# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_publ_section _journal_name_full 'Dalton Trans.' #TrackingRef 'Dalton-Transaction---data[1].cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ingo-Peter Lorenz' _publ_contact_author_address ; Department Chemie und Biochemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; _publ_contact_author_email ipl@cup.uni-muenchen.de _publ_contact_author_phone 'Int+ 089-2180-77486' _publ_contact_author_fax 'Int+ 089-2180-77867' loop_ _publ_author_name _publ_author_address R.Bobka ; Department Chemie und Biochemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; N.J.Roedel ; Department Chemie und Biochemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; S.Wirth ; Department Chemie und Biochemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; I.-P.Lorenz ; Department Chemie und Biochemie Ludwig-Maximilians Universitaet Butenandtstrasse 5-13 (Haus D) D-81377 Muenchen Bundesrepublik Deutschland ; _publ_section_title ; Reactions of Cu(I)Br with aziridine derivatives. Synthesis, characterizastion and crystal structure of monomeric, dimeric and hexameric aziridine (= az) complexes of the formal type [CuBr(az)2)n (n = 1,2) and [CuBr(az)]6 ; _publ_section_abstract ? _publ_section_comment ? data_5_(CCDC-771766) _database_code_depnum_ccdc_archive 'CCDC 771766' #TrackingRef 'Dalton-Transaction---data[1].cif' _audit_author_name 'S. Wirth, P. Mayer' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 08-Feb-06 _chemical_name_systematic Bis[?2-bromo-bis(2-phenylaziridine)copper(I)] _chemical_name_common Bis(?2-bromo-bis(2-phenylaziridine)copper(i)) _chemical_formula_moiety 'C32 H36 Br2 Cu2 N4' _chemical_formula_sum 'C32 H36 Br2 Cu2 N4' _chemical_compound_source ? _chemical_properties_physical 'air-sensitive, oxygen-sensitive' _exptl_crystal_recrystallization_method 'slow isothermic diffusion of n-pentane into a solution in dichloromethane' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 200(2) _chemical_formula_weight 763.555 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' Cu Cu 0.3201 1.2651 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6189(3) _cell_length_b 10.3653(3) _cell_length_c 16.4816(5) _cell_angle_alpha 79.4170(10) _cell_angle_beta 73.3740(10) _cell_angle_gamma 89.2180(10) _cell_volume 1546.46(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5765 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 26.022 _cell_special_details ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.63979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 3.987 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.48282 _exptl_absorpt_correction_T_max 0.74504 _exptl_absorpt_process_details ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ABSTomba Analytical Absorption Correction following the de Meulenaer & Tompa algorithm (see. N.W. Alcock (1970). Crystallographic Computing, p 271) ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.070000 -1 0 0 0.090000 0 0 1 0.040000 0 0 -1 0.040000 3 3 2 0.050000 -3 -3 -2 0.050000 -5 6 -1 0.120000 5 -6 1 0.120000 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type ? _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle omega-scan _kl_diffrn_measurement_scan_step_degree 1.90 _kl_diffrn_measurement_scan_time_per_degree 10 _kl_diffrn_measurement_detector_distance 30 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22371 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 26.05 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.021 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.089 _reflns_number_total 6017 _reflns_number_gt 4849 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0332P)^2^+2.4687P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6017 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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. ; 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 Br1 Br 0.24793(4) 0.42281(4) 0.48974(3) 0.03904(12) Uani 1 1 d . . . Br2 Br 0.24740(4) -0.01441(4) 0.49939(3) 0.04104(12) Uani 1 1 d . . . Cu1 Cu 0.26013(5) 0.23697(5) 0.40567(3) 0.04178(14) Uani 1 1 d . . . Cu2 Cu 0.23607(5) 0.19473(5) 0.58331(3) 0.04147(14) Uani 1 1 d . . . N1 N 0.0657(3) 0.2332(3) 0.3862(2) 0.0364(7) Uani 1 1 d . . . H1A H 0.0176 0.1518 0.4096 0.044 Uiso 1 1 calc R . . C1 C 0.0235(4) 0.2996(4) 0.3082(3) 0.0420(9) Uani 1 1 d . . . H1B H -0.0457 0.2478 0.2903 0.050 Uiso 1 1 calc R . . C2 C -0.0365(4) 0.3416(4) 0.3932(3) 0.0472(10) Uani 1 1 d . . . H2A H -0.0005 0.4270 0.3998 0.057 Uiso 1 1 calc R . . H2B H -0.1398 0.3187 0.4246 0.057 Uiso 1 1 calc R . . C3 C 0.1369(4) 0.3799(4) 0.2368(3) 0.0384(9) Uani 1 1 d . . . C4 C 0.2338(4) 0.4651(4) 0.2512(3) 0.0427(9) Uani 1 1 d . . . H4 H 0.2293 0.4718 0.3086 0.051 Uiso 1 1 calc R . . C5 C 0.3367(5) 0.5403(5) 0.1828(3) 0.0560(12) Uani 1 1 d . . . H5 H 0.4025 0.5980 0.1935 0.067 Uiso 1 1 calc R . . C6 C 0.3437(6) 0.5315(5) 0.0985(3) 0.0648(14) Uani 1 1 d . . . H6 H 0.4140 0.5832 0.0514 0.078 Uiso 1 1 calc R . . C7 C 0.2479(7) 0.4472(5) 0.0840(3) 0.0678(14) Uani 1 1 d . . . H7 H 0.2527 0.4405 0.0265 0.081 Uiso 1 1 calc R . . C8 C 0.1451(6) 0.3723(5) 0.1518(3) 0.0538(11) Uani 1 1 d . . . H8 H 0.0793 0.3151 0.1406 0.065 Uiso 1 1 calc R . . N2 N 0.4709(4) 0.2214(4) 0.3517(3) 0.0579(10) Uani 1 1 d . . . H2 H 0.4930 0.1333 0.3553 0.069 Uiso 1 1 calc R . . C9 C 0.5793(5) 0.3006(5) 0.2814(3) 0.0543(11) Uani 1 1 d . . . H9 H 0.5440 0.3845 0.2550 0.065 Uiso 1 1 calc R . . C10 C 0.5863(5) 0.2956(6) 0.3677(3) 0.0629(14) Uani 1 1 d . . . H10A H 0.5592 0.3746 0.3937 0.075 Uiso 1 1 calc R . . H10B H 0.6647 0.2456 0.3853 0.075 Uiso 1 1 calc R . . C11 C 0.6868(4) 0.2320(5) 0.2179(3) 0.0505(11) Uani 1 1 d . . . C12 C 0.7543(5) 0.1183(5) 0.2384(3) 0.0575(12) Uani 1 1 d . . . H12 H 0.7344 0.0754 0.2969 0.069 Uiso 1 1 calc R . . C13 C 0.8516(6) 0.0655(5) 0.1742(4) 0.0673(15) Uani 1 1 d . . . H13 H 0.8971 -0.0140 0.1884 0.081 Uiso 1 1 calc R . . C14 C 0.8821(5) 0.1299(6) 0.0887(4) 0.0674(15) Uani 1 1 d . . . H14 H 0.9499 0.0958 0.0442 0.081 Uiso 1 1 calc R . . C15 C 0.8136(6) 0.2419(6) 0.0697(3) 0.0655(14) Uani 1 1 d . . . H15 H 0.8328 0.2857 0.0115 0.079 Uiso 1 1 calc R . . C16 C 0.7180(5) 0.2920(5) 0.1331(3) 0.0559(12) Uani 1 1 d . . . H16 H 0.6715 0.3707 0.1183 0.067 Uiso 1 1 calc R . . N3 N 0.4301(3) 0.1775(3) 0.6021(2) 0.0365(7) Uani 1 1 d . . . H3 H 0.4766 0.1056 0.5818 0.044 Uiso 1 1 calc R . . C17 C 0.4771(4) 0.2070(4) 0.6759(3) 0.0423(9) Uani 1 1 d . . . H17 H 0.5469 0.1448 0.6949 0.051 Uiso 1 1 calc R . . C18 C 0.5340(4) 0.2879(4) 0.5890(3) 0.0455(10) Uani 1 1 d . . . H18A H 0.4989 0.3780 0.5790 0.055 Uiso 1 1 calc R . . H18B H 0.6365 0.2780 0.5570 0.055 Uiso 1 1 calc R . . C19 C 0.3668(4) 0.2546(4) 0.7464(3) 0.0383(9) Uani 1 1 d . . . C20 C 0.2704(5) 0.3497(4) 0.7290(3) 0.0443(9) Uani 1 1 d . . . H20 H 0.2740 0.3844 0.6709 0.053 Uiso 1 1 calc R . . C21 C 0.1689(5) 0.3945(5) 0.7953(3) 0.0536(11) Uani 1 1 d . . . H21 H 0.1032 0.4590 0.7827 0.064 Uiso 1 1 calc R . . C22 C 0.1643(6) 0.3449(5) 0.8795(3) 0.0598(13) Uani 1 1 d . . . H22 H 0.0962 0.3759 0.9253 0.072 Uiso 1 1 calc R . . C23 C 0.2581(6) 0.2507(5) 0.8970(3) 0.0622(13) Uani 1 1 d . . . H23 H 0.2538 0.2158 0.9552 0.075 Uiso 1 1 calc R . . C24 C 0.3586(5) 0.2058(4) 0.8313(3) 0.0517(11) Uani 1 1 d . . . H24 H 0.4229 0.1405 0.8447 0.062 Uiso 1 1 calc R . . N4 N 0.0257(4) 0.1579(4) 0.6364(3) 0.0539(10) Uani 1 1 d . . . H4A H 0.0019 0.0725 0.6334 0.065 Uiso 1 1 calc R . . C25 C -0.0809(5) 0.1996(5) 0.7081(3) 0.0549(11) Uani 1 1 d . . . H25 H -0.0431 0.2676 0.7332 0.066 Uiso 1 1 calc R . . C26 C -0.0896(5) 0.2446(5) 0.6218(3) 0.0579(13) Uani 1 1 d . . . H26A H -0.0621 0.3379 0.5953 0.069 Uiso 1 1 calc R . . H26B H -0.1693 0.2072 0.6052 0.069 Uiso 1 1 calc R . . C27 C -0.1855(4) 0.0984(4) 0.7734(3) 0.0478(10) Uani 1 1 d . . . C28 C -0.2144(5) 0.1114(5) 0.8577(3) 0.0554(12) Uani 1 1 d . . . H28 H -0.1693 0.1819 0.8717 0.066 Uiso 1 1 calc R . . C29 C -0.3075(6) 0.0240(6) 0.9220(3) 0.0649(14) Uani 1 1 d . . . H29 H -0.3271 0.0349 0.9802 0.078 Uiso 1 1 calc R . . C30 C -0.3727(5) -0.0791(5) 0.9033(4) 0.0642(14) Uani 1 1 d . . . H30 H -0.4366 -0.1398 0.9482 0.077 Uiso 1 1 calc R . . C31 C -0.3447(5) -0.0937(5) 0.8190(4) 0.0584(12) Uani 1 1 d . . . H31 H -0.3895 -0.1645 0.8052 0.070 Uiso 1 1 calc R . . C32 C -0.2501(5) -0.0040(5) 0.7541(3) 0.0527(11) Uani 1 1 d . . . H32 H -0.2302 -0.0141 0.6957 0.063 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 Br1 0.0418(2) 0.0339(2) 0.0402(2) -0.00761(16) -0.00945(17) 0.00045(15) Br2 0.0403(2) 0.0357(2) 0.0470(2) -0.01091(17) -0.01048(18) 0.00110(15) Cu1 0.0306(3) 0.0487(3) 0.0437(3) -0.0109(2) -0.0056(2) 0.0015(2) Cu2 0.0310(3) 0.0466(3) 0.0438(3) -0.0077(2) -0.0064(2) -0.0002(2) N1 0.0325(16) 0.0323(15) 0.0423(18) -0.0085(14) -0.0067(14) 0.0008(13) C1 0.031(2) 0.045(2) 0.054(3) -0.0137(19) -0.0171(18) 0.0023(16) C2 0.032(2) 0.051(2) 0.056(3) -0.015(2) -0.0063(19) 0.0056(17) C3 0.038(2) 0.041(2) 0.041(2) -0.0096(17) -0.0181(17) 0.0108(16) C4 0.046(2) 0.044(2) 0.039(2) -0.0063(18) -0.0136(18) 0.0023(18) C5 0.055(3) 0.051(3) 0.057(3) 0.001(2) -0.014(2) -0.002(2) C6 0.074(3) 0.057(3) 0.046(3) 0.005(2) 0.001(2) 0.010(3) C7 0.100(4) 0.065(3) 0.040(3) -0.013(2) -0.019(3) 0.016(3) C8 0.068(3) 0.052(3) 0.051(3) -0.016(2) -0.027(2) 0.010(2) N2 0.037(2) 0.066(2) 0.066(3) -0.025(2) 0.0004(18) -0.0079(17) C9 0.046(2) 0.055(3) 0.056(3) -0.006(2) -0.008(2) -0.005(2) C10 0.035(2) 0.092(4) 0.065(3) -0.038(3) -0.005(2) -0.003(2) C11 0.031(2) 0.070(3) 0.052(3) -0.023(2) -0.0049(19) -0.007(2) C12 0.042(2) 0.075(3) 0.050(3) 0.001(2) -0.012(2) -0.020(2) C13 0.053(3) 0.049(3) 0.107(5) -0.020(3) -0.030(3) 0.006(2) C14 0.049(3) 0.086(4) 0.067(4) -0.044(3) 0.002(2) -0.001(3) C15 0.062(3) 0.086(4) 0.041(3) -0.010(3) -0.004(2) -0.006(3) C16 0.047(3) 0.054(3) 0.062(3) -0.009(2) -0.009(2) 0.000(2) N3 0.0340(17) 0.0333(16) 0.0410(18) -0.0116(14) -0.0062(14) 0.0018(13) C17 0.0302(19) 0.044(2) 0.058(3) -0.0131(19) -0.0202(18) 0.0055(16) C18 0.032(2) 0.042(2) 0.059(3) -0.012(2) -0.0067(19) -0.0052(17) C19 0.038(2) 0.038(2) 0.043(2) -0.0099(17) -0.0175(17) -0.0031(16) C20 0.048(2) 0.049(2) 0.044(2) -0.0167(19) -0.0209(19) 0.0091(19) C21 0.052(3) 0.058(3) 0.060(3) -0.025(2) -0.022(2) 0.016(2) C22 0.061(3) 0.069(3) 0.050(3) -0.027(2) -0.006(2) -0.003(2) C23 0.084(4) 0.062(3) 0.042(3) -0.007(2) -0.021(3) -0.005(3) C24 0.062(3) 0.046(2) 0.052(3) -0.006(2) -0.027(2) 0.003(2) N4 0.0394(19) 0.051(2) 0.061(2) -0.0056(18) -0.0009(17) 0.0057(16) C25 0.044(2) 0.062(3) 0.059(3) -0.021(2) -0.009(2) 0.005(2) C26 0.036(2) 0.063(3) 0.062(3) 0.011(2) -0.009(2) 0.002(2) C27 0.028(2) 0.057(3) 0.051(3) 0.002(2) -0.0073(18) 0.0070(18) C28 0.045(2) 0.057(3) 0.063(3) -0.020(2) -0.010(2) 0.008(2) C29 0.063(3) 0.083(4) 0.043(3) -0.013(3) -0.006(2) 0.017(3) C30 0.044(3) 0.064(3) 0.065(3) 0.014(3) -0.001(2) 0.001(2) C31 0.048(3) 0.051(3) 0.083(4) -0.020(3) -0.025(3) 0.006(2) C32 0.040(2) 0.076(3) 0.045(3) -0.019(2) -0.013(2) 0.018(2) 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 Br1 Cu1 2.5545(6) . ? Br1 Cu2 2.5589(6) . ? Br2 Cu1 2.7591(6) . ? Br2 Cu2 2.7628(6) . ? Cu1 N2 1.985(4) . ? Cu1 N1 1.988(3) . ? Cu1 Cu2 2.8216(7) . ? Cu2 N4 1.973(4) . ? Cu2 N3 1.978(3) . ? N1 C2 1.481(5) . ? N1 C1 1.502(5) . ? N1 H1A 0.9300 . ? C1 C3 1.482(6) . ? C1 C2 1.496(6) . ? C1 H1B 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.390(6) . ? C3 C8 1.397(6) . ? C4 C5 1.384(6) . ? C4 H4 0.9500 . ? C5 C6 1.392(7) . ? C5 H5 0.9500 . ? C6 C7 1.378(8) . ? C6 H6 0.9500 . ? C7 C8 1.378(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? N2 C9 1.445(6) . ? N2 C10 1.469(6) . ? N2 H2 0.9300 . ? C9 C10 1.435(7) . ? C9 C11 1.518(6) . ? C9 H9 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.369(7) . ? C11 C12 1.373(7) . ? C12 C13 1.388(7) . ? C12 H12 0.9500 . ? C13 C14 1.393(8) . ? C13 H13 0.9500 . ? C14 C15 1.358(8) . ? C14 H14 0.9500 . ? C15 C16 1.358(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N3 C18 1.473(5) . ? N3 C17 1.494(5) . ? N3 H3 0.9300 . ? C17 C18 1.476(6) . ? C17 C19 1.487(6) . ? C17 H17 1.0000 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.378(6) . ? C19 C20 1.392(5) . ? C20 C21 1.388(6) . ? C20 H20 0.9500 . ? C21 C22 1.377(7) . ? C21 H21 0.9500 . ? C22 C23 1.368(7) . ? C22 H22 0.9500 . ? C23 C24 1.378(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? N4 C25 1.455(6) . ? N4 C26 1.464(6) . ? N4 H4A 0.9300 . ? C25 C26 1.439(7) . ? C25 C27 1.505(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.368(7) . ? C27 C28 1.368(7) . ? C28 C29 1.368(7) . ? C28 H28 0.9500 . ? C29 C30 1.371(8) . ? C29 H29 0.9500 . ? C30 C31 1.374(8) . ? C30 H30 0.9500 . ? C31 C32 1.392(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 Cu1 Br1 Cu2 66.982(19) . . ? Cu1 Br2 Cu2 61.460(17) . . ? N2 Cu1 N1 144.00(16) . . ? N2 Cu1 Br1 104.25(12) . . ? N1 Cu1 Br1 103.70(9) . . ? N2 Cu1 Br2 89.64(13) . . ? N1 Cu1 Br2 98.10(9) . . ? Br1 Cu1 Br2 115.92(2) . . ? N2 Cu1 Cu2 103.11(13) . . ? N1 Cu1 Cu2 111.09(9) . . ? Br1 Cu1 Cu2 56.583(17) . . ? Br2 Cu1 Cu2 59.335(17) . . ? N4 Cu2 N3 145.22(15) . . ? N4 Cu2 Br1 103.06(11) . . ? N3 Cu2 Br1 104.35(9) . . ? N4 Cu2 Br2 89.65(12) . . ? N3 Cu2 Br2 97.36(9) . . ? Br1 Cu2 Br2 115.64(2) . . ? N4 Cu2 Cu1 102.27(12) . . ? N3 Cu2 Cu1 110.59(9) . . ? Br1 Cu2 Cu1 56.434(17) . . ? Br2 Cu2 Cu1 59.205(17) . . ? C2 N1 C1 60.2(3) . . ? C2 N1 Cu1 125.1(3) . . ? C1 N1 Cu1 127.6(2) . . ? C2 N1 H1A 111.6 . . ? C1 N1 H1A 111.6 . . ? Cu1 N1 H1A 111.6 . . ? C3 C1 C2 121.7(4) . . ? C3 C1 N1 117.8(3) . . ? C2 C1 N1 59.2(3) . . ? C3 C1 H1B 115.5 . . ? C2 C1 H1B 115.5 . . ? N1 C1 H1B 115.5 . . ? N1 C2 C1 60.6(3) . . ? N1 C2 H2A 117.7 . . ? C1 C2 H2A 117.7 . . ? N1 C2 H2B 117.7 . . ? C1 C2 H2B 117.7 . . ? H2A C2 H2B 114.8 . . ? C4 C3 C8 118.5(4) . . ? C4 C3 C1 122.3(4) . . ? C8 C3 C1 119.2(4) . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 119.4(5) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 120.8(5) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C3 120.5(5) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C9 N2 C10 59.0(3) . . ? C9 N2 Cu1 134.1(3) . . ? C10 N2 Cu1 124.4(3) . . ? C9 N2 H2 109.9 . . ? C10 N2 H2 109.9 . . ? Cu1 N2 H2 109.9 . . ? C10 C9 N2 61.4(3) . . ? C10 C9 C11 122.2(4) . . ? N2 C9 C11 118.6(4) . . ? C10 C9 H9 114.8 . . ? N2 C9 H9 114.8 . . ? C11 C9 H9 114.8 . . ? C9 C10 N2 59.7(3) . . ? C9 C10 H10A 117.8 . . ? N2 C10 H10A 117.8 . . ? C9 C10 H10B 117.8 . . ? N2 C10 H10B 117.8 . . ? H10A C10 H10B 114.9 . . ? C16 C11 C12 118.6(4) . . ? C16 C11 C9 115.5(4) . . ? C12 C11 C9 125.9(4) . . ? C11 C12 C13 120.4(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 119.5(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 121.6(5) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? C18 N3 C17 59.7(3) . . ? C18 N3 Cu2 124.9(3) . . ? C17 N3 Cu2 128.5(2) . . ? C18 N3 H3 111.5 . . ? C17 N3 H3 111.5 . . ? Cu2 N3 H3 111.5 . . ? C18 C17 C19 122.4(4) . . ? C18 C17 N3 59.5(3) . . ? C19 C17 N3 117.9(3) . . ? C18 C17 H17 115.2 . . ? C19 C17 H17 115.2 . . ? N3 C17 H17 115.2 . . ? N3 C18 C17 60.9(3) . . ? N3 C18 H18A 117.7 . . ? C17 C18 H18A 117.7 . . ? N3 C18 H18B 117.7 . . ? C17 C18 H18B 117.7 . . ? H18A C18 H18B 114.8 . . ? C24 C19 C20 118.2(4) . . ? C24 C19 C17 120.4(4) . . ? C20 C19 C17 121.4(4) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.5(4) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.8(5) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C19 C24 C23 120.8(4) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C25 N4 C26 59.1(3) . . ? C25 N4 Cu2 133.7(3) . . ? C26 N4 Cu2 125.9(3) . . ? C25 N4 H4A 109.6 . . ? C26 N4 H4A 109.6 . . ? Cu2 N4 H4A 109.6 . . ? C26 C25 N4 60.8(3) . . ? C26 C25 C27 123.4(4) . . ? N4 C25 C27 119.0(4) . . ? C26 C25 H25 114.4 . . ? N4 C25 H25 114.4 . . ? C27 C25 H25 114.4 . . ? C25 C26 N4 60.1(3) . . ? C25 C26 H26A 117.8 . . ? N4 C26 H26A 117.8 . . ? C25 C26 H26B 117.8 . . ? N4 C26 H26B 117.8 . . ? H26A C26 H26B 114.9 . . ? C32 C27 C28 119.1(4) . . ? C32 C27 C25 124.7(4) . . ? C28 C27 C25 116.2(4) . . ? C29 C28 C27 120.7(5) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.6(5) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C31 119.4(5) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 119.5(5) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C27 C32 C31 120.6(4) . . ? C27 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? 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 Cu2 Br1 Cu1 N2 -96.47(14) . . . . ? Cu2 Br1 Cu1 N1 106.44(10) . . . . ? Cu2 Br1 Cu1 Br2 0.20(2) . . . . ? Cu2 Br2 Cu1 N2 105.51(12) . . . . ? Cu2 Br2 Cu1 N1 -109.77(9) . . . . ? Cu2 Br2 Cu1 Br1 -0.20(2) . . . . ? Cu1 Br1 Cu2 N4 -96.20(13) . . . . ? Cu1 Br1 Cu2 N3 105.43(10) . . . . ? Cu1 Br1 Cu2 Br2 -0.20(2) . . . . ? Cu1 Br2 Cu2 N4 104.54(12) . . . . ? Cu1 Br2 Cu2 N3 -109.63(9) . . . . ? Cu1 Br2 Cu2 Br1 0.20(2) . . . . ? N2 Cu1 Cu2 N4 -163.77(16) . . . . ? N1 Cu1 Cu2 N4 4.81(15) . . . . ? Br1 Cu1 Cu2 N4 97.65(11) . . . . ? Br2 Cu1 Cu2 N4 -82.13(11) . . . . ? N2 Cu1 Cu2 N3 4.66(15) . . . . ? N1 Cu1 Cu2 N3 173.24(13) . . . . ? Br1 Cu1 Cu2 N3 -93.92(10) . . . . ? Br2 Cu1 Cu2 N3 86.29(10) . . . . ? N2 Cu1 Cu2 Br1 98.58(12) . . . . ? N1 Cu1 Cu2 Br1 -92.84(10) . . . . ? Br2 Cu1 Cu2 Br1 -179.79(2) . . . . ? N2 Cu1 Cu2 Br2 -81.63(12) . . . . ? N1 Cu1 Cu2 Br2 86.95(10) . . . . ? Br1 Cu1 Cu2 Br2 179.79(2) . . . . ? N2 Cu1 N1 C2 -121.9(4) . . . . ? Br1 Cu1 N1 C2 18.2(3) . . . . ? Br2 Cu1 N1 C2 137.4(3) . . . . ? Cu2 Cu1 N1 C2 77.3(3) . . . . ? N2 Cu1 N1 C1 -44.9(4) . . . . ? Br1 Cu1 N1 C1 95.1(3) . . . . ? Br2 Cu1 N1 C1 -145.6(3) . . . . ? Cu2 Cu1 N1 C1 154.2(3) . . . . ? C2 N1 C1 C3 112.2(4) . . . . ? Cu1 N1 C1 C3 -1.1(5) . . . . ? Cu1 N1 C1 C2 -113.3(3) . . . . ? Cu1 N1 C2 C1 117.2(3) . . . . ? C3 C1 C2 N1 -105.7(4) . . . . ? C2 C1 C3 C4 26.2(6) . . . . ? N1 C1 C3 C4 -43.0(5) . . . . ? C2 C1 C3 C8 -152.3(4) . . . . ? N1 C1 C3 C8 138.5(4) . . . . ? C8 C3 C4 C5 -0.4(6) . . . . ? C1 C3 C4 C5 -178.8(4) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? C5 C6 C7 C8 0.3(8) . . . . ? C6 C7 C8 C3 -0.5(8) . . . . ? C4 C3 C8 C7 0.5(6) . . . . ? C1 C3 C8 C7 179.0(4) . . . . ? N1 Cu1 N2 C9 67.2(5) . . . . ? Br1 Cu1 N2 C9 -72.8(4) . . . . ? Br2 Cu1 N2 C9 170.5(4) . . . . ? Cu2 Cu1 N2 C9 -131.1(4) . . . . ? N1 Cu1 N2 C10 145.3(4) . . . . ? Br1 Cu1 N2 C10 5.4(4) . . . . ? Br2 Cu1 N2 C10 -111.3(4) . . . . ? Cu2 Cu1 N2 C10 -53.0(4) . . . . ? Cu1 N2 C9 C10 109.6(5) . . . . ? C10 N2 C9 C11 113.2(5) . . . . ? Cu1 N2 C9 C11 -137.2(4) . . . . ? C11 C9 C10 N2 -107.5(5) . . . . ? Cu1 N2 C10 C9 -124.9(4) . . . . ? C10 C9 C11 C16 -148.3(5) . . . . ? N2 C9 C11 C16 139.3(5) . . . . ? C10 C9 C11 C12 31.1(7) . . . . ? N2 C9 C11 C12 -41.3(7) . . . . ? C16 C11 C12 C13 -0.2(7) . . . . ? C9 C11 C12 C13 -179.6(4) . . . . ? C11 C12 C13 C14 1.0(7) . . . . ? C12 C13 C14 C15 -1.3(8) . . . . ? C13 C14 C15 C16 0.9(8) . . . . ? C14 C15 C16 C11 -0.1(8) . . . . ? C12 C11 C16 C15 -0.2(7) . . . . ? C9 C11 C16 C15 179.2(4) . . . . ? N4 Cu2 N3 C18 -123.3(3) . . . . ? Br1 Cu2 N3 C18 17.8(3) . . . . ? Br2 Cu2 N3 C18 136.7(3) . . . . ? Cu1 Cu2 N3 C18 76.9(3) . . . . ? N4 Cu2 N3 C17 -46.7(4) . . . . ? Br1 Cu2 N3 C17 94.3(3) . . . . ? Br2 Cu2 N3 C17 -146.8(3) . . . . ? Cu1 Cu2 N3 C17 153.4(3) . . . . ? Cu2 N3 C17 C18 -112.4(3) . . . . ? C18 N3 C17 C19 113.0(4) . . . . ? Cu2 N3 C17 C19 0.6(5) . . . . ? Cu2 N3 C18 C17 118.1(3) . . . . ? C19 C17 C18 N3 -105.7(4) . . . . ? C18 C17 C19 C24 -153.5(4) . . . . ? N3 C17 C19 C24 136.6(4) . . . . ? C18 C17 C19 C20 25.9(6) . . . . ? N3 C17 C19 C20 -44.0(5) . . . . ? C24 C19 C20 C21 0.2(6) . . . . ? C17 C19 C20 C21 -179.2(4) . . . . ? C19 C20 C21 C22 0.5(7) . . . . ? C20 C21 C22 C23 -1.0(7) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C20 C19 C24 C23 -0.4(6) . . . . ? C17 C19 C24 C23 179.1(4) . . . . ? C22 C23 C24 C19 -0.1(7) . . . . ? N3 Cu2 N4 C25 62.6(5) . . . . ? Br1 Cu2 N4 C25 -78.7(4) . . . . ? Br2 Cu2 N4 C25 165.0(4) . . . . ? Cu1 Cu2 N4 C25 -136.7(4) . . . . ? N3 Cu2 N4 C26 141.9(4) . . . . ? Br1 Cu2 N4 C26 0.6(4) . . . . ? Br2 Cu2 N4 C26 -115.7(4) . . . . ? Cu1 Cu2 N4 C26 -57.4(4) . . . . ? Cu2 N4 C25 C26 111.9(4) . . . . ? C26 N4 C25 C27 114.2(5) . . . . ? Cu2 N4 C25 C27 -133.8(4) . . . . ? C27 C25 C26 N4 -107.2(5) . . . . ? Cu2 N4 C26 C25 -124.1(4) . . . . ? C26 C25 C27 C32 33.1(7) . . . . ? N4 C25 C27 C32 -39.3(6) . . . . ? C26 C25 C27 C28 -147.9(5) . . . . ? N4 C25 C27 C28 139.8(4) . . . . ? C32 C27 C28 C29 -0.6(7) . . . . ? C25 C27 C28 C29 -179.7(4) . . . . ? C27 C28 C29 C30 0.6(7) . . . . ? C28 C29 C30 C31 -0.5(8) . . . . ? C29 C30 C31 C32 0.3(7) . . . . ? C28 C27 C32 C31 0.4(6) . . . . ? C25 C27 C32 C31 179.4(4) . . . . ? C30 C31 C32 C27 -0.2(7) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Br2 0.93 2.81 3.625(3) 146.7 2_556 N3 H3 Br2 0.93 2.85 3.634(3) 143.3 2_656 _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. ; #===END data_6_(CCDC-771767) _database_code_depnum_ccdc_archive 'CCDC 771767' #TrackingRef 'Dalton-Transaction---data[1].cif' _audit_author_name 'S. Wirth, S. Albrecht' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 15-Marz-06 _chemical_name_systematic ; [Bis(?3-bromo)-tris(?4-bromo)-hexakis(2,2-dimethylaziridine) -hexacopper(I)]bromide ; _chemical_name_common ; (Bis(?3-bromo)-tris(?4-bromo)-hexakis(2,2-dimethylaziridine) - hexacopper(i))bromide ; _chemical_formula_moiety 'C24 H54 Br5 Cu6 N6, Br' _chemical_formula_sum 'C24 H54 Br6 Cu6 N6' _chemical_compound_source ? _chemical_properties_physical 'air-sensitive, oxygen-sensitive' _exptl_crystal_recrystallization_method 'slow isothermic diffusion of n-pentane into a solution in dichloromethane' _chemical_melting_point ? _exptl_crystal_description platelet _exptl_crystal_colour colourless loop_ _diffrn_ambient_temperature 200(2) _chemical_formula_weight 1287.426 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' Cu Cu 0.3201 1.2651 '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 hexagonal _symmetry_space_group_name_H-M 'P 63/m' _symmetry_Int_Tables_number 176 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall -P6c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 10.3534(10) _cell_length_b 10.3534(10) _cell_length_c 21.751(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2019.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3104 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.1175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 9.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.411 _exptl_absorpt_correction_T_max 0.696 _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction. University of Goettingen, Germany, 2001 ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type ? _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle phi/omega-scan _kl_diffrn_measurement_scan_step_degree 1.50 _kl_diffrn_measurement_scan_time_per_degree 20 _kl_diffrn_measurement_detector_distance 35 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6163 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.516 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.075 _reflns_number_total 1591 _reflns_number_gt 1378 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0203P)^2^+2.7610P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1591 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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. ; 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 Br1 Br 0.10002(4) 0.64521(4) 0.2500 0.02926(11) Uani 1 2 d S . . Br2 Br 0.3333 0.6667 0.09471(2) 0.03939(14) Uani 1 3 d S . . Br3 Br 0.0000 0.0000 0.2500 0.03272(16) Uani 1 6 d S . . Cu1 Cu 0.18223(5) 0.49767(5) 0.17803(2) 0.04819(13) Uani 1 1 d . . . N1 N 0.0011(3) 0.2988(3) 0.16458(11) 0.0342(5) Uani 1 1 d . . . H1 H 0.0129 0.2225 0.1812 0.041 Uiso 1 1 calc R . . C1 C -0.1050(3) 0.2447(3) 0.11207(14) 0.0379(7) Uani 1 1 d . . . C2 C -0.1541(3) 0.2686(4) 0.17224(16) 0.0483(8) Uani 1 1 d . . . H2A H -0.2241 0.1795 0.1962 0.058 Uiso 1 1 calc R . . H2B H -0.1692 0.3553 0.1767 0.058 Uiso 1 1 calc R . . C3 C -0.1611(5) 0.0870(4) 0.0917(2) 0.0629(11) Uani 1 1 d . . . H3A H -0.2561 0.0500 0.0701 0.094 Uiso 1 1 calc R . . H3B H -0.1757 0.0243 0.1277 0.094 Uiso 1 1 calc R . . H3C H -0.0880 0.0837 0.0641 0.094 Uiso 1 1 calc R . . C4 C -0.0697(5) 0.3573(5) 0.06219(19) 0.0716(13) Uani 1 1 d . . . H4A H -0.1601 0.3301 0.0384 0.107 Uiso 1 1 calc R . . H4B H 0.0068 0.3592 0.0350 0.107 Uiso 1 1 calc R . . H4C H -0.0326 0.4561 0.0805 0.107 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 Br1 0.02450(18) 0.02797(19) 0.0354(2) 0.000 0.000 0.01316(15) Br2 0.04135(18) 0.04135(18) 0.0355(3) 0.000 0.000 0.02068(9) Br3 0.0291(2) 0.0291(2) 0.0400(4) 0.000 0.000 0.01453(10) Cu1 0.0379(2) 0.0422(2) 0.0553(3) -0.00329(19) -0.00476(18) 0.01314(17) N1 0.0356(12) 0.0311(12) 0.0362(13) -0.0018(10) -0.0069(11) 0.0170(10) C1 0.0341(15) 0.0402(16) 0.0387(16) -0.0033(13) -0.0088(13) 0.0180(13) C2 0.0332(16) 0.0468(18) 0.056(2) -0.0032(16) 0.0047(14) 0.0131(14) C3 0.063(2) 0.053(2) 0.073(3) -0.0230(19) -0.029(2) 0.0286(19) C4 0.070(3) 0.071(3) 0.053(2) 0.017(2) -0.021(2) 0.019(2) 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 Br1 Cu1 2.5753(6) 12_566 ? Br1 Cu1 2.5753(6) 3_565 ? Br1 Cu1 2.6093(6) 10_556 ? Br1 Cu1 2.6093(6) . ? Br2 Cu1 2.4609(6) 3_565 ? Br2 Cu1 2.4609(6) . ? Br2 Cu1 2.4609(6) 2_665 ? Cu1 N1 1.995(2) . ? Cu1 Br1 2.5753(6) 2_665 ? Cu1 Cu1 2.8836(7) 3_565 ? Cu1 Cu1 2.8836(7) 2_665 ? N1 C2 1.486(4) . ? N1 C1 1.487(4) . ? N1 H1 0.9300 . ? C1 C2 1.469(5) . ? C1 C4 1.497(5) . ? C1 C3 1.500(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 Cu1 Br1 Cu1 74.87(2) 12_566 3_565 ? Cu1 Br1 Cu1 67.58(2) 12_566 10_556 ? Cu1 Br1 Cu1 110.36(2) 3_565 10_556 ? Cu1 Br1 Cu1 110.36(2) 12_566 . ? Cu1 Br1 Cu1 67.58(2) 3_565 . ? Cu1 Br1 Cu1 73.73(2) 10_556 . ? Cu1 Br2 Cu1 71.73(2) 3_565 . ? Cu1 Br2 Cu1 71.73(2) 3_565 2_665 ? Cu1 Br2 Cu1 71.73(2) . 2_665 ? N1 Cu1 Br2 124.13(7) . . ? N1 Cu1 Br1 106.64(7) . 2_665 ? Br2 Cu1 Br1 108.721(19) . 2_665 ? N1 Cu1 Br1 106.19(7) . . ? Br2 Cu1 Br1 107.642(19) . . ? Br1 Cu1 Br1 101.17(2) 2_665 . ? N1 Cu1 Cu1 148.08(7) . 3_565 ? Br2 Cu1 Cu1 54.134(11) . 3_565 ? Br1 Cu1 Cu1 102.925(14) 2_665 3_565 ? Br1 Cu1 Cu1 55.649(16) . 3_565 ? N1 Cu1 Cu1 149.80(7) . 2_665 ? Br2 Cu1 Cu1 54.134(11) . 2_665 ? Br1 Cu1 Cu1 56.771(16) 2_665 2_665 ? Br1 Cu1 Cu1 102.067(14) . 2_665 ? Cu1 Cu1 Cu1 60.0 3_565 2_665 ? C2 N1 C1 59.2(2) . . ? C2 N1 Cu1 124.1(2) . . ? C1 N1 Cu1 129.62(19) . . ? C2 N1 H1 111.4 . . ? C1 N1 H1 111.4 . . ? Cu1 N1 H1 111.4 . . ? C2 C1 N1 60.35(19) . . ? C2 C1 C4 119.0(3) . . ? N1 C1 C4 114.6(3) . . ? C2 C1 C3 117.9(3) . . ? N1 C1 C3 116.6(3) . . ? C4 C1 C3 116.4(3) . . ? C1 C2 N1 60.41(19) . . ? C1 C2 H2A 117.7 . . ? N1 C2 H2A 117.7 . . ? C1 C2 H2B 117.7 . . ? N1 C2 H2B 117.7 . . ? H2A C2 H2B 114.9 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 Cu1 Br2 Cu1 N1 140.83(9) 3_565 . . . ? Cu1 Br2 Cu1 N1 -142.98(9) 2_665 . . . ? Cu1 Br2 Cu1 Br1 -92.661(11) 3_565 . . 2_665 ? Cu1 Br2 Cu1 Br1 -16.468(17) 2_665 . . 2_665 ? Cu1 Br2 Cu1 Br1 16.145(17) 3_565 . . . ? Cu1 Br2 Cu1 Br1 92.337(11) 2_665 . . . ? Cu1 Br2 Cu1 Cu1 76.192(12) 2_665 . . 3_565 ? Cu1 Br2 Cu1 Cu1 -76.192(12) 3_565 . . 2_665 ? Cu1 Br1 Cu1 N1 146.31(7) 12_566 . . . ? Cu1 Br1 Cu1 N1 -150.71(7) 3_565 . . . ? Cu1 Br1 Cu1 N1 88.46(7) 10_556 . . . ? Cu1 Br1 Cu1 Br2 -78.82(2) 12_566 . . . ? Cu1 Br1 Cu1 Br2 -15.840(18) 3_565 . . . ? Cu1 Br1 Cu1 Br2 -136.671(13) 10_556 . . . ? Cu1 Br1 Cu1 Br1 35.141(10) 12_566 . . 2_665 ? Cu1 Br1 Cu1 Br1 98.119(17) 3_565 . . 2_665 ? Cu1 Br1 Cu1 Br1 -22.71(2) 10_556 . . 2_665 ? Cu1 Br1 Cu1 Cu1 -62.98(2) 12_566 . . 3_565 ? Cu1 Br1 Cu1 Cu1 -120.831(16) 10_556 . . 3_565 ? Cu1 Br1 Cu1 Cu1 -22.922(19) 12_566 . . 2_665 ? Cu1 Br1 Cu1 Cu1 40.056(9) 3_565 . . 2_665 ? Cu1 Br1 Cu1 Cu1 -80.775(13) 10_556 . . 2_665 ? Br2 Cu1 N1 C2 -103.0(2) . . . . ? Br1 Cu1 N1 C2 129.6(2) 2_665 . . . ? Br1 Cu1 N1 C2 22.3(3) . . . . ? Cu1 Cu1 N1 C2 -27.5(3) 3_565 . . . ? Cu1 Cu1 N1 C2 -178.96(18) 2_665 . . . ? Br2 Cu1 N1 C1 -27.0(3) . . . . ? Br1 Cu1 N1 C1 -154.4(2) 2_665 . . . ? Br1 Cu1 N1 C1 98.3(2) . . . . ? Cu1 Cu1 N1 C1 48.5(3) 3_565 . . . ? Cu1 Cu1 N1 C1 -102.9(2) 2_665 . . . ? Cu1 N1 C1 C2 -110.7(3) . . . . ? C2 N1 C1 C4 110.7(4) . . . . ? Cu1 N1 C1 C4 -0.1(4) . . . . ? C2 N1 C1 C3 -108.5(4) . . . . ? Cu1 N1 C1 C3 140.8(3) . . . . ? C4 C1 C2 N1 -103.4(3) . . . . ? C3 C1 C2 N1 106.3(3) . . . . ? Cu1 N1 C2 C1 119.6(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Br3 0.93 2.69 3.604(2) 166.0 . _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. ; #===END data_7_(CCDC-771768) _database_code_depnum_ccdc_archive 'CCDC 771768' #TrackingRef 'Dalton-Transaction---data[1].cif' _audit_author_name 'S. Wirth, P. Mayer' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date 22-Oct-07 _chemical_name_systematic ;[(N-(2-Aminoisobutyl)-2,2-dimethylaziridine-2N,N0)- bromidocopper(I)] ; _chemical_name_common ;((N-(2-Aminoisobutyl)-2,2-dimethylaziridine-2N,N0)- bromidocopper(i)) ; _chemical_formula_moiety 'C8 H18 Br Cu N2' _chemical_formula_sum 'C8 H18 Br Cu N2' _chemical_compound_source ? _chemical_properties_physical 'air-sensitive, oxygen-sensitive' _exptl_crystal_recrystallization_method 'slow isothermic diffusion of n-pentane into a solution in dichloromethane' _chemical_melting_point ? _exptl_crystal_description platelet _exptl_crystal_colour colourless _diffrn_ambient_temperature 200(2) _chemical_formula_weight 285.692 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' Cu Cu 0.3201 1.2651 '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 'C 2/c' _symmetry_Int_Tables_number 15 _chemical_absolute_configuration ? _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.6475(9) _cell_length_b 16.6004(8) _cell_length_c 9.3899(5) _cell_angle_alpha 90.00 _cell_angle_beta 120.918(3) _cell_angle_gamma 90.00 _cell_volume 2359.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14689 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 26.022 _cell_special_details ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.60824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 5.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details ; Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction. University of Goettingen, Germany, 2001 ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -6 -1 5 0.022000 6 1 -4 0.005000 -6 -7 -1 0.061000 11 -10 0 0.036000 -1 16 1 0.045000 19 20 3 0.061000 -2 3 0 0.065000 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type ? _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _kl_diffrn_measurement_scan_angle omega-scan _kl_diffrn_measurement_scan_step_degree 2.0 _kl_diffrn_measurement_scan_time_per_degree 20 _kl_diffrn_measurement_detector_distance 30 _diffrn_special_details ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7876 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.99 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.589 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.080 _reflns_number_total 2303 _reflns_number_gt 1744 _reflns_threshold_expression >2sigma(I) _reflns_special_details ? _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565 ; _computing_publication_material ? _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^)+(0.0384P)^2^+2.0960P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2303 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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. ; 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 Br1 Br 0.14749(3) 0.86975(2) 0.10430(5) 0.04845(16) Uani 1 1 d . . . Cu1 Cu 0.14491(3) 1.00254(3) 0.15722(6) 0.04928(18) Uani 1 1 d . . . N1 N 0.2525(2) 1.08565(18) 0.2022(4) 0.0520(9) Uani 1 1 d . . . N2 N 0.08907(19) 1.10120(17) 0.1805(4) 0.0446(8) Uani 1 1 d . . . H2A H 0.0294 1.1005 0.1043 0.053 Uiso 1 1 calc R . . H2B H 0.0968 1.1032 0.2850 0.053 Uiso 1 1 calc R . . C1 C 0.3454(2) 1.0711(2) 0.2547(5) 0.0510(10) Uani 1 1 d . . . C2 C 0.2841(3) 1.0926(3) 0.0816(6) 0.0683(13) Uani 1 1 d . . . H2C H 0.2666 1.0498 -0.0032 0.082 Uiso 1 1 calc R . . H2D H 0.2889 1.1471 0.0445 0.082 Uiso 1 1 calc R . . C3 C 0.4153(3) 1.1319(3) 0.3674(7) 0.0779(16) Uani 1 1 d . . . H3A H 0.4714 1.1190 0.3747 0.117 Uiso 1 1 calc R . . H3B H 0.4231 1.1295 0.4784 0.117 Uiso 1 1 calc R . . H3C H 0.3965 1.1861 0.3217 0.117 Uiso 1 1 calc R . . C4 C 0.3743(3) 0.9848(3) 0.2997(8) 0.0793(16) Uani 1 1 d . . . H4A H 0.3279 0.9489 0.2193 0.119 Uiso 1 1 calc R . . H4B H 0.3852 0.9735 0.4111 0.119 Uiso 1 1 calc R . . H4C H 0.4287 0.9758 0.2978 0.119 Uiso 1 1 calc R . . C6 C 0.1301(3) 1.1736(2) 0.1527(5) 0.0463(9) Uani 1 1 d . . . C5 C 0.2289(2) 1.1618(2) 0.2508(6) 0.0516(10) Uani 1 1 d . . . H5A H 0.2581 1.2074 0.2301 0.062 Uiso 1 1 calc R . . H5B H 0.2499 1.1606 0.3709 0.062 Uiso 1 1 calc R . . C7 C 0.1063(3) 1.2505(2) 0.2124(6) 0.0606(11) Uani 1 1 d . . . H7A H 0.0419 1.2563 0.1540 0.091 Uiso 1 1 calc R . . H7B H 0.1320 1.2974 0.1891 0.091 Uiso 1 1 calc R . . H7C H 0.1297 1.2469 0.3321 0.091 Uiso 1 1 calc R . . C8 C 0.0926(3) 1.1788(3) -0.0345(5) 0.0637(12) Uani 1 1 d . . . H8A H 0.0285 1.1864 -0.0918 0.096 Uiso 1 1 calc R . . H8B H 0.1059 1.1289 -0.0732 0.096 Uiso 1 1 calc R . . H8C H 0.1195 1.2245 -0.0585 0.096 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 Br1 0.0522(3) 0.0349(2) 0.0493(3) -0.00479(17) 0.0197(2) -0.00328(16) Cu1 0.0554(3) 0.0351(3) 0.0477(3) -0.0052(2) 0.0197(3) -0.00249(19) N1 0.0408(18) 0.0426(18) 0.065(2) -0.0092(16) 0.0218(17) -0.0056(14) N2 0.0427(18) 0.0420(17) 0.0421(19) -0.0028(14) 0.0168(15) -0.0031(13) C1 0.037(2) 0.048(2) 0.061(3) 0.003(2) 0.020(2) -0.0016(16) C2 0.060(3) 0.079(3) 0.069(3) -0.001(3) 0.035(3) 0.000(2) C3 0.050(3) 0.054(3) 0.101(4) -0.008(3) 0.018(3) -0.009(2) C4 0.057(3) 0.052(3) 0.121(5) 0.003(3) 0.040(3) 0.003(2) C6 0.053(2) 0.036(2) 0.050(2) 0.0023(17) 0.026(2) -0.0018(16) C5 0.047(2) 0.034(2) 0.067(3) -0.0071(19) 0.024(2) -0.0057(16) C7 0.067(3) 0.039(2) 0.072(3) 0.001(2) 0.033(2) 0.0069(19) C8 0.062(3) 0.077(3) 0.050(3) 0.011(2) 0.027(2) 0.001(2) 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 Br1 Cu1 2.2653(6) . ? Cu1 N2 1.981(3) . ? Cu1 N1 2.205(3) . ? N1 C1 1.469(5) . ? N1 C5 1.474(5) . ? N1 C2 1.503(6) . ? N2 C6 1.493(5) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 C2 1.460(6) . ? C1 C4 1.507(6) . ? C1 C3 1.523(6) . ? C2 H2C 0.9900 . ? C2 H2D 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C5 1.509(5) . ? C6 C8 1.530(6) . ? C6 C7 1.538(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 Cu1 N1 83.66(12) . . ? N2 Cu1 Br1 153.65(9) . . ? N1 Cu1 Br1 122.59(9) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 C2 58.8(3) . . ? C5 N1 C2 116.2(3) . . ? C1 N1 Cu1 131.6(2) . . ? C5 N1 Cu1 104.1(2) . . ? C2 N1 Cu1 121.3(3) . . ? C6 N2 Cu1 109.4(2) . . ? C6 N2 H2A 109.8 . . ? Cu1 N2 H2A 109.8 . . ? C6 N2 H2B 109.8 . . ? Cu1 N2 H2B 109.8 . . ? H2A N2 H2B 108.2 . . ? C2 C1 N1 61.7(3) . . ? C2 C1 C4 119.6(4) . . ? N1 C1 C4 114.2(3) . . ? C2 C1 C3 118.9(4) . . ? N1 C1 C3 119.4(4) . . ? C4 C1 C3 113.5(4) . . ? C1 C2 N1 59.4(3) . . ? C1 C2 H2C 117.8 . . ? N1 C2 H2C 117.8 . . ? C1 C2 H2D 117.8 . . ? N1 C2 H2D 117.8 . . ? H2C C2 H2D 115.0 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C6 C5 107.5(3) . . ? N2 C6 C8 106.5(3) . . ? C5 C6 C8 113.0(4) . . ? N2 C6 C7 110.9(3) . . ? C5 C6 C7 109.4(3) . . ? C8 C6 C7 109.5(3) . . ? N1 C5 C6 110.1(3) . . ? N1 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 N2 Cu1 N1 C1 161.5(4) . . . . ? Br1 Cu1 N1 C1 -20.9(4) . . . . ? N2 Cu1 N1 C5 9.2(3) . . . . ? Br1 Cu1 N1 C5 -173.2(2) . . . . ? N2 Cu1 N1 C2 -124.1(3) . . . . ? Br1 Cu1 N1 C2 53.5(3) . . . . ? N1 Cu1 N2 C6 20.1(2) . . . . ? Br1 Cu1 N2 C6 -155.33(19) . . . . ? C5 N1 C1 C2 -104.9(4) . . . . ? Cu1 N1 C1 C2 106.0(4) . . . . ? C5 N1 C1 C4 143.2(4) . . . . ? C2 N1 C1 C4 -112.0(5) . . . . ? Cu1 N1 C1 C4 -5.9(6) . . . . ? C5 N1 C1 C3 4.3(6) . . . . ? C2 N1 C1 C3 109.1(5) . . . . ? Cu1 N1 C1 C3 -144.8(4) . . . . ? C4 C1 C2 N1 103.3(4) . . . . ? C3 C1 C2 N1 -109.8(4) . . . . ? C5 N1 C2 C1 109.2(4) . . . . ? Cu1 N1 C2 C1 -122.7(3) . . . . ? Cu1 N2 C6 C5 -46.0(3) . . . . ? Cu1 N2 C6 C8 75.3(3) . . . . ? Cu1 N2 C6 C7 -165.6(3) . . . . ? C1 N1 C5 C6 166.7(3) . . . . ? C2 N1 C5 C6 99.5(4) . . . . ? Cu1 N1 C5 C6 -36.7(4) . . . . ? N2 C6 C5 N1 56.1(4) . . . . ? C8 C6 C5 N1 -61.2(4) . . . . ? C7 C6 C5 N1 176.6(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A Br1 0.92 2.75 3.652(3) 168.4 5_575 N2 H2B Br1 0.92 2.69 3.594(3) 167.9 6_576 _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. ; #===END