# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Cameron Jones' 'Shaun P. Green' 'Andreas Stasch' _publ_contact_author_name 'Prof Cameron Jones' _publ_contact_author_email CAMERON.JONES@SCI.MONASH.EDU.AU _publ_section_title ; Synthesis and Structural Characterisation of a Soluble, Metastable Indium(I) Halide Complex, [InBr(tmeda)] ; # Attachment '[In2Br4_tmeda_2].CIF' data_[In2Br4(tmeda)2] _database_code_depnum_ccdc_archive 'CCDC 699631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Br4 In2 N4' _chemical_formula_weight 781.70 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca 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 17.327(4) _cell_length_b 12.110(2) _cell_length_c 22.420(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4704.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 8.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_T_max 0.353 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 32336 _diffrn_reflns_av_R_equivalents 0.1382 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4317 _reflns_number_gt 2539 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^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 4317 _refine_ls_number_parameters 208 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.06494(4) 0.21178(6) 0.35853(3) 0.0261(2) Uani 1 1 d . . . In2 In -0.07530(4) 0.28265(6) 0.40269(3) 0.0278(2) Uani 1 1 d . . . Br1 Br 0.01638(7) 0.00028(9) 0.34276(5) 0.0384(3) Uani 1 1 d . . . Br2 Br 0.18490(6) 0.14822(10) 0.41700(6) 0.0420(4) Uani 1 1 d . . . Br3 Br -0.13388(7) 0.32065(11) 0.29266(5) 0.0479(4) Uani 1 1 d . . . Br4 Br -0.11122(7) 0.47552(10) 0.44083(6) 0.0446(4) Uani 1 1 d . . . N1 N 0.1113(5) 0.2082(8) 0.2612(4) 0.040(3) Uani 1 1 d . . . N2 N 0.1256(5) 0.3919(7) 0.3452(4) 0.031(2) Uani 1 1 d . . . N3 N -0.1843(5) 0.1740(8) 0.4217(4) 0.034(2) Uani 1 1 d D . . N4 N -0.0586(4) 0.2194(7) 0.5070(4) 0.024(2) Uani 1 1 d D . . C1 C 0.0507(8) 0.1786(11) 0.2194(5) 0.055(4) Uani 1 1 d . . . H1A H 0.0715 0.1780 0.1788 0.082 Uiso 1 1 calc R . . H1B H 0.0087 0.2327 0.2220 0.082 Uiso 1 1 calc R . . H1C H 0.0308 0.1050 0.2293 0.082 Uiso 1 1 calc R . . C2 C 0.1730(7) 0.1223(10) 0.2576(6) 0.053(4) Uani 1 1 d . . . H2A H 0.1539 0.0531 0.2747 0.080 Uiso 1 1 calc R . . H2B H 0.2185 0.1472 0.2798 0.080 Uiso 1 1 calc R . . H2C H 0.1871 0.1103 0.2157 0.080 Uiso 1 1 calc R . . C3 C 0.1441(8) 0.3190(9) 0.2450(5) 0.050(4) Uani 1 1 d . . . H3A H 0.1831 0.3095 0.2132 0.060 Uiso 1 1 calc R . . H3B H 0.1023 0.3663 0.2290 0.060 Uiso 1 1 calc R . . C4 C 0.1805(7) 0.3754(10) 0.2970(6) 0.052(4) Uani 1 1 d . . . H4A H 0.2242 0.3303 0.3117 0.062 Uiso 1 1 calc R . . H4B H 0.2011 0.4479 0.2842 0.062 Uiso 1 1 calc R . . C5 C 0.1658(7) 0.4337(11) 0.3999(6) 0.052(4) Uani 1 1 d . . . H5A H 0.2063 0.3815 0.4116 0.078 Uiso 1 1 calc R . . H5B H 0.1284 0.4409 0.4325 0.078 Uiso 1 1 calc R . . H5C H 0.1889 0.5058 0.3915 0.078 Uiso 1 1 calc R . . C6 C 0.0658(6) 0.4735(9) 0.3292(6) 0.052(4) Uani 1 1 d . . . H6A H 0.0905 0.5431 0.3177 0.079 Uiso 1 1 calc R . . H6B H 0.0320 0.4862 0.3636 0.079 Uiso 1 1 calc R . . H6C H 0.0352 0.4454 0.2957 0.079 Uiso 1 1 calc R . . C7 C -0.1869(6) 0.0834(10) 0.3777(6) 0.042(3) Uani 1 1 d . . . H7A H -0.2300 0.0339 0.3871 0.064 Uiso 1 1 calc R . . H7B H -0.1384 0.0419 0.3791 0.064 Uiso 1 1 calc R . . H7C H -0.1941 0.1142 0.3376 0.064 Uiso 1 1 calc R . . C8 C -0.2540(6) 0.2422(11) 0.4163(5) 0.049(4) Uani 1 1 d . . . H8A H -0.2593 0.2678 0.3750 0.074 Uiso 1 1 calc R . . H8B H -0.2498 0.3060 0.4430 0.074 Uiso 1 1 calc R . . H8C H -0.2993 0.1983 0.4273 0.074 Uiso 1 1 calc R . . C9 C -0.1819(6) 0.1305(12) 0.4837(5) 0.059(4) Uani 1 1 d DU . . H9A H -0.2062 0.0565 0.4841 0.071 Uiso 1 1 calc R . . H9B H -0.2136 0.1794 0.5094 0.071 Uiso 1 1 calc R . . C10 C -0.1030(7) 0.1213(13) 0.5106(7) 0.095(5) Uani 1 1 d DU . . H10A H -0.1083 0.1002 0.5531 0.113 Uiso 1 1 calc R . . H10B H -0.0746 0.0612 0.4901 0.113 Uiso 1 1 calc R . . C11 C -0.0714(9) 0.2967(12) 0.5549(7) 0.076(5) Uani 1 1 d U . . H11A H -0.0636 0.2595 0.5932 0.113 Uiso 1 1 calc R . . H11B H -0.1244 0.3248 0.5527 0.113 Uiso 1 1 calc R . . H11C H -0.0351 0.3583 0.5513 0.113 Uiso 1 1 calc R . . C12 C 0.0211(9) 0.1790(13) 0.5140(7) 0.083(5) Uani 1 1 d U . . H12A H 0.0249 0.1346 0.5504 0.124 Uiso 1 1 calc R . . H12B H 0.0564 0.2420 0.5167 0.124 Uiso 1 1 calc R . . H12C H 0.0350 0.1335 0.4795 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0234(4) 0.0264(5) 0.0285(5) -0.0012(4) -0.0002(3) 0.0019(3) In2 0.0214(4) 0.0273(5) 0.0346(5) 0.0060(4) 0.0005(3) 0.0009(3) Br1 0.0470(7) 0.0273(7) 0.0411(7) -0.0002(6) 0.0034(6) -0.0050(6) Br2 0.0285(6) 0.0422(8) 0.0554(8) 0.0013(6) -0.0067(6) 0.0072(6) Br3 0.0352(7) 0.0657(10) 0.0427(8) 0.0220(7) -0.0074(6) -0.0084(6) Br4 0.0443(7) 0.0305(8) 0.0589(9) 0.0049(6) 0.0083(6) 0.0147(6) N1 0.043(6) 0.035(6) 0.044(6) 0.000(5) 0.018(5) -0.010(5) N2 0.023(5) 0.019(5) 0.051(6) -0.005(5) 0.006(5) 0.001(4) N3 0.023(5) 0.045(6) 0.035(6) 0.015(5) -0.008(4) -0.009(4) N4 0.022(5) 0.020(5) 0.030(5) -0.003(4) -0.002(4) -0.005(4) C1 0.064(9) 0.065(10) 0.034(7) -0.003(7) 0.006(7) -0.012(8) C2 0.070(9) 0.039(8) 0.050(8) 0.000(7) 0.039(7) 0.010(7) C3 0.071(9) 0.032(8) 0.046(8) 0.006(7) 0.028(7) 0.000(7) C4 0.041(7) 0.041(8) 0.074(10) -0.004(7) 0.011(7) -0.014(6) C5 0.044(7) 0.040(8) 0.071(10) -0.017(7) 0.003(7) -0.015(6) C6 0.036(7) 0.037(8) 0.084(10) 0.004(7) -0.016(7) 0.009(6) C7 0.031(7) 0.035(8) 0.061(9) 0.004(7) 0.006(6) -0.012(6) C8 0.019(6) 0.086(10) 0.043(8) -0.019(7) 0.006(6) -0.012(6) C9 0.047(6) 0.072(6) 0.058(6) 0.021(5) 0.001(5) -0.015(5) C10 0.101(8) 0.098(8) 0.084(7) 0.022(6) -0.009(6) -0.021(6) C11 0.094(7) 0.065(7) 0.067(7) -0.006(6) -0.012(6) 0.004(6) C12 0.082(7) 0.091(7) 0.076(7) 0.014(6) -0.001(6) 0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 N1 2.326(9) . ? In1 N2 2.440(8) . ? In1 Br2 2.5752(14) . ? In1 Br1 2.7190(14) . ? In1 In2 2.7608(11) . ? In2 N3 2.341(8) . ? In2 N4 2.478(8) . ? In2 Br4 2.5639(14) . ? In2 Br3 2.7070(14) . ? N1 C1 1.453(15) . ? N1 C2 1.493(14) . ? N1 C3 1.501(14) . ? N2 C4 1.453(13) . ? N2 C6 1.475(13) . ? N2 C5 1.499(14) . ? N3 C8 1.468(14) . ? N3 C7 1.477(15) . ? N3 C9 1.487(12) . ? N4 C10 1.417(13) . ? N4 C11 1.441(16) . ? N4 C12 1.473(16) . ? C3 C4 1.492(16) . ? C9 C10 1.500(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 In1 N2 75.7(3) . . ? N1 In1 Br2 101.1(3) . . ? N2 In1 Br2 89.0(2) . . ? N1 In1 Br1 88.1(2) . . ? N2 In1 Br1 163.7(2) . . ? Br2 In1 Br1 91.97(5) . . ? N1 In1 In2 130.3(3) . . ? N2 In1 In2 98.34(19) . . ? Br2 In1 In2 128.37(5) . . ? Br1 In1 In2 93.84(4) . . ? N3 In2 N4 75.4(3) . . ? N3 In2 Br4 104.8(2) . . ? N4 In2 Br4 89.72(19) . . ? N3 In2 Br3 87.7(2) . . ? N4 In2 Br3 163.03(18) . . ? Br4 In2 Br3 93.32(5) . . ? N3 In2 In1 126.9(2) . . ? N4 In2 In1 98.03(18) . . ? Br4 In2 In1 128.06(4) . . ? Br3 In2 In1 93.21(4) . . ? C1 N1 C2 108.1(10) . . ? C1 N1 C3 109.8(10) . . ? C2 N1 C3 109.8(9) . . ? C1 N1 In1 111.0(7) . . ? C2 N1 In1 108.1(7) . . ? C3 N1 In1 109.9(7) . . ? C4 N2 C6 111.8(10) . . ? C4 N2 C5 110.5(9) . . ? C6 N2 C5 107.4(9) . . ? C4 N2 In1 104.5(6) . . ? C6 N2 In1 109.1(6) . . ? C5 N2 In1 113.6(7) . . ? C8 N3 C7 109.7(9) . . ? C8 N3 C9 107.4(9) . . ? C7 N3 C9 111.3(10) . . ? C8 N3 In2 109.4(7) . . ? C7 N3 In2 108.7(6) . . ? C9 N3 In2 110.3(6) . . ? C10 N4 C11 114.7(11) . . ? C10 N4 C12 102.9(10) . . ? C11 N4 C12 106.3(10) . . ? C10 N4 In2 104.4(7) . . ? C11 N4 In2 119.0(8) . . ? C12 N4 In2 108.2(7) . . ? C4 C3 N1 112.3(10) . . ? N2 C4 C3 111.5(9) . . ? N3 C9 C10 115.3(10) . . ? N4 C10 C9 114.1(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.705 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.243 # Attachment '[_quin_2_H][In5Cl8_quin_5].CIF' data_[(quin)2)H][In5Cl8(quin)5] _database_code_depnum_ccdc_archive 'CCDC 699632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H92 Cl8 In5 N7' _chemical_formula_weight 1637.00 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.079(2) _cell_length_b 21.690(4) _cell_length_c 12.363(3) _cell_angle_alpha 90.38(3) _cell_angle_beta 97.84(3) _cell_angle_gamma 103.65(3) _cell_volume 3115.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 2.204 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.621 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 20134 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.09 _reflns_number_total 10832 _reflns_number_gt 8006 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal chosen for the diffraction experiment was a non-merohedral twin. All attempts to find a more suitable crystal for the experiment failed. In addition, all attempts to deconvolute the diffraction patterns of the twin components failed. This led to a number of large residual electron density peaks in the final difference map (highest 5.152 e/A3, near In5). This led to poor r-factors for the structure. Despite this, the molecular connectivity of the compound is unambiguous. ; _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^)+(0.0598P)^2^+326.8534P] 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 10832 _refine_ls_number_parameters 622 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1388 _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.3065 _refine_ls_wR_factor_gt 0.2923 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.94305(12) 0.24416(7) 0.20879(12) 0.0223(3) Uani 1 1 d . . . In2 In 1.14635(13) 0.29732(7) 0.34495(13) 0.0276(4) Uani 1 1 d . . . In3 In 0.95959(13) 0.14249(7) 0.08290(12) 0.0253(4) Uani 1 1 d . . . In4 In 0.86859(12) 0.33361(7) 0.08061(12) 0.0232(4) Uani 1 1 d . . . In5 In 0.76194(14) 0.19323(8) 0.32092(14) 0.0324(4) Uani 1 1 d . . . Cl1 Cl 1.2198(5) 0.4061(3) 0.4242(4) 0.0324(12) Uani 1 1 d . . . Cl2 Cl 1.2845(5) 0.2313(3) 0.3943(5) 0.0321(12) Uani 1 1 d . . . Cl3 Cl 1.1110(5) 0.1429(3) -0.0282(5) 0.0330(12) Uani 1 1 d . . . Cl4 Cl 0.7901(5) 0.0800(3) -0.0306(5) 0.0390(14) Uani 1 1 d . . . Cl5 Cl 0.6659(5) 0.3151(3) 0.0009(5) 0.0350(13) Uani 1 1 d . . . Cl6 Cl 0.9576(5) 0.3949(3) -0.0611(5) 0.0394(14) Uani 1 1 d . . . Cl7 Cl 0.6883(5) 0.2634(3) 0.4344(5) 0.0403(14) Uani 1 1 d . . . Cl8 Cl 0.7681(6) 0.1031(3) 0.4401(5) 0.0453(15) Uani 1 1 d . . . N1 N 1.2718(15) 0.3367(9) 0.2068(15) 0.030(4) Uani 1 1 d . . . N2 N 1.0911(18) 0.2764(9) 0.5345(16) 0.037(5) Uani 1 1 d . . . N3 N 0.9933(14) 0.0621(8) 0.1969(13) 0.023(4) Uani 1 1 d . . . N4 N 0.8640(14) 0.4200(8) 0.1916(13) 0.021(4) Uani 1 1 d . . . N5 N 0.5827(15) 0.1425(8) 0.2374(14) 0.026(4) Uani 1 1 d . . . N6 N 0.5291(17) 0.2066(9) -0.2990(16) 0.035(5) Uani 1 1 d . . . H6 H 0.5410 0.2505 -0.3008 0.043 Uiso 1 1 calc R . . N7 N 0.5571(16) 0.3320(9) -0.3200(14) 0.030(4) Uani 1 1 d . . . C1 C 1.3974(17) 0.3591(11) 0.2500(19) 0.030(5) Uani 1 1 d . . . H1A H 1.4265 0.3225 0.2784 0.037 Uiso 1 1 calc R . . H1B H 1.4070 0.3901 0.3116 0.037 Uiso 1 1 calc R . . C2 C 1.469(2) 0.3899(14) 0.164(2) 0.045(6) Uani 1 1 d . . . H2A H 1.5363 0.3712 0.1628 0.054 Uiso 1 1 calc R . . H2B H 1.4977 0.4360 0.1807 0.054 Uiso 1 1 calc R . . C3 C 1.257(2) 0.2854(10) 0.121(2) 0.035(6) Uani 1 1 d . . . H3A H 1.1766 0.2747 0.0837 0.042 Uiso 1 1 calc R . . H3B H 1.2729 0.2467 0.1556 0.042 Uiso 1 1 calc R . . C4 C 1.340(2) 0.3067(12) 0.036(2) 0.045(6) Uani 1 1 d . . . H4A H 1.4014 0.2834 0.0447 0.054 Uiso 1 1 calc R . . H4B H 1.2970 0.2970 -0.0390 0.054 Uiso 1 1 calc R . . C5 C 1.2351(19) 0.3923(10) 0.1489(18) 0.029(5) Uani 1 1 d U . . H5A H 1.1507 0.3809 0.1264 0.034 Uiso 1 1 calc R . . H5B H 1.2539 0.4297 0.2004 0.034 Uiso 1 1 calc R . . C6 C 1.292(2) 0.4087(14) 0.054(2) 0.053(8) Uani 1 1 d . . . H6A H 1.3194 0.4554 0.0534 0.064 Uiso 1 1 calc R . . H6B H 1.2353 0.3947 -0.0127 0.064 Uiso 1 1 calc R . . C7 C 1.3931(19) 0.3784(12) 0.051(2) 0.038(6) Uani 1 1 d . . . H7 H 1.4381 0.3948 -0.0091 0.045 Uiso 1 1 calc R . . C8 C 1.047(2) 0.2062(10) 0.5437(18) 0.032(5) Uani 1 1 d . . . H8A H 1.1098 0.1845 0.5380 0.039 Uiso 1 1 calc R . . H8B H 0.9841 0.1896 0.4832 0.039 Uiso 1 1 calc R . . C9 C 1.003(3) 0.1929(12) 0.653(2) 0.046(7) Uani 1 1 d . . . H9A H 0.9194 0.1731 0.6399 0.056 Uiso 1 1 calc R . . H9B H 1.0421 0.1625 0.6922 0.056 Uiso 1 1 calc R . . C10 C 1.003(2) 0.3094(11) 0.549(2) 0.036(5) Uani 1 1 d . . . H10A H 0.9353 0.2938 0.4922 0.043 Uiso 1 1 calc R . . H10B H 1.0324 0.3554 0.5396 0.043 Uiso 1 1 calc R . . C11 C 0.965(2) 0.2995(14) 0.662(2) 0.047(7) Uani 1 1 d . . . H11A H 0.9845 0.3406 0.7039 0.056 Uiso 1 1 calc R . . H11B H 0.8804 0.2826 0.6543 0.056 Uiso 1 1 calc R . . C12 C 1.186(2) 0.2974(13) 0.621(2) 0.043(6) Uani 1 1 d . . . H12A H 1.2174 0.3436 0.6156 0.051 Uiso 1 1 calc R . . H12B H 1.2470 0.2756 0.6110 0.051 Uiso 1 1 calc R . . C13 C 1.151(2) 0.2848(14) 0.7327(19) 0.047(7) Uani 1 1 d . . . H13A H 1.1964 0.2569 0.7712 0.057 Uiso 1 1 calc R . . H13B H 1.1674 0.3252 0.7760 0.057 Uiso 1 1 calc R . . C14 C 1.025(3) 0.2533(11) 0.722(2) 0.045(7) Uani 1 1 d . . . H14 H 0.9996 0.2445 0.7957 0.054 Uiso 1 1 calc R . . C15 C 0.883(2) 0.0210(12) 0.227(2) 0.040(6) Uani 1 1 d . . . H15A H 0.8384 0.0488 0.2554 0.048 Uiso 1 1 calc R . . H15B H 0.8361 -0.0012 0.1593 0.048 Uiso 1 1 calc R . . C16 C 0.898(2) -0.0257(13) 0.306(2) 0.046(6) Uani 1 1 d . . . H16A H 0.8620 -0.0690 0.2746 0.056 Uiso 1 1 calc R . . H16B H 0.8621 -0.0190 0.3711 0.056 Uiso 1 1 calc R . . C17 C 1.062(2) 0.0959(12) 0.2965(19) 0.038(6) Uani 1 1 d . . . H17A H 1.0203 0.1260 0.3235 0.046 Uiso 1 1 calc R . . H17B H 1.1362 0.1209 0.2787 0.046 Uiso 1 1 calc R . . C18 C 1.083(2) 0.0507(12) 0.386(2) 0.044(6) Uani 1 1 d . . . H18A H 1.0467 0.0587 0.4499 0.053 Uiso 1 1 calc R . . H18B H 1.1672 0.0574 0.4101 0.053 Uiso 1 1 calc R . . C19 C 1.054(2) 0.0186(12) 0.153(2) 0.038(6) Uani 1 1 d . . . H19A H 1.1250 0.0434 0.1277 0.046 Uiso 1 1 calc R . . H19B H 1.0044 -0.0060 0.0889 0.046 Uiso 1 1 calc R . . C20 C 1.085(2) -0.0274(11) 0.2403(19) 0.033(5) Uani 1 1 d . . . H20A H 1.0559 -0.0718 0.2113 0.039 Uiso 1 1 calc R . . H20B H 1.1698 -0.0191 0.2589 0.039 Uiso 1 1 calc R . . C21 C 1.0326(19) -0.0182(10) 0.3406(19) 0.031(5) Uani 1 1 d . . . H21 H 1.0476 -0.0494 0.3967 0.038 Uiso 1 1 calc R . . C22 C 0.9838(18) 0.4549(11) 0.2326(19) 0.032(5) Uani 1 1 d . . . H22A H 1.0205 0.4769 0.1720 0.038 Uiso 1 1 calc R . . H22B H 1.0293 0.4248 0.2623 0.038 Uiso 1 1 calc R . . C23 C 0.981(2) 0.5048(11) 0.325(2) 0.041(6) Uani 1 1 d . . . H23A H 1.0135 0.4919 0.3967 0.049 Uiso 1 1 calc R . . H23B H 1.0281 0.5471 0.3101 0.049 Uiso 1 1 calc R . . C24 C 0.807(2) 0.3921(10) 0.285(2) 0.033(5) Uani 1 1 d . . . H24A H 0.8547 0.3667 0.3266 0.039 Uiso 1 1 calc R . . H24B H 0.7315 0.3634 0.2565 0.039 Uiso 1 1 calc R . . C25 C 0.789(2) 0.4434(12) 0.358(2) 0.043(6) Uani 1 1 d . . . H25A H 0.8157 0.4359 0.4354 0.051 Uiso 1 1 calc R . . H25B H 0.7064 0.4430 0.3511 0.051 Uiso 1 1 calc R . . C26 C 0.8033(19) 0.4643(10) 0.1352(18) 0.028(5) Uani 1 1 d . . . H26A H 0.7224 0.4422 0.1092 0.034 Uiso 1 1 calc R . . H26B H 0.8404 0.4805 0.0709 0.034 Uiso 1 1 calc R . . C27 C 0.807(2) 0.5203(10) 0.215(2) 0.035(5) Uani 1 1 d . . . H27A H 0.8538 0.5599 0.1893 0.042 Uiso 1 1 calc R . . H27B H 0.7281 0.5257 0.2160 0.042 Uiso 1 1 calc R . . C28 C 0.858(2) 0.5078(10) 0.326(2) 0.035(6) Uani 1 1 d . . . H28 H 0.8541 0.5421 0.3789 0.042 Uiso 1 1 calc R . . C29 C 0.538(3) 0.1863(15) 0.157(3) 0.062(8) Uani 1 1 d . . . H29A H 0.5899 0.1964 0.1002 0.075 Uiso 1 1 calc R . . H29B H 0.5388 0.2265 0.1952 0.075 Uiso 1 1 calc R . . C30 C 0.415(3) 0.1555(14) 0.101(3) 0.063(9) Uani 1 1 d . . . H30A H 0.4108 0.1567 0.0206 0.076 Uiso 1 1 calc R . . H30B H 0.3600 0.1788 0.1239 0.076 Uiso 1 1 calc R . . C31 C 0.596(2) 0.0865(11) 0.174(2) 0.035(5) Uani 1 1 d . . . H31A H 0.6229 0.0561 0.2241 0.042 Uiso 1 1 calc R . . H31B H 0.6539 0.1005 0.1239 0.042 Uiso 1 1 calc R . . C32 C 0.479(2) 0.0537(12) 0.107(2) 0.042(6) Uani 1 1 d . . . H32A H 0.4834 0.0584 0.0276 0.050 Uiso 1 1 calc R . . H32B H 0.4602 0.0078 0.1206 0.050 Uiso 1 1 calc R . . C33 C 0.493(2) 0.1300(12) 0.3205(19) 0.041(6) Uani 1 1 d U . . H33A H 0.5241 0.1115 0.3876 0.049 Uiso 1 1 calc R . . H33B H 0.4733 0.1699 0.3408 0.049 Uiso 1 1 calc R . . C34 C 0.389(3) 0.0834(14) 0.260(2) 0.054(7) Uani 1 1 d . . . H34A H 0.3894 0.0401 0.2842 0.065 Uiso 1 1 calc R . . H34B H 0.3183 0.0938 0.2796 0.065 Uiso 1 1 calc R . . C35 C 0.382(2) 0.0832(13) 0.137(2) 0.046(7) Uani 1 1 d . . . H35 H 0.3048 0.0597 0.1004 0.055 Uiso 1 1 calc R . . C36 C 0.454(2) 0.1762(13) -0.401(2) 0.052(7) Uani 1 1 d . . . H36A H 0.4943 0.1878 -0.4652 0.063 Uiso 1 1 calc R . . H36B H 0.3824 0.1918 -0.4118 0.063 Uiso 1 1 calc R . . C37 C 0.423(3) 0.1035(14) -0.393(3) 0.070(9) Uani 1 1 d . . . H37A H 0.3400 0.0885 -0.3870 0.084 Uiso 1 1 calc R . . H37B H 0.4384 0.0833 -0.4592 0.084 Uiso 1 1 calc R . . C38 C 0.642(2) 0.1886(14) -0.291(2) 0.048(7) Uani 1 1 d . . . H38A H 0.6881 0.2033 -0.2191 0.058 Uiso 1 1 calc R . . H38B H 0.6851 0.2086 -0.3490 0.058 Uiso 1 1 calc R . . C39 C 0.616(3) 0.1129(14) -0.304(3) 0.061(8) Uani 1 1 d . . . H39A H 0.6356 0.1006 -0.3754 0.074 Uiso 1 1 calc R . . H39B H 0.6635 0.0962 -0.2453 0.074 Uiso 1 1 calc R . . C40 C 0.470(3) 0.1836(13) -0.207(2) 0.053(7) Uani 1 1 d . . . H40A H 0.3912 0.1909 -0.2184 0.064 Uiso 1 1 calc R . . H40B H 0.5118 0.2069 -0.1389 0.064 Uiso 1 1 calc R . . C41 C 0.463(3) 0.1121(13) -0.197(2) 0.062(9) Uani 1 1 d . . . H41A H 0.5191 0.1055 -0.1347 0.074 Uiso 1 1 calc R . . H41B H 0.3852 0.0898 -0.1837 0.074 Uiso 1 1 calc R . . C42 C 0.489(3) 0.0856(14) -0.299(3) 0.066(9) Uani 1 1 d . . . H42 H 0.4730 0.0382 -0.2969 0.079 Uiso 1 1 calc R . . C43 C 0.5162(19) 0.3498(11) -0.4341(17) 0.030(5) Uani 1 1 d . . . H43A H 0.4326 0.3310 -0.4532 0.036 Uiso 1 1 calc R . . H43B H 0.5567 0.3328 -0.4874 0.036 Uiso 1 1 calc R . . C44 C 0.540(2) 0.4221(12) -0.439(2) 0.040(6) Uani 1 1 d . . . H44A H 0.4697 0.4345 -0.4727 0.048 Uiso 1 1 calc R . . H44B H 0.6013 0.4375 -0.4853 0.048 Uiso 1 1 calc R . . C45 C 0.6833(19) 0.3642(11) -0.290(2) 0.033(5) Uani 1 1 d . . . H45A H 0.7275 0.3549 -0.3471 0.040 Uiso 1 1 calc R . . H45B H 0.7143 0.3484 -0.2198 0.040 Uiso 1 1 calc R . . C46 C 0.694(2) 0.4360(11) -0.278(2) 0.047(7) Uani 1 1 d . . . H46A H 0.7548 0.4587 -0.3199 0.056 Uiso 1 1 calc R . . H46B H 0.7169 0.4502 -0.2006 0.056 Uiso 1 1 calc R . . C47 C 0.489(2) 0.3515(11) -0.241(2) 0.036(5) Uani 1 1 d . . . H47A H 0.5232 0.3453 -0.1652 0.043 Uiso 1 1 calc R . . H47B H 0.4092 0.3250 -0.2532 0.043 Uiso 1 1 calc R . . C48 C 0.488(3) 0.4211(15) -0.254(3) 0.061(8) Uani 1 1 d . . . H48A H 0.4113 0.4243 -0.2904 0.073 Uiso 1 1 calc R . . H48B H 0.5026 0.4432 -0.1815 0.073 Uiso 1 1 calc R . . C49 C 0.579(2) 0.4524(12) -0.322(2) 0.039(6) Uani 1 1 d . . . H49 H 0.5874 0.4994 -0.3218 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0214(7) 0.0214(7) 0.0246(8) -0.0005(6) 0.0012(6) 0.0070(6) In2 0.0218(8) 0.0219(8) 0.0374(9) -0.0005(6) -0.0032(6) 0.0063(6) In3 0.0255(8) 0.0234(8) 0.0269(8) -0.0028(6) 0.0001(6) 0.0075(6) In4 0.0225(8) 0.0239(8) 0.0239(8) 0.0001(6) 0.0017(6) 0.0075(6) In5 0.0262(8) 0.0298(9) 0.0416(10) 0.0042(7) 0.0105(7) 0.0044(7) Cl1 0.035(3) 0.029(3) 0.031(3) -0.005(2) 0.006(2) 0.002(2) Cl2 0.029(3) 0.031(3) 0.038(3) 0.003(2) -0.004(2) 0.014(2) Cl3 0.032(3) 0.030(3) 0.036(3) 0.000(2) 0.007(2) 0.004(2) Cl4 0.030(3) 0.047(4) 0.036(3) -0.012(3) -0.004(2) 0.005(3) Cl5 0.025(3) 0.044(3) 0.033(3) 0.000(2) -0.005(2) 0.008(2) Cl6 0.041(3) 0.042(3) 0.037(3) 0.007(3) 0.016(3) 0.007(3) Cl7 0.036(3) 0.038(3) 0.049(4) 0.000(3) 0.017(3) 0.007(3) Cl8 0.041(3) 0.047(4) 0.044(4) 0.012(3) 0.005(3) 0.005(3) N1 0.018(9) 0.044(11) 0.034(10) -0.011(9) 0.000(8) 0.021(8) N2 0.045(12) 0.025(10) 0.038(11) -0.005(8) 0.005(9) 0.007(9) N3 0.025(9) 0.028(9) 0.019(9) -0.002(7) 0.001(7) 0.013(8) N4 0.020(9) 0.022(9) 0.024(9) 0.005(7) 0.001(7) 0.009(7) N5 0.029(10) 0.025(9) 0.029(10) -0.001(7) 0.005(8) 0.015(8) N6 0.043(12) 0.029(10) 0.039(11) 0.010(9) 0.006(9) 0.016(9) N7 0.033(10) 0.036(11) 0.023(10) 0.009(8) -0.004(8) 0.015(9) C1 0.014(10) 0.038(13) 0.042(13) 0.006(10) 0.002(9) 0.011(9) C2 0.024(12) 0.057(17) 0.059(17) 0.001(13) 0.011(12) 0.015(12) C3 0.034(13) 0.018(11) 0.055(15) -0.014(10) 0.001(11) 0.013(10) C4 0.063(18) 0.041(15) 0.035(14) 0.004(11) 0.003(13) 0.021(13) C5 0.031(7) 0.025(7) 0.034(7) 0.005(6) 0.007(6) 0.013(6) C6 0.052(17) 0.066(19) 0.051(17) -0.029(14) -0.014(13) 0.046(15) C7 0.019(11) 0.051(15) 0.050(15) 0.014(12) 0.018(11) 0.014(11) C8 0.053(15) 0.018(11) 0.026(12) 0.007(9) 0.004(11) 0.011(10) C9 0.071(19) 0.033(14) 0.030(13) -0.003(11) 0.023(13) -0.006(13) C10 0.034(13) 0.035(13) 0.038(14) 0.008(10) 0.006(11) 0.004(10) C11 0.039(15) 0.071(19) 0.037(14) 0.006(13) 0.006(12) 0.025(14) C12 0.041(15) 0.052(16) 0.038(14) -0.004(12) 0.005(11) 0.018(13) C13 0.057(17) 0.062(18) 0.022(12) -0.012(12) -0.004(11) 0.019(14) C14 0.08(2) 0.026(13) 0.025(13) -0.005(10) 0.010(13) 0.007(13) C15 0.024(12) 0.040(14) 0.055(16) 0.013(12) 0.008(11) 0.006(11) C16 0.040(15) 0.046(16) 0.056(17) 0.004(13) 0.018(13) 0.011(12) C17 0.038(14) 0.049(15) 0.029(13) -0.004(11) -0.004(10) 0.017(12) C18 0.058(17) 0.044(15) 0.029(13) -0.001(11) 0.004(12) 0.013(13) C19 0.044(14) 0.043(14) 0.042(14) 0.017(11) 0.026(12) 0.028(12) C20 0.031(12) 0.029(12) 0.042(14) -0.001(10) -0.003(10) 0.020(10) C21 0.028(12) 0.023(11) 0.042(13) 0.011(10) 0.017(10) -0.003(9) C22 0.015(10) 0.040(13) 0.037(13) -0.005(10) -0.004(9) 0.003(9) C23 0.045(15) 0.027(13) 0.045(15) -0.014(11) -0.013(12) 0.010(11) C24 0.041(13) 0.013(10) 0.049(14) 0.012(10) 0.016(11) 0.011(9) C25 0.051(16) 0.041(14) 0.039(14) 0.005(11) 0.027(12) 0.003(12) C26 0.030(12) 0.030(12) 0.030(12) 0.000(9) 0.001(9) 0.018(10) C27 0.037(13) 0.024(12) 0.052(15) 0.006(10) 0.015(11) 0.019(10) C28 0.033(13) 0.024(12) 0.047(14) -0.020(10) 0.002(11) 0.009(10) C29 0.08(2) 0.055(19) 0.06(2) 0.008(15) 0.008(17) 0.033(17) C30 0.051(18) 0.055(18) 0.09(2) -0.027(17) -0.002(16) 0.036(15) C31 0.032(13) 0.033(13) 0.042(14) -0.003(10) 0.008(11) 0.011(10) C32 0.045(15) 0.030(13) 0.051(16) 0.003(11) 0.004(12) 0.011(11) C33 0.040(8) 0.041(8) 0.032(8) 0.012(6) 0.007(6) -0.009(6) C34 0.054(18) 0.052(17) 0.050(17) -0.013(14) 0.002(14) 0.005(14) C35 0.028(13) 0.049(16) 0.067(18) 0.017(14) 0.012(12) 0.021(12) C36 0.043(16) 0.051(17) 0.054(17) 0.006(13) -0.011(13) 0.004(13) C37 0.07(2) 0.040(17) 0.09(3) 0.011(16) 0.013(19) -0.005(16) C38 0.054(17) 0.066(19) 0.036(14) 0.019(13) 0.007(12) 0.035(15) C39 0.09(2) 0.057(19) 0.056(19) 0.010(15) 0.023(17) 0.042(18) C40 0.08(2) 0.040(15) 0.036(15) -0.002(12) 0.010(14) -0.002(14) C41 0.11(3) 0.050(17) 0.031(15) 0.018(13) 0.036(16) 0.010(17) C42 0.12(3) 0.030(15) 0.057(19) 0.010(13) 0.018(19) 0.022(17) C43 0.028(12) 0.041(13) 0.018(11) 0.001(9) -0.008(9) 0.006(10) C44 0.032(13) 0.042(14) 0.044(15) 0.002(11) 0.011(11) 0.000(11) C45 0.026(12) 0.033(13) 0.037(13) -0.007(10) -0.008(10) 0.007(10) C46 0.038(14) 0.030(13) 0.064(18) 0.014(12) -0.013(13) 0.003(11) C47 0.029(12) 0.032(13) 0.047(15) -0.003(11) 0.009(11) 0.005(10) C48 0.07(2) 0.06(2) 0.055(18) -0.002(15) 0.030(16) 0.016(16) C49 0.040(14) 0.035(13) 0.039(14) -0.008(11) -0.001(11) 0.007(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 In4 2.749(2) . ? In1 In3 2.752(2) . ? In1 In5 2.763(2) . ? In1 In2 2.776(2) . ? In2 Cl1 2.461(6) . ? In2 N1 2.461(19) . ? In2 Cl2 2.463(5) . ? In2 N2 2.54(2) . ? In3 N3 2.325(17) . ? In3 Cl4 2.424(6) . ? In3 Cl3 2.431(6) . ? In4 N4 2.330(17) . ? In4 Cl6 2.421(6) . ? In4 Cl5 2.449(5) . ? In5 N5 2.284(18) . ? In5 Cl7 2.455(6) . ? In5 Cl8 2.465(6) . ? N1 C3 1.50(3) . ? N1 C1 1.50(3) . ? N1 C5 1.53(3) . ? N2 C12 1.44(3) . ? N2 C10 1.45(3) . ? N2 C8 1.50(3) . ? N3 C19 1.47(3) . ? N3 C17 1.47(3) . ? N3 C15 1.51(3) . ? N4 C26 1.47(2) . ? N4 C24 1.48(3) . ? N4 C22 1.48(3) . ? N5 C31 1.50(3) . ? N5 C29 1.51(3) . ? N5 C33 1.57(3) . ? N6 C40 1.45(3) . ? N6 C38 1.49(3) . ? N6 C36 1.50(3) . ? N7 C47 1.48(3) . ? N7 C45 1.51(3) . ? N7 C43 1.51(3) . ? C1 C2 1.52(3) . ? C2 C7 1.54(4) . ? C3 C4 1.55(4) . ? C4 C7 1.54(4) . ? C5 C6 1.44(4) . ? C6 C7 1.52(3) . ? C8 C9 1.52(3) . ? C9 C14 1.51(3) . ? C10 C11 1.53(3) . ? C11 C14 1.52(4) . ? C12 C13 1.51(3) . ? C13 C14 1.50(4) . ? C15 C16 1.44(3) . ? C16 C21 1.59(3) . ? C17 C18 1.52(3) . ? C18 C21 1.55(3) . ? C19 C20 1.55(3) . ? C20 C21 1.50(3) . ? C22 C23 1.58(3) . ? C23 C28 1.51(3) . ? C24 C25 1.51(3) . ? C25 C28 1.53(3) . ? C26 C27 1.54(3) . ? C27 C28 1.48(3) . ? C29 C30 1.55(4) . ? C30 C35 1.61(4) . ? C31 C32 1.55(3) . ? C32 C35 1.54(3) . ? C33 C34 1.52(3) . ? C34 C35 1.50(4) . ? C36 C37 1.54(4) . ? C37 C42 1.42(4) . ? C38 C39 1.60(4) . ? C39 C42 1.52(5) . ? C40 C41 1.54(4) . ? C41 C42 1.48(4) . ? C43 C44 1.53(3) . ? C44 C49 1.56(3) . ? C45 C46 1.54(3) . ? C46 C49 1.54(3) . ? C47 C48 1.52(4) . ? C48 C49 1.51(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag In4 In1 In3 110.93(7) . . ? In4 In1 In5 104.77(7) . . ? In3 In1 In5 103.21(7) . . ? In4 In1 In2 111.45(7) . . ? In3 In1 In2 112.61(7) . . ? In5 In1 In2 113.33(7) . . ? Cl1 In2 N1 83.5(4) . . ? Cl1 In2 Cl2 111.5(2) . . ? N1 In2 Cl2 83.6(4) . . ? Cl1 In2 N2 82.0(4) . . ? N1 In2 N2 157.3(6) . . ? Cl2 In2 N2 85.7(5) . . ? Cl1 In2 In1 129.84(15) . . ? N1 In2 In1 99.7(4) . . ? Cl2 In2 In1 118.60(15) . . ? N2 In2 In1 103.0(5) . . ? N3 In3 Cl4 97.1(5) . . ? N3 In3 Cl3 97.6(4) . . ? Cl4 In3 Cl3 102.6(2) . . ? N3 In3 In1 109.0(4) . . ? Cl4 In3 In1 119.95(16) . . ? Cl3 In3 In1 125.05(15) . . ? N4 In4 Cl6 96.5(4) . . ? N4 In4 Cl5 94.3(4) . . ? Cl6 In4 Cl5 99.8(2) . . ? N4 In4 In1 109.0(4) . . ? Cl6 In4 In1 129.46(16) . . ? Cl5 In4 In1 120.11(15) . . ? N5 In5 Cl7 93.5(4) . . ? N5 In5 Cl8 90.7(5) . . ? Cl7 In5 Cl8 101.9(2) . . ? N5 In5 In1 123.6(4) . . ? Cl7 In5 In1 119.54(16) . . ? Cl8 In5 In1 120.97(17) . . ? C3 N1 C1 108.6(16) . . ? C3 N1 C5 106.5(17) . . ? C1 N1 C5 107.0(17) . . ? C3 N1 In2 109.0(14) . . ? C1 N1 In2 115.1(13) . . ? C5 N1 In2 110.2(11) . . ? C12 N2 C10 108.4(19) . . ? C12 N2 C8 107.4(19) . . ? C10 N2 C8 110.7(19) . . ? C12 N2 In2 113.5(15) . . ? C10 N2 In2 108.3(14) . . ? C8 N2 In2 108.7(13) . . ? C19 N3 C17 110.6(18) . . ? C19 N3 C15 106.2(18) . . ? C17 N3 C15 108.6(18) . . ? C19 N3 In3 115.3(13) . . ? C17 N3 In3 104.2(13) . . ? C15 N3 In3 111.9(12) . . ? C26 N4 C24 111.2(16) . . ? C26 N4 C22 108.5(17) . . ? C24 N4 C22 109.4(17) . . ? C26 N4 In4 113.3(12) . . ? C24 N4 In4 105.3(12) . . ? C22 N4 In4 109.0(12) . . ? C31 N5 C29 107.5(19) . . ? C31 N5 C33 117.5(18) . . ? C29 N5 C33 104.0(19) . . ? C31 N5 In5 107.0(13) . . ? C29 N5 In5 108.9(16) . . ? C33 N5 In5 111.5(13) . . ? C40 N6 C38 111(2) . . ? C40 N6 C36 107(2) . . ? C38 N6 C36 109(2) . . ? C47 N7 C45 110.2(17) . . ? C47 N7 C43 110.3(17) . . ? C45 N7 C43 109.0(17) . . ? N1 C1 C2 112.9(19) . . ? C1 C2 C7 108.7(19) . . ? N1 C3 C4 110.8(19) . . ? C7 C4 C3 109.7(19) . . ? C6 C5 N1 111.6(18) . . ? C5 C6 C7 113(2) . . ? C6 C7 C4 105(2) . . ? C6 C7 C2 109(2) . . ? C4 C7 C2 107(2) . . ? N2 C8 C9 109.7(18) . . ? C14 C9 C8 111(2) . . ? N2 C10 C11 111.6(19) . . ? C14 C11 C10 110(2) . . ? N2 C12 C13 113(2) . . ? C14 C13 C12 110(2) . . ? C13 C14 C9 108(2) . . ? C13 C14 C11 105(2) . . ? C9 C14 C11 109(2) . . ? C16 C15 N3 115(2) . . ? C15 C16 C21 108(2) . . ? N3 C17 C18 112(2) . . ? C17 C18 C21 109(2) . . ? N3 C19 C20 110.8(18) . . ? C21 C20 C19 109.5(17) . . ? C20 C21 C18 108.4(18) . . ? C20 C21 C16 109(2) . . ? C18 C21 C16 107(2) . . ? N4 C22 C23 108.9(18) . . ? C28 C23 C22 108.3(18) . . ? N4 C24 C25 110.8(17) . . ? C24 C25 C28 108.8(18) . . ? N4 C26 C27 109.3(17) . . ? C28 C27 C26 109.9(17) . . ? C27 C28 C23 109(2) . . ? C27 C28 C25 108(2) . . ? C23 C28 C25 109(2) . . ? N5 C29 C30 111(3) . . ? C29 C30 C35 108(2) . . ? N5 C31 C32 109.4(18) . . ? C35 C32 C31 111(2) . . ? C34 C33 N5 105(2) . . ? C35 C34 C33 114(2) . . ? C34 C35 C32 108(2) . . ? C34 C35 C30 108(2) . . ? C32 C35 C30 105(2) . . ? N6 C36 C37 110(2) . . ? C42 C37 C36 110(3) . . ? N6 C38 C39 108(2) . . ? C42 C39 C38 108(2) . . ? N6 C40 C41 109(2) . . ? C42 C41 C40 110(2) . . ? C37 C42 C41 111(3) . . ? C37 C42 C39 109(3) . . ? C41 C42 C39 107(3) . . ? N7 C43 C44 109.6(18) . . ? C43 C44 C49 109(2) . . ? N7 C45 C46 108.0(18) . . ? C45 C46 C49 111(2) . . ? N7 C47 C48 109(2) . . ? C49 C48 C47 110(2) . . ? C48 C49 C46 110(2) . . ? C48 C49 C44 107(2) . . ? C46 C49 C44 107(2) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 5.152 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.349 # Attachment 'cmpd3.CIF' data_ccompound3 _database_code_depnum_ccdc_archive 'CCDC 699633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 Br In N2' _chemical_formula_weight 310.94 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' Br Br -0.2901 2.4595 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3609(15) _cell_length_b 14.693(3) _cell_length_c 10.264(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.82(3) _cell_angle_gamma 90.00 _cell_volume 1073.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue-violet _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 5.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.280 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 3510 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1869 _reflns_number_gt 1523 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The methylene groups of the tmeda ligand were found to be disordered over two sites. This disorder was successfully modelled. ; _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^)+(0.0498P)^2^+0.8613P] 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 1869 _refine_ls_number_parameters 114 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.12504(5) 0.56918(3) 0.14447(4) 0.03762(17) Uani 1 1 d . A . Br1 Br 0.20224(9) 0.41370(4) 0.29932(6) 0.0461(2) Uani 1 1 d . . . N1 N 0.1869(6) 0.6609(3) 0.3601(4) 0.0398(11) Uani 1 1 d D . . N2 N -0.1842(7) 0.5904(3) 0.1994(5) 0.0448(12) Uani 1 1 d D . . C3 C 0.3387(10) 0.6258(5) 0.4678(6) 0.0598(18) Uani 1 1 d . A . H3A H 0.4548 0.6242 0.4378 0.090 Uiso 1 1 calc R . . H3B H 0.3074 0.5642 0.4914 0.090 Uiso 1 1 calc R . . H3C H 0.3563 0.6654 0.5469 0.090 Uiso 1 1 calc R . . C4 C 0.2374(11) 0.7516(4) 0.3260(6) 0.0627(19) Uani 1 1 d . A . H4A H 0.2556 0.7911 0.4053 0.094 Uiso 1 1 calc R . . H4B H 0.1366 0.7763 0.2529 0.094 Uiso 1 1 calc R . . H4C H 0.3542 0.7488 0.2970 0.094 Uiso 1 1 calc R . . C5 C -0.2766(9) 0.5039(5) 0.2093(7) 0.0600(18) Uani 1 1 d . A . H5A H -0.1974 0.4674 0.2819 0.090 Uiso 1 1 calc R . . H5B H -0.2964 0.4709 0.1238 0.090 Uiso 1 1 calc R . . H5C H -0.3981 0.5152 0.2290 0.090 Uiso 1 1 calc R . . C6 C -0.3062(9) 0.6437(5) 0.0907(8) 0.0656(19) Uani 1 1 d . A . H6A H -0.3261 0.6103 0.0056 0.098 Uiso 1 1 calc R . . H6B H -0.2465 0.7023 0.0826 0.098 Uiso 1 1 calc R . . H6C H -0.4274 0.6541 0.1113 0.098 Uiso 1 1 calc R . . C2 C -0.134(2) 0.6088(13) 0.3491(14) 0.038(5) Uani 0.41(2) 1 d PD A 1 H2A H -0.2481 0.6229 0.3791 0.046 Uiso 0.41(2) 1 calc PR A 1 H2B H -0.0723 0.5548 0.3992 0.046 Uiso 0.41(2) 1 calc PR A 1 C1 C -0.001(2) 0.6888(12) 0.375(2) 0.046(5) Uani 0.41(2) 1 d PD A 1 H1A H -0.0523 0.7384 0.3111 0.055 Uiso 0.41(2) 1 calc PR A 1 H1B H 0.0110 0.7120 0.4678 0.055 Uiso 0.41(2) 1 calc PR A 1 C2A C -0.1607(15) 0.6590(11) 0.3112(12) 0.046(4) Uani 0.59(2) 1 d PD A 2 H2A1 H -0.1633 0.7212 0.2737 0.055 Uiso 0.59(2) 1 calc PR A 2 H2A2 H -0.2661 0.6534 0.3544 0.055 Uiso 0.59(2) 1 calc PR A 2 C1A C 0.0219(14) 0.6440(12) 0.4144(11) 0.042(3) Uani 0.59(2) 1 d PD A 2 H1A1 H 0.0281 0.6850 0.4920 0.050 Uiso 0.59(2) 1 calc PR A 2 H1A2 H 0.0266 0.5806 0.4476 0.050 Uiso 0.59(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0437(3) 0.0418(3) 0.0290(2) 0.00026(16) 0.01230(18) 0.00030(17) Br1 0.0525(4) 0.0376(3) 0.0444(4) 0.0018(2) 0.0054(3) 0.0014(3) N1 0.043(3) 0.045(3) 0.031(3) -0.005(2) 0.009(2) -0.003(2) N2 0.043(3) 0.052(3) 0.039(3) -0.008(2) 0.010(2) 0.000(2) C3 0.088(5) 0.052(4) 0.035(4) 0.003(3) 0.007(3) 0.008(4) C4 0.098(5) 0.041(4) 0.043(4) 0.004(3) 0.007(4) 0.006(4) C5 0.053(4) 0.068(5) 0.062(5) 0.024(4) 0.019(3) 0.002(3) C6 0.052(4) 0.055(4) 0.091(6) 0.023(4) 0.021(4) 0.006(3) C2 0.049(10) 0.041(10) 0.028(9) 0.002(7) 0.017(7) 0.005(9) C1 0.050(11) 0.043(11) 0.047(12) 0.013(9) 0.014(9) 0.003(9) C2A 0.047(7) 0.053(9) 0.040(7) -0.007(6) 0.015(5) 0.003(6) C1A 0.046(7) 0.054(9) 0.032(7) -0.007(6) 0.021(5) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 N2 2.500(5) . ? In1 N1 2.531(4) . ? In1 Br1 2.7579(8) . ? N1 C4 1.450(7) . ? N1 C3 1.451(7) . ? N1 C1A 1.482(10) . ? N1 C1 1.491(14) . ? N2 C5 1.457(8) . ? N2 C6 1.467(8) . ? N2 C2A 1.505(11) . ? N2 C2 1.511(13) . ? C2 C1 1.506(17) . ? C2A C1A 1.500(14) . ? 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 N2 In1 N1 72.98(14) . . ? N2 In1 Br1 92.21(12) . . ? N1 In1 Br1 88.44(11) . . ? C4 N1 C3 108.4(5) . . ? C4 N1 C1A 122.0(8) . . ? C3 N1 C1A 101.5(6) . . ? C4 N1 C1 94.3(8) . . ? C3 N1 C1 124.9(10) . . ? C1A N1 C1 29.9(6) . . ? C4 N1 In1 106.2(3) . . ? C3 N1 In1 114.1(4) . . ? C1A N1 In1 105.0(5) . . ? C1 N1 In1 105.9(8) . . ? C5 N2 C6 108.3(5) . . ? C5 N2 C2A 119.7(7) . . ? C6 N2 C2A 98.7(7) . . ? C5 N2 C2 94.8(7) . . ? C6 N2 C2 128.4(10) . . ? C2A N2 C2 32.1(6) . . ? C5 N2 In1 112.0(4) . . ? C6 N2 In1 108.1(4) . . ? C2A N2 In1 108.8(5) . . ? C2 N2 In1 104.5(7) . . ? C1 C2 N2 107.6(14) . . ? N1 C1 C2 110.0(14) . . ? C1A C2A N2 110.4(10) . . ? N1 C1A C2A 112.5(10) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.796 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.123