 C20 C25 C29 178.3(4) . . . . ? N2 C20 C25 C29 -0.1(6) . . . . ? C22 C21 C26 C28 64.1(5) . . . . ? C20 C21 C26 C28 -115.8(5) . . . . ? C22 C21 C26 C27 -59.5(5) . . . . ? C20 C21 C26 C27 120.6(5) . . . . ? C24 C25 C29 C31 -32.7(6) . . . . ? C20 C25 C29 C31 150.8(4) . . . . ? C24 C25 C29 C30 91.4(5) . . . . ? C20 C25 C29 C30 -85.1(5) . . . . ? C2 C1 N1 C8 -7.3(7) . . . . ? C5 C1 N1 C8 165.2(3) . . . . ? C2 C1 N1 In1 177.0(4) . . . . ? C5 C1 N1 In1 -10.6(5) . . . . ? C13 C8 N1 C1 -75.7(5) . . . . ? C9 C8 N1 C1 102.0(4) . . . . ? C13 C8 N1 In1 99.2(4) . . . . ? C9 C8 N1 In1 -83.1(4) . . . . ? C4 C5 N2 C20 -2.2(7) . . . . ? C1 C5 N2 C20 -173.2(4) . . . . ? C4 C5 N2 In1 -179.1(4) . . . . ? C1 C5 N2 In1 9.9(5) . . . . ? C25 C20 N2 C5 95.8(4) . . . . ? C21 C20 N2 C5 -82.7(5) . . . . ? C25 C20 N2 In1 -87.6(4) . . . . ? C21 C20 N2 In1 93.9(4) . . . . ? C5 N2 In1 N1 -10.8(3) . . . . ? C20 N2 In1 N1 172.5(3) . . . . ? C5 N2 In1 Br2 -64.4(3) . . . . ? C20 N2 In1 Br2 119.0(3) . . . . ? C5 N2 In1 Br1 83.6(3) . . . . ? C20 N2 In1 Br1 -93.1(3) . . . . ? C5 N2 In1 Br3 -169.7(3) . . . . ? C20 N2 In1 Br3 13.6(3) . . . . ? C1 N1 In1 N2 11.1(3) . . . . ? C8 N1 In1 N2 -163.9(4) . . . . ? C1 N1 In1 Br2 160.9(3) . . . . ? C8 N1 In1 Br2 -14.1(3) . . . . ? C1 N1 In1 Br1 -84.5(3) . . . . ? C8 N1 In1 Br1 100.5(3) . . . . ? C1 N1 In1 Br3 59.8(4) . . . . ? C8 N1 In1 Br3 -115.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.281 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.125 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 124.0 41.9 2 0.069 0.192 0.272 27.3 0.6 3 0.500 1.000 0.500 124.1 42.3 4 0.430 0.692 0.228 27.3 -0.2 5 0.569 0.308 0.772 27.3 0.5 6 0.930 0.808 0.728 27.3 0.0 _platon_squeeze_details ; ;