Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2007 data_General _audit_creation_date '2007-01-19' _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. H. L. Kwong' _publ_contact_author_email 'bhhoik@cityu.edu.hk' _publ_contact_author_fax '(852) 2788 7406' _publ_contact_author_phone '(852) 2788-7304' _publ_contact_author_address ; Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon Tong, Hong Kong ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'ENTER JOURNAL NAME HERE' _publ_requested_category ? # 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Kwong, Hoi Lun' . ; Department of Biology and Chemistry, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon Tong, Hong Kong ; ' Wong, Wing-Tak' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). PATTY. The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., de Gelder, R., Israel, R. and Smits, J.M.M. (1999). The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Bruker AXS Inc. (1998). SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999). SAINT, version 6.02, Madison, Wisconsin, USA. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Johnson, C. K. (1976). ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC & Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SADABS & SHELXS97. G\"ottingen University, G\"ottingen, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996). CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. Flack, H. D. (1983), Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; All of the non-H atoms were refined isotropically. All H-atoms were placed at geometrical positions with C-H = 0.95\%A and refined using riding model, U~iso~(H) = 1.2U~eq~(C). The absolute configuration was determined based on the anomalous dispersions effects and with reference to the chirality of the starting ligand. The absolute configuration of C9, C11, C20, C22, C33, C35, C44 and C46 were all found to be R. The space group P-1 (#2) has also been tried, however, the R and Rw values obtained were much worst than using the current space group, P 1. ; #============================================================================== data_wt1368w #-HLKwong-C2pinbpyReBr #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H28 Br N2 O3 Re ' _chemical_formula_moiety 'C27 H28 Br N2 O3 Re ' _chemical_formula_weight 694.64 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' #------------------------------------------------------------------------------ _cell_length_a 9.5930(11) _cell_length_b 10.5494(13) _cell_length_c 13.618(2) _cell_angle_alpha 76.415(2) _cell_angle_beta 85.266(2) _cell_angle_gamma 81.798(2) _cell_volume 1324.2(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11107 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 301(1) #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676.00 _exptl_absorpt_coefficient_mu 6.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.399 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11107 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9512 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9512 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9270 _reflns_number_gt 8201 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0310 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8218 _refine_ls_number_parameters 670 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.035]' _refine_ls_shift/su_max 0.0130 _refine_diff_density_max 1.82 _refine_diff_density_min -0.99 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 3476 Friedel Pairs' _refine_ls_abs_structure_Flack 0.076(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Re' 'Re' -1.018 7.231 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Re(1) Re 0.20984(13) 0.89509(12) 0.03895(10) 0.05119(13) Uani 1.00 1 d . . . Re(2) Re 0.49834(13) 0.50458(12) 0.50067(10) 0.0526(1) Uani 1.00 1 d . . . Br(1) Br 0.0963(2) 1.1421(2) -0.0013(2) 0.0752(4) Uani 1.00 1 d . . . Br(2) Br 0.6297(2) 0.2671(2) 0.5566(2) 0.0776(4) Uani 1.00 1 d . . . O(1) O -0.0670(9) 0.7775(9) 0.0601(8) 0.081(3) Uani 1.00 1 d . . . O(2) O 0.343(1) 0.6081(9) 0.0946(10) 0.111(4) Uani 1.00 1 d . . . O(3) O 0.1237(12) 0.8883(12) 0.2612(8) 0.094(4) Uani 1.00 1 d . . . O(4) O 0.5927(12) 0.525(1) 0.2775(8) 0.105(4) Uani 1.00 1 d . . . O(5) O 0.336(1) 0.7779(11) 0.4462(11) 0.127(4) Uani 1.00 1 d . . . O(6) O 0.7676(12) 0.6336(13) 0.4780(7) 0.118(4) Uani 1.00 1 d . . . N(1) N 0.2589(10) 0.9394(9) -0.1302(8) 0.050(2) Uani 1.00 1 d . . . N(2) N 0.4215(10) 0.9642(9) 0.0188(8) 0.050(2) Uani 1.00 1 d . . . N(3) N 0.3034(10) 0.4070(9) 0.5208(8) 0.049(2) Uani 1.00 1 d . . . N(4) N 0.4406(11) 0.4778(9) 0.6624(8) 0.051(2) Uani 1.00 1 d . . . C(1) C 0.0386(12) 0.8262(12) 0.0508(10) 0.063(3) Uani 1.00 1 d . . . C(2) C 0.2992(12) 0.7168(7) 0.0672(9) 0.061(3) Uani 1.00 1 d . . . C(3) C 0.1595(12) 0.8885(10) 0.1809(6) 0.055(3) Uani 1.00 1 d . . . C(4) C 0.548(1) 0.514(2) 0.366(2) 0.106(6) Uani 1.00 1 d . . . C(5) C 0.395(2) 0.673(2) 0.4612(11) 0.097(5) Uani 1.00 1 d . . . C(6) C 0.667(2) 0.584(2) 0.4904(10) 0.079(4) Uani 1.00 1 d . . . C(7) C 0.1690(11) 0.9330(9) -0.1979(8) 0.057(3) Uani 1.00 1 d . . . C(8) C 0.0294(9) 0.8800(8) -0.1683(6) 0.060(2) Uani 1.00 1 d . . . C(9) C -0.0558(9) 0.8897(9) -0.2600(7) 0.071(3) Uani 1.00 1 d . . . C(10) C -0.0541(13) 1.0290(10) -0.3269(10) 0.079(3) Uani 1.00 1 d . . . C(11) C 0.0886(10) 0.9724(9) -0.3726(7) 0.078(3) Uani 1.00 1 d . . . C(12) C 0.1992(11) 0.9776(9) -0.3017(8) 0.060(3) Uani 1.00 1 d . . . C(13) C 0.326(2) 1.026(1) -0.3315(11) 0.075(4) Uani 1.00 1 d . . . C(14) C 0.4112(13) 1.0361(13) -0.2586(10) 0.064(4) Uani 1.00 1 d . . . C(15) C 0.3802(12) 0.9919(11) -0.1594(10) 0.053(3) Uani 1.00 1 d . . . C(16) C 0.4717(13) 0.9992(11) -0.0826(9) 0.049(3) Uani 1.00 1 d . . . C(17) C 0.607(1) 1.037(1) -0.1058(10) 0.066(4) Uani 1.00 1 d . . . C(18) C 0.6885(13) 1.0348(11) -0.0272(10) 0.068(3) Uani 1.00 1 d . . . C(19) C 0.6451(10) 1.0008(8) 0.0700(7) 0.056(3) Uani 1.00 1 d . . . C(20) C 0.7310(9) 0.9958(9) 0.1573(7) 0.068(3) Uani 1.00 1 d . . . C(21) C 0.709(2) 0.866(2) 0.2362(11) 0.095(5) Uani 1.00 1 d . . . C(22) C 0.5758(12) 0.9436(12) 0.2683(7) 0.086(4) Uani 1.00 1 d . . . C(23) C 0.4581(10) 0.9354(11) 0.1996(7) 0.075(3) Uani 1.00 1 d . . . C(24) C 0.5069(11) 0.9683(10) 0.0929(8) 0.059(3) Uani 1.00 1 d . . . C(25) C 0.0329(13) 0.8338(11) -0.3437(8) 0.079(4) Uani 1.00 1 d . . . C(26) C -0.053(2) 0.8149(13) -0.4297(11) 0.110(5) Uani 1.00 1 d . . . C(27) C 0.141(2) 0.7154(13) -0.3161(13) 0.106(5) Uani 1.00 1 d . . . C(28) C 0.6462(11) 1.0713(13) 0.2310(9) 0.084(4) Uani 1.00 1 d . . . C(29) C 0.559(2) 1.200(2) 0.1861(13) 0.119(6) Uani 1.00 1 d . . . C(30) C 0.7369(13) 1.093(2) 0.3143(9) 0.130(6) Uani 1.00 1 d . . . C(31) C 0.2329(10) 0.3815(9) 0.4484(8) 0.051(2) Uani 1.00 1 d . . . C(32) C 0.2969(9) 0.3980(9) 0.3402(6) 0.058(2) Uani 1.00 1 d . . . C(33) C 0.2011(9) 0.3567(10) 0.2717(6) 0.072(3) Uani 1.00 1 d . . . C(34) C 0.154(1) 0.2238(13) 0.3254(11) 0.084(4) Uani 1.00 1 d . . . C(35) C 0.0321(9) 0.3100(9) 0.3782(7) 0.066(3) Uani 1.00 1 d . . . C(36) C 0.0981(9) 0.3391(8) 0.4662(7) 0.053(2) Uani 1.00 1 d . . . C(37) C 0.0333(12) 0.3275(10) 0.5632(9) 0.056(3) Uani 1.00 1 d . . . C(38) C 0.1108(12) 0.3488(11) 0.6363(9) 0.054(3) Uani 1.00 1 d . . . C(39) C 0.2457(11) 0.3861(10) 0.6136(9) 0.045(3) Uani 1.00 1 d . . . C(40) C 0.3279(12) 0.4063(10) 0.6958(8) 0.045(3) Uani 1.00 1 d . . . C(41) C 0.291(1) 0.3573(12) 0.7988(9) 0.062(4) Uani 1.00 1 d . . . C(42) C 0.3695(13) 0.3825(12) 0.8703(8) 0.063(3) Uani 1.00 1 d . . . C(43) C 0.4726(10) 0.4642(9) 0.8406(7) 0.054(3) Uani 1.00 1 d . . . C(44) C 0.5569(10) 0.5108(9) 0.9119(6) 0.071(3) Uani 1.00 1 d . . . C(45) C 0.557(2) 0.661(2) 0.8705(12) 0.111(6) Uani 1.00 1 d . . . C(46) C 0.6743(13) 0.6252(10) 0.8006(7) 0.096(4) Uani 1.00 1 d . . . C(47) C 0.6195(11) 0.5960(10) 0.7070(6) 0.079(3) Uani 1.00 1 d . . . C(48) C 0.5058(11) 0.5081(9) 0.7370(7) 0.055(3) Uani 1.00 1 d . . . C(49) C 0.0483(9) 0.4197(11) 0.2823(7) 0.066(3) Uani 1.00 1 d . . . C(50) C 0.019(2) 0.5578(13) 0.2960(11) 0.095(4) Uani 1.00 1 d . . . C(51) C -0.0394(11) 0.4086(12) 0.1963(8) 0.095(4) Uani 1.00 1 d . . . C(52) C 0.714(1) 0.4975(13) 0.8809(8) 0.085(4) Uani 1.00 1 d . . . C(53) C 0.782(2) 0.376(2) 0.849(1) 0.135(7) Uani 1.00 1 d . . . C(54) C 0.807(2) 0.518(1) 0.9620(11) 0.121(6) Uani 1.00 1 d . . . H(1) H 0.0468 0.7903 -0.1339 0.072 Uiso 1.00 1 c R . . H(2) H -0.0238 0.9290 -0.1245 0.072 Uiso 1.00 1 c R . . H(3) H -0.1466 0.8618 -0.2448 0.085 Uiso 1.00 1 c R . . H(4) H -0.1277 1.0572 -0.3728 0.095 Uiso 1.00 1 c R . . H(5) H -0.0481 1.0956 -0.2916 0.095 Uiso 1.00 1 c R . . H(6) H 0.1086 1.0067 -0.4425 0.094 Uiso 1.00 1 c R . . H(7) H 0.3540 1.0515 -0.4012 0.090 Uiso 1.00 1 c R . . H(8) H 0.4951 1.0758 -0.2787 0.076 Uiso 1.00 1 c R . . H(9) H 0.6413 1.0630 -0.1740 0.079 Uiso 1.00 1 c R . . H(10) H 0.7809 1.0589 -0.0428 0.081 Uiso 1.00 1 c R . . H(11) H 0.8259 1.0126 0.1414 0.081 Uiso 1.00 1 c R . . H(12) H 0.6955 0.7945 0.2085 0.113 Uiso 1.00 1 c R . . H(13) H 0.7777 0.8379 0.2858 0.113 Uiso 1.00 1 c R . . H(14) H 0.5514 0.9224 0.3387 0.103 Uiso 1.00 1 c R . . H(15) H 0.4333 0.8486 0.2160 0.090 Uiso 1.00 1 c R . . H(16) H 0.3779 0.9955 0.2106 0.090 Uiso 1.00 1 c R . . H(17) H -0.0830 0.7301 -0.4131 0.132 Uiso 1.00 1 c R . . H(18) H 0.0043 0.8238 -0.4907 0.132 Uiso 1.00 1 c R . . H(19) H -0.1328 0.8801 -0.4414 0.135 Uiso 1.00 1 c R . . H(20) H 0.2302 0.7425 -0.3112 0.128 Uiso 1.00 1 c R . . H(21) H 0.1487 0.6661 -0.3668 0.128 Uiso 1.00 1 c R . . H(22) H 0.1148 0.6602 -0.2536 0.129 Uiso 1.00 1 c R . . H(23) H 0.6108 1.2727 0.1766 0.142 Uiso 1.00 1 c R . . H(24) H 0.4791 1.2143 0.2302 0.142 Uiso 1.00 1 c R . . H(25) H 0.5316 1.1923 0.1225 0.155 Uiso 1.00 1 c R . . H(26) H 0.7350 1.0205 0.3707 0.156 Uiso 1.00 1 c R . . H(27) H 0.6987 1.1721 0.3343 0.156 Uiso 1.00 1 c R . . H(28) H 0.8315 1.0998 0.2890 0.171 Uiso 1.00 1 c R . . H(29) H 0.3094 0.4877 0.3140 0.069 Uiso 1.00 1 c R . . H(30) H 0.3858 0.3451 0.3409 0.069 Uiso 1.00 1 c R . . H(31) H 0.2374 0.3618 0.2040 0.086 Uiso 1.00 1 c R . . H(32) H 0.1216 0.1761 0.2825 0.100 Uiso 1.00 1 c R . . H(33) H 0.2189 0.1672 0.3699 0.100 Uiso 1.00 1 c R . . H(34) H -0.0570 0.2785 0.3917 0.079 Uiso 1.00 1 c R . . H(35) H -0.0602 0.3058 0.5776 0.067 Uiso 1.00 1 c R . . H(36) H 0.0722 0.3379 0.7038 0.065 Uiso 1.00 1 c R . . H(37) H 0.2141 0.3080 0.8183 0.074 Uiso 1.00 1 c R . . H(38) H 0.3526 0.3438 0.9399 0.076 Uiso 1.00 1 c R . . H(39) H 0.5330 0.4829 0.9820 0.085 Uiso 1.00 1 c R . . H(40) H 0.4732 0.7051 0.8387 0.133 Uiso 1.00 1 c R . . H(41) H 0.5803 0.7067 0.9176 0.133 Uiso 1.00 1 c R . . H(42) H 0.7440 0.6835 0.7864 0.116 Uiso 1.00 1 c R . . H(43) H 0.5823 0.6763 0.6640 0.095 Uiso 1.00 1 c R . . H(44) H 0.6951 0.5538 0.6720 0.095 Uiso 1.00 1 c R . . H(45) H 0.0139 0.5538 0.3666 0.114 Uiso 1.00 1 c R . . H(46) H -0.0680 0.5982 0.2674 0.114 Uiso 1.00 1 c R . . H(47) H 0.0928 0.6065 0.2643 0.105 Uiso 1.00 1 c R . . H(48) H -0.0335 0.4790 0.1386 0.114 Uiso 1.00 1 c R . . H(49) H -0.1358 0.4090 0.2191 0.114 Uiso 1.00 1 c R . . H(50) H -0.0041 0.3278 0.1783 0.115 Uiso 1.00 1 c R . . H(51) H 0.8165 0.3131 0.9062 0.162 Uiso 1.00 1 c R . . H(52) H 0.8583 0.3976 0.8011 0.162 Uiso 1.00 1 c R . . H(53) H 0.7172 0.3405 0.8173 0.166 Uiso 1.00 1 c R . . H(54) H 0.8204 0.6078 0.9501 0.146 Uiso 1.00 1 c R . . H(55) H 0.8957 0.4658 0.9594 0.146 Uiso 1.00 1 c R . . H(56) H 0.7665 0.4906 1.0285 0.152 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0466(3) 0.0496(3) 0.0539(3) -0.0155(2) 0.0094(2) -0.0032(2) Re(2) 0.0489(3) 0.0684(3) 0.0413(2) -0.0262(3) 0.0012(2) -0.0043(2) Br(1) 0.0744(9) 0.0524(6) 0.0905(9) -0.0107(6) 0.0252(7) -0.0084(6) Br(2) 0.0504(6) 0.0815(9) 0.0949(10) -0.0065(6) 0.0073(6) -0.0126(7) O(1) 0.059(5) 0.089(6) 0.097(7) -0.031(4) 0.015(5) -0.017(5) O(2) 0.125(8) 0.074(6) 0.108(7) -0.004(6) 0.039(6) 0.010(6) O(3) 0.087(7) 0.133(8) 0.069(7) -0.049(6) 0.016(5) -0.024(6) O(4) 0.093(7) 0.179(11) 0.059(6) -0.071(7) 0.024(5) -0.035(6) O(5) 0.123(9) 0.081(7) 0.133(10) 0.000(6) 0.021(7) 0.049(6) O(6) 0.118(8) 0.196(11) 0.063(6) -0.117(8) 0.002(5) -0.017(6) N(1) 0.051(5) 0.042(4) 0.054(5) -0.009(4) 0.007(4) -0.006(4) N(2) 0.041(4) 0.046(4) 0.058(5) -0.009(3) 0.015(4) -0.004(4) N(3) 0.050(5) 0.047(4) 0.047(4) -0.011(3) -0.002(4) -0.003(3) N(4) 0.059(5) 0.050(4) 0.045(4) -0.023(4) -0.007(4) 0.003(3) C(1) 0.048(6) 0.061(6) 0.066(7) -0.006(5) 0.016(5) 0.005(5) C(2) 0.069(6) 0.039(5) 0.060(6) -0.010(4) 0.022(5) 0.011(4) C(3) 0.064(6) 0.074(7) 0.023(3) -0.031(5) 0.017(3) 0.001(3) C(4) 0.048(7) 0.143(13) 0.15(2) -0.046(8) -0.005(8) -0.064(11) C(5) 0.108(11) 0.142(13) 0.045(6) -0.064(10) 0.001(6) -0.006(8) C(6) 0.093(10) 0.115(10) 0.044(6) -0.071(8) 0.001(6) -0.017(6) C(7) 0.057(5) 0.051(5) 0.063(5) -0.013(4) 0.004(4) -0.011(4) C(8) 0.062(5) 0.051(5) 0.069(5) -0.015(4) 0.001(4) -0.013(4) C(9) 0.063(5) 0.068(6) 0.080(6) -0.022(4) -0.017(4) -0.001(4) C(10) 0.072(7) 0.051(5) 0.104(8) -0.001(5) -0.034(6) 0.011(5) C(11) 0.086(7) 0.069(6) 0.069(5) -0.022(5) -0.019(5) 0.017(5) C(12) 0.065(6) 0.056(6) 0.053(4) -0.007(4) -0.004(4) 0.001(4) C(13) 0.083(9) 0.074(8) 0.060(8) -0.013(7) 0.004(7) -0.001(7) C(14) 0.051(7) 0.073(8) 0.060(8) -0.019(6) 0.008(6) 0.002(7) C(15) 0.040(6) 0.046(6) 0.069(8) -0.003(5) 0.008(6) -0.010(6) C(16) 0.053(6) 0.044(5) 0.046(5) -0.008(4) 0.016(4) -0.008(4) C(17) 0.055(7) 0.083(8) 0.061(7) -0.021(6) 0.013(5) -0.017(6) C(18) 0.050(5) 0.072(7) 0.070(6) -0.015(5) 0.012(5) 0.005(5) C(19) 0.051(5) 0.052(5) 0.064(5) -0.007(4) 0.003(4) -0.013(4) C(20) 0.051(5) 0.066(5) 0.083(6) -0.010(4) 0.000(4) -0.011(5) C(21) 0.097(9) 0.110(11) 0.070(7) -0.023(8) -0.018(7) 0.003(7) C(22) 0.075(7) 0.136(10) 0.054(5) -0.042(7) 0.006(5) -0.020(5) C(23) 0.054(5) 0.104(8) 0.068(5) -0.028(5) 0.009(4) -0.014(6) C(24) 0.057(6) 0.065(7) 0.051(5) -0.019(5) 0.005(4) -0.003(4) C(25) 0.105(9) 0.071(7) 0.066(6) -0.036(7) -0.009(5) -0.010(5) C(26) 0.132(12) 0.119(11) 0.087(8) -0.055(9) -0.029(8) -0.007(7) C(27) 0.16(1) 0.044(6) 0.119(12) -0.004(7) -0.011(10) -0.029(6) C(28) 0.069(6) 0.111(9) 0.085(7) -0.033(7) 0.010(5) -0.042(7) C(29) 0.118(12) 0.130(12) 0.140(13) -0.029(10) 0.027(9) -0.098(11) C(30) 0.108(9) 0.22(2) 0.099(9) -0.083(11) 0.009(7) -0.076(10) C(31) 0.039(4) 0.058(6) 0.052(4) -0.009(4) -0.006(3) -0.005(4) C(32) 0.051(5) 0.080(6) 0.044(4) -0.014(4) -0.001(3) -0.015(4) C(33) 0.061(5) 0.105(7) 0.060(5) -0.025(5) -0.001(4) -0.030(5) C(34) 0.079(8) 0.081(8) 0.098(8) -0.009(6) -0.011(6) -0.032(6) C(35) 0.056(5) 0.083(6) 0.065(5) -0.030(5) -0.009(4) -0.014(5) C(36) 0.045(5) 0.057(5) 0.058(4) -0.014(4) -0.011(4) -0.005(4) C(37) 0.044(5) 0.049(5) 0.070(6) -0.023(4) -0.008(4) 0.006(4) C(38) 0.051(6) 0.054(6) 0.046(5) -0.010(5) 0.014(4) 0.008(4) C(39) 0.034(5) 0.042(5) 0.055(6) -0.005(4) -0.006(4) -0.001(4) C(40) 0.058(7) 0.040(6) 0.035(5) -0.015(5) 0.002(5) 0.000(4) C(41) 0.074(8) 0.061(7) 0.047(7) -0.023(7) 0.008(6) 0.001(6) C(42) 0.072(7) 0.077(8) 0.037(6) -0.027(6) 0.010(5) 0.003(5) C(43) 0.061(5) 0.048(5) 0.054(4) -0.001(4) -0.006(4) -0.013(4) C(44) 0.090(7) 0.077(6) 0.047(4) -0.016(5) -0.009(4) -0.012(4) C(45) 0.17(2) 0.086(10) 0.096(10) -0.016(10) -0.047(10) -0.047(8) C(46) 0.149(10) 0.083(7) 0.068(6) -0.068(7) -0.023(6) -0.001(5) C(47) 0.105(8) 0.083(6) 0.053(4) -0.054(6) -0.014(5) 0.006(5) C(48) 0.068(6) 0.050(5) 0.046(4) -0.015(4) -0.001(4) -0.006(4) C(49) 0.050(5) 0.088(7) 0.063(5) -0.022(5) -0.008(4) -0.014(5) C(50) 0.092(9) 0.083(8) 0.087(9) 0.014(7) -0.017(7) 0.015(6) C(51) 0.071(6) 0.136(10) 0.079(6) -0.031(7) -0.020(5) -0.012(7) C(52) 0.099(9) 0.100(10) 0.061(6) -0.044(8) -0.023(6) -0.005(6) C(53) 0.073(9) 0.22(2) 0.125(13) -0.016(11) -0.009(8) -0.06(1) C(54) 0.141(13) 0.16(1) 0.082(8) -0.069(11) -0.046(8) -0.015(9) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998); CrystalStructure (Rigaku/MSC & Rigaku Corporation, 2003)' _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Re(1) Br(1) 2.626(2) ? . . Re(1) N(1) 2.26(1) ? . . Re(1) N(2) 2.23(1) ? . . Re(1) C(1) 1.87(1) ? . . Re(1) C(2) 1.917(8) ? . . Re(1) C(3) 1.940(8) ? . . Re(2) Br(2) 2.609(2) ? . . Re(2) N(3) 2.23(1) ? . . Re(2) N(4) 2.19(1) ? . . Re(2) C(4) 1.84(2) ? . . Re(2) C(5) 1.89(2) ? . . Re(2) C(6) 1.90(2) ? . . O(1) C(1) 1.18(2) ? . . O(2) C(2) 1.15(1) ? . . O(3) C(3) 1.12(1) ? . . O(4) C(4) 1.23(2) ? . . O(5) C(5) 1.15(2) ? . . O(6) C(6) 1.15(2) ? . . N(1) C(7) 1.33(2) ? . . N(1) C(15) 1.35(2) ? . . N(2) C(16) 1.41(2) ? . . N(2) C(24) 1.36(2) ? . . N(3) C(31) 1.34(2) ? . . N(3) C(39) 1.32(1) ? . . N(4) C(40) 1.39(2) ? . . N(4) C(48) 1.36(2) ? . . C(7) C(8) 1.51(1) ? . . C(7) C(12) 1.40(1) ? . . C(8) C(9) 1.52(1) ? . . C(8) H(1) 0.9500 ? . . C(8) H(2) 0.9500 ? . . C(9) C(10) 1.54(1) ? . . C(9) C(25) 1.54(2) ? . . C(9) H(3) 0.9500 ? . . C(10) C(11) 1.56(2) ? . . C(10) H(4) 0.9500 ? . . C(10) H(5) 0.9500 ? . . C(11) C(12) 1.51(2) ? . . C(11) C(25) 1.58(2) ? . . C(11) H(6) 0.9500 ? . . C(12) C(13) 1.38(2) ? . . C(13) C(14) 1.37(2) ? . . C(13) H(7) 0.9500 ? . . C(14) C(15) 1.34(2) ? . . C(14) H(8) 0.9500 ? . . C(15) C(16) 1.44(2) ? . . C(16) C(17) 1.40(2) ? . . C(17) C(18) 1.37(2) ? . . C(17) H(9) 0.9500 ? . . C(18) C(19) 1.34(2) ? . . C(18) H(10) 0.9500 ? . . C(19) C(20) 1.49(1) ? . . C(19) C(24) 1.41(1) ? . . C(20) C(21) 1.56(2) ? . . C(20) C(28) 1.54(2) ? . . C(20) H(11) 0.9500 ? . . C(21) C(22) 1.51(2) ? . . C(21) H(12) 0.9500 ? . . C(21) H(13) 0.9500 ? . . C(22) C(23) 1.55(2) ? . . C(22) C(28) 1.55(2) ? . . C(22) H(14) 0.9500 ? . . C(23) C(24) 1.47(1) ? . . C(23) H(15) 0.9500 ? . . C(23) H(16) 0.9500 ? . . C(25) C(26) 1.55(2) ? . . C(25) C(27) 1.50(2) ? . . C(26) H(17) 0.9500 ? . . C(26) H(18) 0.9500 ? . . C(26) H(19) 0.9500 ? . . C(27) H(20) 0.9500 ? . . C(27) H(21) 0.9500 ? . . C(27) H(22) 0.9500 ? . . C(28) C(29) 1.51(2) ? . . C(28) C(30) 1.56(2) ? . . C(29) H(23) 0.9500 ? . . C(29) H(24) 0.9500 ? . . C(29) H(25) 0.9501 ? . . C(30) H(26) 0.9499 ? . . C(30) H(27) 0.9500 ? . . C(30) H(28) 0.9500 ? . . C(31) C(32) 1.53(1) ? . . C(31) C(36) 1.41(1) ? . . C(32) C(33) 1.53(1) ? . . C(32) H(29) 0.9500 ? . . C(32) H(30) 0.9500 ? . . C(33) C(34) 1.53(2) ? . . C(33) C(49) 1.53(1) ? . . C(33) H(31) 0.9500 ? . . C(34) C(35) 1.60(2) ? . . C(34) H(32) 0.9500 ? . . C(34) H(33) 0.9500 ? . . C(35) C(36) 1.51(1) ? . . C(35) C(49) 1.54(1) ? . . C(35) H(34) 0.9500 ? . . C(36) C(37) 1.40(1) ? . . C(37) C(38) 1.37(2) ? . . C(37) H(35) 0.9500 ? . . C(38) C(39) 1.40(2) ? . . C(38) H(36) 0.9500 ? . . C(39) C(40) 1.49(2) ? . . C(40) C(41) 1.41(1) ? . . C(41) C(42) 1.37(2) ? . . C(41) H(37) 0.9500 ? . . C(42) C(43) 1.38(2) ? . . C(42) H(38) 0.9500 ? . . C(43) C(44) 1.52(2) ? . . C(43) C(48) 1.40(1) ? . . C(44) C(45) 1.55(2) ? . . C(44) C(52) 1.53(2) ? . . C(44) H(39) 0.9500 ? . . C(45) C(46) 1.48(2) ? . . C(45) H(40) 0.9500 ? . . C(45) H(41) 0.9500 ? . . C(46) C(47) 1.53(2) ? . . C(46) C(52) 1.54(1) ? . . C(46) H(42) 0.9500 ? . . C(47) C(48) 1.50(2) ? . . C(47) H(43) 0.9500 ? . . C(47) H(44) 0.9500 ? . . C(49) C(50) 1.50(2) ? . . C(49) C(51) 1.53(2) ? . . C(50) H(45) 0.9502 ? . . C(50) H(46) 0.9500 ? . . C(50) H(47) 0.9500 ? . . C(51) H(48) 0.9500 ? . . C(51) H(49) 0.9500 ? . . C(51) H(50) 0.9500 ? . . C(52) C(53) 1.49(2) ? . . C(52) C(54) 1.54(2) ? . . C(53) H(51) 0.9500 ? . . C(53) H(52) 0.9500 ? . . C(53) H(53) 0.9499 ? . . C(54) H(54) 0.9500 ? . . C(54) H(55) 0.9500 ? . . C(54) H(56) 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_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Re(1) Br(1) 82.4(2) ? . . . N(2) Re(1) Br(1) 88.5(2) ? . . . C(1) Re(1) Br(1) 95.1(4) ? . . . C(2) Re(1) Br(1) 178.0(3) ? . . . C(3) Re(1) Br(1) 88.2(3) ? . . . N(2) Re(1) N(1) 75.2(4) ? . . . C(1) Re(1) N(1) 102.5(5) ? . . . C(2) Re(1) N(1) 96.9(4) ? . . . C(3) Re(1) N(1) 170.5(4) ? . . . Re(1) N(1) C(7) 124.0(7) ? . . . Re(1) N(1) C(15) 114.3(9) ? . . . C(1) Re(1) N(2) 175.4(5) ? . . . C(2) Re(1) N(2) 89.5(4) ? . . . C(3) Re(1) N(2) 102.8(5) ? . . . Re(1) N(2) C(16) 114.1(8) ? . . . Re(1) N(2) C(24) 127.1(7) ? . . . Re(1) C(1) O(1) 177.2(9) ? . . . C(2) Re(1) C(1) 86.9(5) ? . . . C(3) Re(1) C(1) 80.1(5) ? . . . Re(1) C(2) O(2) 171(1) ? . . . C(3) Re(1) C(2) 92.4(5) ? . . . Re(1) C(3) O(3) 176(1) ? . . . N(3) Re(2) Br(2) 85.3(2) ? . . . N(4) Re(2) Br(2) 83.1(2) ? . . . C(4) Re(2) Br(2) 93.0(5) ? . . . C(5) Re(2) Br(2) 177.2(6) ? . . . C(6) Re(2) Br(2) 93.3(4) ? . . . N(4) Re(2) N(3) 76.0(4) ? . . . C(4) Re(2) N(3) 102.0(6) ? . . . C(5) Re(2) N(3) 91.9(6) ? . . . C(6) Re(2) N(3) 177.2(5) ? . . . Re(2) N(3) C(39) 114.5(8) ? . . . Re(2) N(3) C(31) 127.2(7) ? . . . C(4) Re(2) N(4) 175.7(6) ? . . . C(5) Re(2) N(4) 96.1(5) ? . . . C(6) Re(2) N(4) 101.5(5) ? . . . Re(2) N(4) C(40) 114.8(8) ? . . . Re(2) N(4) C(48) 130.2(8) ? . . . Re(2) C(4) O(4) 173(1) ? . . . C(5) Re(2) C(4) 87.7(7) ? . . . C(6) Re(2) C(4) 80.5(7) ? . . . Re(2) C(5) O(5) 172(1) ? . . . C(6) Re(2) C(5) 89.5(7) ? . . . Re(2) C(6) O(6) 175(1) ? . . . N(1) C(7) C(8) 122.8(9) ? . . . N(1) C(7) C(12) 120(1) ? . . . C(15) N(1) C(7) 121(1) ? . . . N(1) C(15) C(14) 119(1) ? . . . N(1) C(15) C(16) 118(1) ? . . . N(2) C(16) C(15) 117(1) ? . . . N(2) C(16) C(17) 120(1) ? . . . C(24) N(2) C(16) 118(1) ? . . . N(2) C(24) C(19) 121.4(9) ? . . . N(2) C(24) C(23) 120.6(9) ? . . . C(39) N(3) C(31) 117(1) ? . . . N(3) C(31) C(32) 120.4(9) ? . . . N(3) C(31) C(36) 123.0(9) ? . . . N(3) C(39) C(40) 118(1) ? . . . N(3) C(39) C(38) 122(1) ? . . . N(4) C(40) C(39) 114.7(9) ? . . . N(4) C(40) C(41) 123(1) ? . . . C(48) N(4) C(40) 114.6(9) ? . . . N(4) C(48) C(43) 124(1) ? . . . N(4) C(48) C(47) 118.0(8) ? . . . C(7) C(8) H(1) 108.8339 ? . . . C(7) C(8) H(2) 108.8338 ? . . . C(12) C(7) C(8) 116(1) ? . . . C(7) C(8) C(9) 112.0(7) ? . . . C(7) C(12) C(13) 117(1) ? . . . C(7) C(12) C(11) 117.3(9) ? . . . H(1) C(8) C(9) 108.8346 ? . . . H(2) C(8) C(9) 108.8344 ? . . . C(8) C(9) C(10) 107.7(9) ? . . . C(8) C(9) C(25) 112.0(8) ? . . . C(8) C(9) H(3) 115.0020 ? . . . H(2) C(8) H(1) 109.4598 ? . . . C(9) C(10) C(11) 85.3(7) ? . . . C(25) C(9) C(10) 89.3(8) ? . . . C(9) C(10) H(5) 115.1240 ? . . . H(3) C(9) C(10) 115.0023 ? . . . C(9) C(10) H(4) 115.1242 ? . . . C(9) C(25) C(11) 84.4(8) ? . . . C(9) C(25) C(27) 120(1) ? . . . H(3) C(9) C(25) 115.0023 ? . . . C(9) C(25) C(26) 114(1) ? . . . C(10) C(11) C(12) 106.1(9) ? . . . C(10) C(11) C(25) 87.4(8) ? . . . H(5) C(10) C(11) 115.1242 ? . . . H(4) C(10) C(11) 115.1242 ? . . . C(10) C(11) H(6) 116.3945 ? . . . H(5) C(10) H(4) 109.4602 ? . . . C(11) C(12) C(13) 124(1) ? . . . C(25) C(11) C(12) 110.3(8) ? . . . H(6) C(11) C(12) 116.3941 ? . . . C(11) C(25) C(27) 116(1) ? . . . C(11) C(25) C(26) 110.7(8) ? . . . H(6) C(11) C(25) 116.3942 ? . . . C(12) C(13) C(14) 118(1) ? . . . C(12) C(13) H(7) 120.7366 ? . . . C(13) C(14) C(15) 122(1) ? . . . H(7) C(13) C(14) 120.7366 ? . . . C(13) C(14) H(8) 118.8617 ? . . . C(14) C(15) C(16) 122(1) ? . . . H(8) C(14) C(15) 118.8616 ? . . . C(15) C(16) C(17) 122(1) ? . . . C(16) C(17) C(18) 118(1) ? . . . C(16) C(17) H(9) 120.9546 ? . . . C(17) C(18) C(19) 123(1) ? . . . H(9) C(17) C(18) 120.9547 ? . . . C(17) C(18) H(10) 118.2277 ? . . . C(18) C(19) C(24) 118(1) ? . . . H(10) C(18) C(19) 118.2274 ? . . . C(18) C(19) C(20) 125.1(9) ? . . . C(24) C(19) C(20) 116.7(8) ? . . . C(19) C(20) H(11) 116.1517 ? . . . C(19) C(20) C(21) 106.9(9) ? . . . C(19) C(20) C(28) 110.0(7) ? . . . C(19) C(24) C(23) 117(1) ? . . . C(20) C(21) H(12) 115.2072 ? . . . C(20) C(21) H(13) 115.2068 ? . . . H(11) C(20) C(21) 116.1513 ? . . . C(20) C(21) C(22) 85.0(9) ? . . . C(28) C(20) C(21) 87.9(9) ? . . . H(11) C(20) C(28) 116.1511 ? . . . C(20) C(28) C(22) 84.1(9) ? . . . C(20) C(28) C(29) 117(1) ? . . . C(20) C(28) C(30) 113.3(9) ? . . . H(12) C(21) C(22) 115.2069 ? . . . C(21) C(22) H(14) 114.8078 ? . . . H(13) C(21) C(22) 115.2068 ? . . . C(21) C(22) C(23) 107(1) ? . . . C(21) C(22) C(28) 89.2(9) ? . . . H(13) C(21) H(12) 109.4605 ? . . . C(22) C(23) H(15) 109.2332 ? . . . C(22) C(23) H(16) 109.2335 ? . . . H(14) C(22) C(23) 114.8076 ? . . . C(22) C(23) C(24) 110.4(8) ? . . . C(28) C(22) C(23) 112.5(8) ? . . . H(14) C(22) C(28) 114.8082 ? . . . C(22) C(28) C(29) 120(1) ? . . . C(22) C(28) C(30) 111.0(9) ? . . . H(15) C(23) C(24) 109.2334 ? . . . H(16) C(23) C(24) 109.2334 ? . . . H(16) C(23) H(15) 109.4601 ? . . . C(27) C(25) C(26) 108(1) ? . . . C(25) C(26) H(17) 110.3602 ? . . . C(25) C(26) H(19) 110.8754 ? . . . C(25) C(26) H(18) 109.4702 ? . . . C(25) C(27) H(20) 109.7925 ? . . . C(25) C(27) H(22) 110.7460 ? . . . C(25) C(27) H(21) 109.4698 ? . . . H(19) C(26) H(17) 109.4733 ? . . . H(18) C(26) H(17) 109.0255 ? . . . H(19) C(26) H(18) 107.5740 ? . . . H(22) C(27) H(20) 109.4756 ? . . . H(21) C(27) H(20) 109.3112 ? . . . H(22) C(27) H(21) 108.0118 ? . . . C(28) C(29) H(25) 106.3828 ? . . . C(30) C(28) C(29) 108(1) ? . . . C(28) C(29) H(23) 112.1022 ? . . . C(28) C(29) H(24) 109.4701 ? . . . C(28) C(30) H(26) 108.5687 ? . . . C(28) C(30) H(28) 110.2263 ? . . . C(28) C(30) H(27) 109.4702 ? . . . H(25) C(29) H(23) 109.4791 ? . . . H(24) C(29) H(23) 108.1406 ? . . . H(25) C(29) H(24) 111.2960 ? . . . H(28) C(30) H(26) 109.4792 ? . . . H(27) C(30) H(26) 109.9210 ? . . . H(28) C(30) H(27) 109.1643 ? . . . C(31) C(32) H(29) 109.0243 ? . . . C(31) C(32) H(30) 109.0248 ? . . . C(36) C(31) C(32) 116.6(9) ? . . . C(31) C(32) C(33) 111.3(7) ? . . . C(31) C(36) C(37) 118(1) ? . . . C(31) C(36) C(35) 117.5(8) ? . . . H(29) C(32) C(33) 109.0249 ? . . . C(32) C(33) H(31) 114.9016 ? . . . H(30) C(32) C(33) 109.0244 ? . . . C(32) C(33) C(34) 109.1(8) ? . . . C(32) C(33) C(49) 111.7(8) ? . . . H(30) C(32) H(29) 109.4600 ? . . . H(31) C(33) C(34) 114.9012 ? . . . C(33) C(34) C(35) 84.8(8) ? . . . C(49) C(33) C(34) 88.4(8) ? . . . C(33) C(34) H(33) 115.2304 ? . . . C(33) C(34) H(32) 115.2303 ? . . . H(31) C(33) C(49) 114.9014 ? . . . C(33) C(49) C(35) 87.1(6) ? . . . C(33) C(49) C(50) 119(1) ? . . . C(33) C(49) C(51) 111.9(8) ? . . . C(34) C(35) C(36) 105.9(8) ? . . . C(34) C(35) C(49) 85.6(7) ? . . . H(33) C(34) C(35) 115.2302 ? . . . H(32) C(34) C(35) 115.2304 ? . . . C(34) C(35) H(34) 116.7453 ? . . . H(33) C(34) H(32) 109.4600 ? . . . C(35) C(36) C(37) 124.0(9) ? . . . C(49) C(35) C(36) 110.7(8) ? . . . H(34) C(35) C(36) 116.7449 ? . . . C(35) C(49) C(50) 116.2(9) ? . . . C(35) C(49) C(51) 112.8(9) ? . . . H(34) C(35) C(49) 116.7451 ? . . . C(36) C(37) C(38) 116(1) ? . . . C(36) C(37) H(35) 121.5911 ? . . . C(37) C(38) C(39) 121(1) ? . . . H(35) C(37) C(38) 121.5915 ? . . . C(37) C(38) H(36) 119.3737 ? . . . C(38) C(39) C(40) 119(1) ? . . . H(36) C(38) C(39) 119.3734 ? . . . C(39) C(40) C(41) 121(1) ? . . . C(40) C(41) C(42) 118(1) ? . . . C(40) C(41) H(37) 120.7168 ? . . . C(41) C(42) C(43) 119(1) ? . . . H(37) C(41) C(42) 120.7163 ? . . . C(41) C(42) H(38) 120.2052 ? . . . C(42) C(43) C(48) 118(1) ? . . . H(38) C(42) C(43) 120.2054 ? . . . C(42) C(43) C(44) 125.1(9) ? . . . C(48) C(43) C(44) 116.0(9) ? . . . C(43) C(44) H(39) 116.1993 ? . . . C(43) C(44) C(45) 106.5(9) ? . . . C(43) C(44) C(52) 111.3(8) ? . . . C(43) C(48) C(47) 117.7(9) ? . . . H(39) C(44) C(45) 116.1999 ? . . . C(44) C(45) C(46) 86(1) ? . . . C(52) C(44) C(45) 86(1) ? . . . C(44) C(45) H(40) 114.9774 ? . . . C(44) C(45) H(41) 114.9773 ? . . . H(39) C(44) C(52) 116.1998 ? . . . C(44) C(52) C(46) 84.5(8) ? . . . C(44) C(52) C(53) 119(1) ? . . . C(44) C(52) C(54) 112(1) ? . . . C(45) C(46) C(47) 111(1) ? . . . C(45) C(46) C(52) 88.4(9) ? . . . H(40) C(45) C(46) 114.9768 ? . . . H(41) C(45) C(46) 114.9770 ? . . . C(45) C(46) H(42) 114.4340 ? . . . H(41) C(45) H(40) 109.4599 ? . . . C(46) C(47) H(43) 109.2382 ? . . . C(46) C(47) H(44) 109.2387 ? . . . C(46) C(47) C(48) 110.4(8) ? . . . C(52) C(46) C(47) 111(1) ? . . . H(42) C(46) C(47) 114.4334 ? . . . C(46) C(52) C(53) 119(1) ? . . . C(46) C(52) C(54) 112(1) ? . . . H(42) C(46) C(52) 114.4338 ? . . . H(43) C(47) C(48) 109.2382 ? . . . H(44) C(47) C(48) 109.2382 ? . . . H(44) C(47) H(43) 109.4603 ? . . . C(49) C(50) H(46) 109.4699 ? . . . C(49) C(50) H(47) 110.1272 ? . . . C(49) C(50) H(45) 107.5092 ? . . . C(51) C(49) C(50) 108.1(9) ? . . . C(49) C(51) H(48) 112.6354 ? . . . C(49) C(51) H(50) 106.9174 ? . . . C(49) C(51) H(49) 109.4704 ? . . . H(46) C(50) H(45) 110.4439 ? . . . H(47) C(50) H(45) 109.4597 ? . . . H(47) C(50) H(46) 109.8008 ? . . . H(50) C(51) H(48) 109.4752 ? . . . H(49) C(51) H(48) 107.8674 ? . . . H(50) C(51) H(49) 110.4897 ? . . . C(52) C(53) H(53) 111.0430 ? . . . C(54) C(52) C(53) 106(1) ? . . . C(52) C(53) H(51) 109.1269 ? . . . C(52) C(53) H(52) 109.4700 ? . . . C(52) C(54) H(54) 110.0696 ? . . . C(52) C(54) H(56) 111.9748 ? . . . C(52) C(54) H(55) 109.4699 ? . . . H(53) C(53) H(51) 109.4680 ? . . . H(52) C(53) H(51) 109.6438 ? . . . H(53) C(53) H(52) 108.0708 ? . . . H(56) C(54) H(54) 109.4758 ? . . . H(55) C(54) H(54) 109.1717 ? . . . H(56) C(54) H(55) 106.5885 ? . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Re(1) Re(2) 7.185(2) ? . . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(41) H(37) Br(1) 1_546 0.95 2.91 3.677(12) 139 ? #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================