# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? # 1. SUBMISSION DETAILS _publ_contact_author ; Ulrich Abram Free University of Berlin Institute of Chemistry Fabeckstrasse 34-36 D-14195 Berlin Germany ; _publ_contact_author_phone '0049 (0)30 838 54002' _publ_contact_author_fax '0049 (0)30 838 52676' _publ_contact_author_email abram@chemie.fu-berlin.de _publ_requested_journal 'Chem. Commun.' #============================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; Stable Nitridorhenium(V) Complexes With An N-Heterocyclic Carbene ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address "Braband, Henrik'" ; Free University of Berlin Institute of Chemistry Fabeckstrasse 34-36 D-14195 Berlin Germany ; 'Abram, Ulrich' ; Free University of Berlin Institute of Chemistry Fabeckstrasse 34-36 D-14195 Berlin Germany ; #=============== STRUCTURE I ============================ data_rencarbenep2cl _database_code_CSD 213784 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(dimethylphenylphosphine)(1,3,4-triphenyl-1,2,4-triazol-5-ylidene) nitridorhenium(V) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 Cl2 N4 P2 Re' _chemical_formula_weight 844.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 10.825(2) _cell_length_b 31.595(3) _cell_length_c 11.319(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.48(1) _cell_angle_gamma 90.00 _cell_volume 3550.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.03 _cell_measurement_theta_max 11.55 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.694 _exptl_absorpt_correction_type Psi-Scans _exptl_absorpt_correction_T_min 0.8321 _exptl_absorpt_correction_T_max 0.9772 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CAD4 ENRAF NONIUS' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 3600 _diffrn_standards_interval_time 500 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6427 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_sigmaI/netI 0.1783 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5500 _reflns_number_gt 2836 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction HELENA _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0574P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5500 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.003 _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 Re1 Re 0.66038(5) 0.117751(18) 0.36491(6) 0.0481(2) Uani 1 1 d . . . N10 N 0.7529(9) 0.1596(3) 0.4773(13) 0.076(4) Uani 1 1 d . . . Cl1 Cl 0.7758(4) 0.10599(16) 0.2207(4) 0.0939(16) Uani 1 1 d . . . Cl2 Cl 0.5217(4) 0.05106(12) 0.2823(4) 0.0786(12) Uani 1 1 d . . . C1 C 0.5331(13) 0.1567(4) 0.2053(13) 0.045(3) Uani 1 1 d . . . C2 C 0.3795(13) 0.1851(4) 0.0211(13) 0.048(3) Uani 1 1 d . . . N1 N 0.4346(10) 0.1472(3) 0.0835(10) 0.048(3) Uani 1 1 d . . . N2 N 0.5295(10) 0.1996(4) 0.2041(11) 0.053(3) Uani 1 1 d . . . N3 N 0.4333(10) 0.2178(3) 0.0924(11) 0.053(3) Uani 1 1 d . . . C11 C 0.3938(13) 0.1058(4) 0.0177(13) 0.050(4) Uani 1 1 d . . . C12 C 0.2718(14) 0.0925(5) -0.0016(15) 0.067(4) Uani 1 1 d . . . H12 H 0.2165 0.1070 0.0299 0.080 Uiso 1 1 calc R . . C13 C 0.2322(19) 0.0561(6) -0.0707(17) 0.085(6) Uani 1 1 d . . . H13 H 0.1460 0.0463 -0.0864 0.102 Uiso 1 1 calc R . . C14 C 0.305(3) 0.0332(6) -0.1179(18) 0.112(9) Uani 1 1 d . . . H14 H 0.2721 0.0085 -0.1643 0.134 Uiso 1 1 calc R . . C15 C 0.425(2) 0.0475(7) -0.0951(18) 0.104(7) Uani 1 1 d . . . H15 H 0.4800 0.0324 -0.1258 0.125 Uiso 1 1 calc R . . C16 C 0.4759(16) 0.0859(5) -0.0239(15) 0.066(4) Uani 1 1 d . . . H16 H 0.5616 0.0961 -0.0082 0.079 Uiso 1 1 calc R . . C21 C 0.6176(14) 0.2295(5) 0.2953(13) 0.053(4) Uani 1 1 d . . . C22 C 0.7420(15) 0.2314(5) 0.3056(15) 0.070(4) Uani 1 1 d . . . H22 H 0.7758 0.2139 0.2594 0.084 Uiso 1 1 calc R . . C23 C 0.8219(15) 0.2629(6) 0.3951(17) 0.078(5) Uani 1 1 d . . . H23 H 0.9131 0.2643 0.4119 0.094 Uiso 1 1 calc R . . C24 C 0.773(2) 0.2907(5) 0.4563(18) 0.090(6) Uani 1 1 d . . . H24 H 0.8301 0.3110 0.5101 0.108 Uiso 1 1 calc R . . C25 C 0.6488(18) 0.2896(5) 0.4419(18) 0.087(6) Uani 1 1 d . . . H25 H 0.6137 0.3081 0.4845 0.104 Uiso 1 1 calc R . . C26 C 0.5703(15) 0.2582(5) 0.3563(14) 0.062(4) Uani 1 1 d . . . H26 H 0.4792 0.2570 0.3406 0.075 Uiso 1 1 calc R . . C31 C 0.2745(14) 0.1860(4) -0.1155(15) 0.056(4) Uani 1 1 d . . . C32 C 0.1569(18) 0.2026(5) -0.1359(17) 0.079(5) Uani 1 1 d . . . H32 H 0.1377 0.2122 -0.0674 0.095 Uiso 1 1 calc R . . C33 C 0.0566(17) 0.2058(6) -0.268(2) 0.097(6) Uani 1 1 d . . . H33 H -0.0275 0.2173 -0.2830 0.117 Uiso 1 1 calc R . . C34 C 0.085(2) 0.1918(6) -0.372(2) 0.098(6) Uani 1 1 d . . . H34 H 0.0196 0.1949 -0.4555 0.117 Uiso 1 1 calc R . . C35 C 0.1999(17) 0.1747(6) -0.3555(17) 0.088(6) Uani 1 1 d . . . H35 H 0.2185 0.1642 -0.4234 0.105 Uiso 1 1 calc R . . C36 C 0.2947(15) 0.1732(5) -0.2260(15) 0.075(5) Uani 1 1 d . . . H36 H 0.3796 0.1627 -0.2122 0.090 Uiso 1 1 calc R . . P1 P 0.8207(4) 0.06852(13) 0.5183(4) 0.0576(11) Uani 1 1 d . . . C41 C 0.8298(14) 0.0623(5) 0.6867(15) 0.058(4) Uani 1 1 d . . . C42 C 0.8648(16) 0.0955(5) 0.7762(17) 0.084(6) Uani 1 1 d . . . H42 H 0.8881 0.1218 0.7544 0.101 Uiso 1 1 calc R . . C43 C 0.8646(19) 0.0886(8) 0.9062(19) 0.107(7) Uani 1 1 d . . . H43 H 0.8920 0.1103 0.9669 0.129 Uiso 1 1 calc R . . C44 C 0.825(3) 0.0509(9) 0.937(2) 0.127(9) Uani 1 1 d . . . H44 H 0.8204 0.0463 1.0161 0.152 Uiso 1 1 calc R . . C45 C 0.791(3) 0.0206(9) 0.846(3) 0.169(12) Uani 1 1 d . . . H45 H 0.7662 -0.0057 0.8655 0.203 Uiso 1 1 calc R . . C46 C 0.792(2) 0.0261(7) 0.725(2) 0.109(7) Uani 1 1 d . . . H46 H 0.7653 0.0036 0.6673 0.131 Uiso 1 1 calc R . . C47 C 0.9831(14) 0.0852(5) 0.5482(17) 0.098(6) Uani 1 1 d . . . H47A H 0.9959 0.1134 0.5820 0.147 Uiso 1 1 calc R . . H47B H 0.9967 0.0847 0.4694 0.147 Uiso 1 1 calc R . . H47C H 1.0467 0.0666 0.6096 0.147 Uiso 1 1 calc R . . C48 C 0.8173(16) 0.0157(4) 0.4575(16) 0.090(6) Uani 1 1 d . . . H48A H 0.7304 0.0033 0.4382 0.135 Uiso 1 1 calc R . . H48B H 0.8852 -0.0012 0.5213 0.135 Uiso 1 1 calc R . . H48C H 0.8345 0.0167 0.3807 0.135 Uiso 1 1 calc R . . P2 P 0.5185(4) 0.12142(15) 0.4818(4) 0.0605(10) Uani 1 1 d . . . C51 C 0.3492(13) 0.1318(4) 0.3775(13) 0.052(4) Uani 1 1 d . . . C52 C 0.3108(15) 0.1742(5) 0.3438(17) 0.080(5) Uani 1 1 d . . . H52 H 0.3738 0.1960 0.3721 0.096 Uiso 1 1 calc R . . C53 C 0.179(2) 0.1826(7) 0.269(2) 0.114(8) Uani 1 1 d . . . H53 H 0.1504 0.2100 0.2416 0.137 Uiso 1 1 calc R . . C54 C 0.094(2) 0.1499(10) 0.237(2) 0.124(10) Uani 1 1 d . . . H54 H 0.0022 0.1552 0.1929 0.149 Uiso 1 1 calc R . . C55 C 0.134(2) 0.1113(9) 0.264(2) 0.137(10) Uani 1 1 d . . . H55 H 0.0716 0.0895 0.2320 0.164 Uiso 1 1 calc R . . C56 C 0.2598(16) 0.1015(5) 0.3366(17) 0.079(5) Uani 1 1 d . . . H56 H 0.2848 0.0735 0.3583 0.095 Uiso 1 1 calc R . . C57 C 0.5089(16) 0.0781(6) 0.5836(17) 0.110(7) Uani 1 1 d . . . H57A H 0.5980 0.0709 0.6436 0.165 Uiso 1 1 calc R . . H57B H 0.4681 0.0540 0.5310 0.165 Uiso 1 1 calc R . . H57C H 0.4556 0.0867 0.6299 0.165 Uiso 1 1 calc R . . C58 C 0.5617(15) 0.1653(6) 0.6015(17) 0.117(8) Uani 1 1 d . . . H58A H 0.6532 0.1621 0.6624 0.176 Uiso 1 1 calc R . . H58B H 0.5026 0.1644 0.6460 0.176 Uiso 1 1 calc R . . H58C H 0.5517 0.1919 0.5578 0.176 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 Re1 0.0425(3) 0.0483(3) 0.0536(3) 0.0050(4) 0.0191(2) 0.0089(4) N10 0.016(5) 0.048(8) 0.125(11) 0.042(8) -0.013(6) -0.005(5) Cl1 0.067(3) 0.148(5) 0.085(3) 0.007(3) 0.050(2) 0.021(3) Cl2 0.078(3) 0.058(3) 0.085(3) -0.005(2) 0.017(2) 0.003(2) C1 0.050(8) 0.038(8) 0.058(9) -0.006(7) 0.034(8) -0.001(6) C2 0.049(8) 0.047(9) 0.044(9) 0.012(8) 0.014(7) 0.016(7) N1 0.040(6) 0.057(8) 0.040(7) -0.001(6) 0.009(6) 0.005(6) N2 0.037(6) 0.057(8) 0.054(8) -0.003(7) 0.006(6) -0.003(6) N3 0.048(7) 0.042(7) 0.055(8) 0.001(6) 0.008(6) 0.001(6) C11 0.049(8) 0.051(10) 0.045(8) -0.017(7) 0.016(7) -0.016(7) C12 0.048(9) 0.058(10) 0.081(12) -0.007(9) 0.013(9) 0.002(8) C13 0.091(14) 0.076(14) 0.067(13) 0.003(11) 0.009(11) -0.028(12) C14 0.17(2) 0.060(14) 0.055(13) -0.029(10) -0.013(15) -0.015(15) C15 0.127(19) 0.113(19) 0.057(13) -0.016(12) 0.021(14) 0.047(15) C16 0.080(12) 0.061(11) 0.060(11) 0.002(9) 0.033(10) 0.015(9) C21 0.056(9) 0.057(10) 0.055(9) 0.006(8) 0.032(8) -0.004(8) C22 0.064(11) 0.064(11) 0.076(12) -0.003(9) 0.021(9) -0.018(9) C23 0.045(10) 0.084(14) 0.096(14) 0.026(12) 0.018(10) -0.011(10) C24 0.102(16) 0.059(12) 0.108(16) -0.008(11) 0.040(13) -0.021(11) C25 0.073(12) 0.077(13) 0.115(16) 0.002(11) 0.042(12) -0.023(10) C26 0.057(10) 0.058(10) 0.066(10) -0.001(9) 0.019(9) -0.012(8) C31 0.042(8) 0.047(9) 0.064(11) 0.014(8) 0.006(8) 0.001(7) C32 0.074(11) 0.083(12) 0.067(11) -0.006(11) 0.014(9) 0.016(11) C33 0.062(11) 0.095(15) 0.106(16) 0.016(13) 0.004(12) 0.039(10) C34 0.075(14) 0.102(16) 0.098(16) -0.002(13) 0.016(13) -0.021(12) C35 0.054(11) 0.132(17) 0.071(13) -0.010(12) 0.018(10) -0.020(11) C36 0.050(9) 0.108(14) 0.058(11) 0.002(10) 0.014(9) -0.013(9) P1 0.051(2) 0.052(3) 0.061(3) 0.004(2) 0.013(2) 0.0134(19) C41 0.057(9) 0.049(10) 0.072(11) 0.008(9) 0.029(9) 0.006(8) C42 0.084(12) 0.058(11) 0.067(13) 0.006(10) -0.015(10) 0.026(9) C43 0.100(15) 0.122(19) 0.065(14) -0.022(13) -0.005(12) 0.049(14) C44 0.18(2) 0.11(2) 0.10(2) 0.060(17) 0.066(19) 0.056(19) C45 0.22(3) 0.11(2) 0.15(3) 0.02(2) 0.05(3) 0.02(2) C46 0.148(19) 0.098(18) 0.084(16) 0.028(13) 0.048(15) 0.025(14) C47 0.046(9) 0.121(15) 0.129(16) 0.042(13) 0.038(10) 0.025(10) C48 0.104(13) 0.060(11) 0.099(14) -0.015(10) 0.035(11) 0.029(10) P2 0.050(2) 0.075(3) 0.060(2) 0.010(3) 0.0245(19) 0.012(2) C51 0.045(8) 0.053(10) 0.069(10) 0.001(8) 0.033(8) 0.010(7) C52 0.049(10) 0.076(12) 0.113(15) 0.014(11) 0.029(10) 0.007(9) C53 0.105(17) 0.088(16) 0.14(2) 0.051(15) 0.041(16) 0.062(13) C54 0.053(13) 0.16(3) 0.14(2) 0.00(2) 0.015(13) 0.028(16) C55 0.065(16) 0.18(3) 0.15(2) -0.06(2) 0.031(15) -0.043(16) C56 0.053(10) 0.052(10) 0.107(14) -0.012(9) 0.006(10) -0.019(8) C57 0.073(12) 0.160(19) 0.102(15) 0.078(14) 0.041(11) 0.031(12) C58 0.056(11) 0.18(2) 0.104(15) -0.079(15) 0.016(11) 0.006(12) _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 Re1 N10 1.831(12) . ? Re1 C1 2.167(14) . ? Re1 P2 2.396(4) . ? Re1 Cl1 2.448(4) . ? Re1 P1 2.459(4) . ? Re1 Cl2 2.540(4) . ? C1 N2 1.356(15) . ? C1 N1 1.400(15) . ? C2 N3 1.298(15) . ? C2 N1 1.397(15) . ? C2 C31 1.510(18) . ? N1 C11 1.482(15) . ? N2 N3 1.401(13) . ? N2 C21 1.443(16) . ? C11 C12 1.320(17) . ? C11 C16 1.320(17) . ? C12 C13 1.36(2) . ? C13 C14 1.33(2) . ? C14 C15 1.30(3) . ? C15 C16 1.44(2) . ? C21 C22 1.306(17) . ? C21 C26 1.358(18) . ? C22 C23 1.44(2) . ? C23 C24 1.35(2) . ? C24 C25 1.29(2) . ? C25 C26 1.41(2) . ? C31 C32 1.311(19) . ? C31 C36 1.41(2) . ? C32 C33 1.46(2) . ? C33 C34 1.41(2) . ? C34 C35 1.30(2) . ? C35 C36 1.42(2) . ? P1 C47 1.735(14) . ? P1 C48 1.801(14) . ? P1 C41 1.879(16) . ? C41 C46 1.34(2) . ? C41 C42 1.40(2) . ? C42 C43 1.49(2) . ? C43 C44 1.36(3) . ? C44 C45 1.35(3) . ? C45 C46 1.38(3) . ? P2 C51 1.771(13) . ? P2 C57 1.818(15) . ? P2 C58 1.863(16) . ? C51 C56 1.309(18) . ? C51 C52 1.410(18) . ? C52 C53 1.36(2) . ? C53 C54 1.34(3) . ? C54 C55 1.29(3) . ? C55 C56 1.32(2) . ? 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 N10 Re1 C1 99.1(5) . . ? N10 Re1 P2 82.8(4) . . ? C1 Re1 P2 95.6(3) . . ? N10 Re1 Cl1 106.9(4) . . ? C1 Re1 Cl1 81.6(3) . . ? P2 Re1 Cl1 170.23(16) . . ? N10 Re1 P1 85.9(3) . . ? C1 Re1 P1 169.7(3) . . ? P2 Re1 P1 93.91(14) . . ? Cl1 Re1 P1 88.32(15) . . ? N10 Re1 Cl2 159.1(4) . . ? C1 Re1 Cl2 94.5(4) . . ? P2 Re1 Cl2 80.13(15) . . ? Cl1 Re1 Cl2 90.71(16) . . ? P1 Re1 Cl2 83.25(14) . . ? N2 C1 N1 101.4(11) . . ? N2 C1 Re1 125.7(10) . . ? N1 C1 Re1 132.9(9) . . ? N3 C2 N1 111.9(11) . . ? N3 C2 C31 126.1(12) . . ? N1 C2 C31 121.9(13) . . ? C2 N1 C1 108.5(11) . . ? C2 N1 C11 121.4(11) . . ? C1 N1 C11 130.0(11) . . ? C1 N2 N3 115.2(11) . . ? C1 N2 C21 129.7(12) . . ? N3 N2 C21 114.8(11) . . ? C2 N3 N2 102.9(10) . . ? C12 C11 C16 124.1(14) . . ? C12 C11 N1 116.3(13) . . ? C16 C11 N1 119.5(13) . . ? C11 C12 C13 115.5(16) . . ? C14 C13 C12 126.1(19) . . ? C15 C14 C13 116.0(19) . . ? C14 C15 C16 122(2) . . ? C11 C16 C15 116.2(16) . . ? C22 C21 C26 120.7(15) . . ? C22 C21 N2 117.2(14) . . ? C26 C21 N2 121.6(13) . . ? C21 C22 C23 113.7(15) . . ? C24 C23 C22 124.2(15) . . ? C25 C24 C23 121.4(18) . . ? C24 C25 C26 114.8(18) . . ? C21 C26 C25 124.9(15) . . ? C32 C31 C36 116.2(15) . . ? C32 C31 C2 118.0(16) . . ? C36 C31 C2 125.6(13) . . ? C31 C32 C33 118.9(17) . . ? C34 C33 C32 121.1(16) . . ? C35 C34 C33 121.6(19) . . ? C34 C35 C36 114.9(18) . . ? C31 C36 C35 127.1(15) . . ? C47 P1 C48 102.7(8) . . ? C47 P1 C41 101.3(8) . . ? C48 P1 C41 106.0(8) . . ? C47 P1 Re1 108.7(6) . . ? C48 P1 Re1 114.5(6) . . ? C41 P1 Re1 121.3(5) . . ? C46 C41 C42 115.7(17) . . ? C46 C41 P1 121.1(15) . . ? C42 C41 P1 123.0(13) . . ? C41 C42 C43 120.0(17) . . ? C44 C43 C42 120(2) . . ? C45 C44 C43 116(2) . . ? C44 C45 C46 124(3) . . ? C41 C46 C45 123(2) . . ? C51 P2 C57 104.9(7) . . ? C51 P2 C58 103.9(7) . . ? C57 P2 C58 99.2(9) . . ? C51 P2 Re1 111.2(5) . . ? C57 P2 Re1 121.6(6) . . ? C58 P2 Re1 114.0(6) . . ? C56 C51 C52 120.2(14) . . ? C56 C51 P2 121.6(12) . . ? C52 C51 P2 118.2(11) . . ? C53 C52 C51 118.4(17) . . ? C54 C53 C52 117.4(19) . . ? C55 C54 C53 122(2) . . ? C54 C55 C56 122(2) . . ? C51 C56 C55 119.0(17) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.738 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.139 #=============== STRUCTURE II ============================ data_rencarbene2 _database_code_CSD 213785 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Isothiocyanato(1,3,4-triphenyl-1,2,4-triazol-5-ylidene) (1-C6H4-3,4-diphenyl-1,2,4-triazol-5-ylidene)nitridorhenium(V) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H29 N8 Re S' _chemical_formula_weight 851.98 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 15.229(3) _cell_length_b 12.320(2) _cell_length_c 19.344(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.11(1) _cell_angle_gamma 90.00 _cell_volume 3535.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.49 _cell_measurement_theta_max 12.13 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 3.539 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.169 _exptl_absorpt_correction_T_max 0.642 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 ENRAF NONIUS' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 3600 _diffrn_standards_interval_time 500 _diffrn_standards_decay_% 6 _diffrn_reflns_number 8692 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.97 _reflns_number_total 7645 _reflns_number_gt 5315 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction HELENA _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1380P)^2^+11.0596P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7645 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.790 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.005 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 Re1 Re 0.28239(2) 0.03682(2) 0.220596(16) 0.04552(13) Uani 1 1 d . . . N10 N 0.3882(5) 0.0512(7) 0.2209(5) 0.068(2) Uani 1 1 d . . . C1 C 0.2628(5) 0.1474(6) 0.2980(4) 0.0449(16) Uani 1 1 d . . . N1 N 0.3251(4) 0.1938(5) 0.3511(3) 0.0478(14) Uani 1 1 d . . . C11 C 0.4203(5) 0.1706(7) 0.3682(4) 0.0501(18) Uani 1 1 d . . . C12 C 0.4799(6) 0.2496(8) 0.3593(5) 0.064(2) Uani 1 1 d . . . H12 H 0.4592 0.3165 0.3401 0.076 Uiso 1 1 calc R . . C13 C 0.5697(7) 0.2286(10) 0.3791(6) 0.080(3) Uani 1 1 d . . . H13 H 0.6106 0.2817 0.3726 0.096 Uiso 1 1 calc R . . C14 C 0.6009(7) 0.1323(12) 0.4079(6) 0.088(4) Uani 1 1 d . . . H14 H 0.6626 0.1196 0.4212 0.106 Uiso 1 1 calc R . . C15 C 0.5418(8) 0.0537(9) 0.4176(6) 0.079(3) Uani 1 1 d . . . H15 H 0.5635 -0.0126 0.4374 0.095 Uiso 1 1 calc R . . C16 C 0.4490(7) 0.0721(8) 0.3979(5) 0.062(2) Uani 1 1 d . . . H16 H 0.4080 0.0194 0.4048 0.074 Uiso 1 1 calc R . . N2 N 0.1847(4) 0.1940(6) 0.3051(3) 0.0508(15) Uani 1 1 d . . . C21 C 0.0979(5) 0.1735(7) 0.2645(4) 0.0527(19) Uani 1 1 d . . . C22 C 0.0326(6) 0.2517(8) 0.2579(6) 0.070(3) Uani 1 1 d . . . H22 H 0.0455 0.3180 0.2809 0.084 Uiso 1 1 calc R . . C23 C -0.0525(7) 0.2314(10) 0.2168(6) 0.081(3) Uani 1 1 d . . . H23 H -0.0973 0.2836 0.2138 0.097 Uiso 1 1 calc R . . C24 C -0.0719(7) 0.1375(10) 0.1812(6) 0.080(3) Uani 1 1 d . . . H24 H -0.1289 0.1267 0.1522 0.096 Uiso 1 1 calc R . . C25 C -0.0080(7) 0.0577(9) 0.1876(6) 0.070(3) Uani 1 1 d . . . H25 H -0.0214 -0.0076 0.1634 0.084 Uiso 1 1 calc R . . C26 C 0.0775(6) 0.0754(8) 0.2308(5) 0.0556(19) Uani 1 1 d . . . H26 H 0.1207 0.0208 0.2368 0.067 Uiso 1 1 calc R . . N3 N 0.1967(5) 0.2711(6) 0.3582(4) 0.0531(16) Uani 1 1 d . . . C2 C 0.2825(5) 0.2697(6) 0.3863(4) 0.0500(18) Uani 1 1 d . . . C31 C 0.3278(5) 0.3388(7) 0.4441(4) 0.0508(18) Uani 1 1 d . . . C32 C 0.3041(7) 0.4475(8) 0.4445(5) 0.067(2) Uani 1 1 d . . . H32 H 0.2596 0.4757 0.4078 0.080 Uiso 1 1 calc R . . C33 C 0.3473(9) 0.5146(9) 0.5001(6) 0.077(3) Uani 1 1 d . . . H33 H 0.3317 0.5876 0.5001 0.092 Uiso 1 1 calc R . . C34 C 0.4114(8) 0.4743(10) 0.5537(6) 0.077(3) Uani 1 1 d . . . H34 H 0.4389 0.5194 0.5909 0.092 Uiso 1 1 calc R . . C35 C 0.4366(7) 0.3667(9) 0.5540(5) 0.069(3) Uani 1 1 d . . . H35 H 0.4815 0.3395 0.5907 0.083 Uiso 1 1 calc R . . C36 C 0.3945(7) 0.3000(8) 0.4994(4) 0.064(2) Uani 1 1 d . . . H36 H 0.4113 0.2274 0.4998 0.077 Uiso 1 1 calc R . . C3 C 0.2255(5) 0.1389(6) 0.1358(4) 0.0446(16) Uani 1 1 d . . . N4 N 0.2215(4) 0.2439(5) 0.1158(3) 0.0474(14) Uani 1 1 d . . . C41 C 0.2615(6) 0.3332(7) 0.1603(4) 0.056(2) Uani 1 1 d . . . C42 C 0.3527(8) 0.3420(9) 0.1798(5) 0.074(3) Uani 1 1 d . . . H42 H 0.3894 0.2901 0.1657 0.089 Uiso 1 1 calc R . . C43 C 0.3902(12) 0.4295(12) 0.2209(7) 0.103(5) Uani 1 1 d . . . H43 H 0.4526 0.4367 0.2335 0.123 Uiso 1 1 calc R . . C44 C 0.3390(18) 0.5033(15) 0.2427(8) 0.133(8) Uani 1 1 d . . . H44 H 0.3655 0.5619 0.2699 0.160 Uiso 1 1 calc R . . C45 C 0.2465(15) 0.4928(10) 0.2251(8) 0.117(6) Uani 1 1 d . . . H45 H 0.2113 0.5441 0.2415 0.140 Uiso 1 1 calc R . . C46 C 0.2041(9) 0.4065(9) 0.1830(6) 0.084(3) Uani 1 1 d . . . H46 H 0.1418 0.3987 0.1711 0.101 Uiso 1 1 calc R . . N5 N 0.1739(5) 0.0892(5) 0.0789(3) 0.0487(15) Uani 1 1 d . . . C51 C 0.1664(6) -0.0255(7) 0.0773(5) 0.0523(19) Uani 1 1 d . . . C52 C 0.1177(7) -0.0785(8) 0.0186(5) 0.064(2) Uani 1 1 d . . . H52 H 0.0846 -0.0410 -0.0204 0.077 Uiso 1 1 calc R . . C53 C 0.1204(7) -0.1911(9) 0.0204(6) 0.074(3) Uani 1 1 d . . . H53 H 0.0913 -0.2306 -0.0191 0.089 Uiso 1 1 calc R . . C54 C 0.1659(7) -0.2446(8) 0.0805(6) 0.071(3) Uani 1 1 d . . . H54 H 0.1649 -0.3200 0.0821 0.085 Uiso 1 1 calc R . . C55 C 0.2126(6) -0.1872(7) 0.1380(5) 0.058(2) Uani 1 1 d . . . H55 H 0.2428 -0.2253 0.1778 0.069 Uiso 1 1 calc R . . C56 C 0.2168(5) -0.0735(7) 0.1390(4) 0.0487(17) Uani 1 1 d . . . N6 N 0.1367(5) 0.1568(6) 0.0241(3) 0.0530(16) Uani 1 1 d . . . C4 C 0.1682(5) 0.2529(7) 0.0472(4) 0.0498(18) Uani 1 1 d . . . C61 C 0.1483(6) 0.3517(7) 0.0049(4) 0.056(2) Uani 1 1 d . . . C62 C 0.2131(8) 0.4298(8) 0.0052(5) 0.071(3) Uani 1 1 d . . . H62 H 0.2701 0.4229 0.0349 0.085 Uiso 1 1 calc R . . C63 C 0.1924(12) 0.5186(8) -0.0393(7) 0.095(4) Uani 1 1 d . . . H63 H 0.2358 0.5721 -0.0384 0.114 Uiso 1 1 calc R . . C64 C 0.1109(13) 0.5295(10) -0.0839(7) 0.100(5) Uani 1 1 d . . . H64 H 0.0978 0.5905 -0.1127 0.120 Uiso 1 1 calc R . . C65 C 0.0482(10) 0.4506(12) -0.0864(7) 0.101(4) Uani 1 1 d . . . H65 H -0.0073 0.4565 -0.1182 0.122 Uiso 1 1 calc R . . C66 C 0.0661(7) 0.3613(9) -0.0419(6) 0.078(3) Uani 1 1 d . . . H66 H 0.0225 0.3079 -0.0438 0.094 Uiso 1 1 calc R . . N20 N 0.2799(5) -0.0889(6) 0.2905(4) 0.0581(17) Uani 1 1 d . . . C20 C 0.2937(6) -0.1597(8) 0.3306(5) 0.060(2) Uani 1 1 d . . . S20 S 0.3131(3) -0.2596(3) 0.38510(18) 0.0963(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.04367(19) 0.04431(18) 0.04671(18) 0.00007(14) 0.00636(12) 0.00233(14) N10 0.054(4) 0.075(5) 0.071(5) -0.010(4) 0.003(4) 0.001(4) C1 0.046(4) 0.050(4) 0.038(3) 0.006(3) 0.008(3) 0.000(3) N1 0.045(3) 0.050(4) 0.046(3) 0.000(3) 0.005(3) 0.006(3) C11 0.052(4) 0.055(5) 0.043(4) -0.008(3) 0.009(3) 0.004(4) C12 0.052(5) 0.064(5) 0.070(6) -0.014(5) 0.003(4) -0.005(4) C13 0.050(5) 0.092(8) 0.095(8) -0.021(7) 0.010(5) -0.012(5) C14 0.050(6) 0.119(10) 0.088(7) -0.022(7) 0.000(5) 0.008(6) C15 0.074(7) 0.080(7) 0.075(7) 0.002(5) 0.001(5) 0.030(6) C16 0.059(5) 0.061(5) 0.060(5) 0.000(4) 0.001(4) 0.010(4) N2 0.045(4) 0.054(4) 0.053(4) -0.001(3) 0.009(3) 0.007(3) C21 0.047(4) 0.060(5) 0.050(4) 0.007(4) 0.009(3) 0.001(4) C22 0.050(5) 0.060(5) 0.094(7) 0.002(5) 0.001(5) 0.013(4) C23 0.055(6) 0.088(8) 0.095(8) 0.020(7) 0.007(5) 0.013(5) C24 0.058(6) 0.095(8) 0.081(7) 0.015(6) 0.002(5) -0.001(6) C25 0.067(6) 0.073(6) 0.068(6) 0.000(5) 0.010(5) -0.024(5) C26 0.043(4) 0.061(5) 0.063(5) 0.004(4) 0.014(4) -0.001(4) N3 0.052(4) 0.053(4) 0.054(4) -0.003(3) 0.012(3) 0.005(3) C2 0.052(4) 0.044(4) 0.054(4) -0.001(3) 0.012(4) 0.002(3) C31 0.048(4) 0.057(5) 0.051(4) -0.001(4) 0.020(3) 0.001(4) C32 0.070(6) 0.065(6) 0.064(5) -0.006(4) 0.014(5) 0.012(5) C33 0.108(9) 0.056(6) 0.073(7) -0.009(5) 0.033(6) -0.008(6) C34 0.087(8) 0.089(8) 0.055(5) -0.018(5) 0.018(5) -0.018(6) C35 0.077(6) 0.071(7) 0.056(5) -0.011(4) 0.008(4) 0.001(5) C36 0.084(6) 0.059(5) 0.048(4) -0.005(4) 0.012(4) 0.004(5) C3 0.048(4) 0.039(4) 0.047(4) 0.000(3) 0.011(3) -0.002(3) N4 0.045(3) 0.048(4) 0.048(3) -0.002(3) 0.008(3) -0.004(3) C41 0.063(5) 0.053(5) 0.051(4) -0.001(4) 0.011(4) -0.019(4) C42 0.088(7) 0.066(6) 0.062(5) 0.007(5) 0.003(5) -0.017(5) C43 0.130(12) 0.087(9) 0.076(8) 0.011(7) -0.004(8) -0.045(9) C44 0.21(2) 0.090(10) 0.075(9) -0.003(8) -0.010(12) -0.072(14) C45 0.23(2) 0.049(6) 0.091(9) -0.023(6) 0.069(12) -0.006(10) C46 0.116(9) 0.061(6) 0.083(7) -0.002(5) 0.038(7) 0.012(6) N5 0.053(4) 0.044(4) 0.045(3) 0.000(3) 0.003(3) -0.002(3) C51 0.047(4) 0.050(5) 0.058(5) -0.008(4) 0.007(4) -0.002(4) C52 0.062(6) 0.057(5) 0.067(5) -0.003(4) 0.001(4) -0.015(4) C53 0.077(7) 0.069(6) 0.072(6) -0.021(5) 0.006(5) -0.019(5) C54 0.078(7) 0.046(5) 0.090(7) -0.011(5) 0.021(6) -0.005(5) C55 0.055(5) 0.047(5) 0.070(5) -0.002(4) 0.012(4) -0.001(4) C56 0.046(4) 0.048(4) 0.053(4) -0.007(3) 0.014(3) 0.001(3) N6 0.051(4) 0.054(4) 0.049(4) -0.002(3) 0.000(3) 0.000(3) C4 0.047(4) 0.053(4) 0.049(4) 0.001(4) 0.008(3) -0.006(4) C61 0.058(5) 0.057(5) 0.054(4) 0.006(4) 0.016(4) 0.004(4) C62 0.092(8) 0.058(5) 0.059(5) 0.013(4) 0.010(5) -0.013(5) C63 0.164(14) 0.047(6) 0.073(7) 0.014(5) 0.026(8) -0.018(7) C64 0.170(15) 0.055(7) 0.070(7) 0.009(5) 0.019(9) 0.019(8) C65 0.102(10) 0.111(11) 0.082(8) 0.023(7) 0.003(7) 0.046(9) C66 0.067(6) 0.083(7) 0.079(6) 0.025(6) 0.007(5) 0.008(5) N20 0.067(5) 0.048(4) 0.055(4) 0.015(3) 0.006(3) 0.007(3) C20 0.056(5) 0.054(5) 0.069(5) -0.012(4) 0.008(4) 0.000(4) S20 0.120(3) 0.0718(18) 0.090(2) 0.0344(16) 0.0088(18) 0.0166(17) _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 Re1 N10 1.620(8) . ? Re1 N20 2.062(7) . ? Re1 C1 2.095(8) . ? Re1 C3 2.091(7) . ? Re1 C56 2.150(8) . ? C1 N2 1.356(10) . ? C1 N1 1.356(10) . ? N1 C2 1.401(10) . ? N1 C11 1.440(10) . ? C11 C12 1.367(12) . ? C11 C16 1.372(12) . ? C12 C13 1.360(13) . ? C13 C14 1.351(17) . ? C14 C15 1.363(17) . ? C15 C16 1.398(14) . ? N2 N3 1.380(9) . ? N2 C21 1.400(10) . ? C21 C22 1.369(12) . ? C21 C26 1.374(12) . ? C22 C23 1.381(14) . ? C23 C24 1.344(16) . ? C24 C25 1.369(15) . ? C25 C26 1.395(13) . ? N3 C2 1.297(10) . ? C2 C31 1.449(11) . ? C31 C36 1.383(12) . ? C31 C32 1.388(12) . ? C32 C33 1.396(15) . ? C33 C34 1.349(17) . ? C34 C35 1.379(15) . ? C35 C36 1.376(12) . ? C3 N5 1.347(10) . ? C3 N4 1.348(10) . ? N4 C4 1.393(10) . ? N4 C41 1.445(10) . ? C41 C42 1.358(13) . ? C41 C46 1.396(14) . ? C42 C43 1.383(16) . ? C43 C44 1.33(3) . ? C44 C45 1.38(3) . ? C45 C46 1.404(19) . ? N5 N6 1.365(9) . ? N5 C51 1.418(11) . ? C51 C52 1.373(12) . ? C51 C56 1.396(12) . ? C52 C53 1.387(14) . ? C53 C54 1.378(14) . ? C54 C55 1.372(13) . ? C55 C56 1.402(12) . ? N6 C4 1.317(10) . ? C4 C61 1.459(11) . ? C61 C62 1.378(13) . ? C61 C66 1.374(13) . ? C62 C63 1.384(14) . ? C63 C64 1.35(2) . ? C64 C65 1.36(2) . ? C65 C66 1.384(16) . ? N20 C20 1.155(11) . ? C20 S20 1.604(10) . ? 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 N10 Re1 N20 104.3(4) . . ? N10 Re1 C1 103.2(4) . . ? N20 Re1 C1 89.6(3) . . ? N10 Re1 C3 99.9(4) . . ? N20 Re1 C3 154.1(3) . . ? C1 Re1 C3 93.9(3) . . ? N10 Re1 C56 111.6(4) . . ? N20 Re1 C56 86.1(3) . . ? C1 Re1 C56 144.9(3) . . ? C3 Re1 C56 76.3(3) . . ? N2 C1 N1 103.0(6) . . ? N2 C1 Re1 128.2(5) . . ? N1 C1 Re1 128.8(6) . . ? C1 N1 C2 109.1(6) . . ? C1 N1 C11 125.8(7) . . ? C2 N1 C11 125.0(6) . . ? C12 C11 C16 121.7(8) . . ? C12 C11 N1 119.5(8) . . ? C16 C11 N1 118.6(8) . . ? C13 C12 C11 119.0(10) . . ? C14 C13 C12 121.3(11) . . ? C13 C14 C15 120.0(10) . . ? C14 C15 C16 120.4(10) . . ? C11 C16 C15 117.7(10) . . ? C1 N2 N3 113.3(6) . . ? C1 N2 C21 127.2(7) . . ? N3 N2 C21 119.4(7) . . ? C22 C21 C26 119.6(8) . . ? C22 C21 N2 119.9(8) . . ? C26 C21 N2 120.6(8) . . ? C21 C22 C23 119.6(10) . . ? C24 C23 C22 121.3(10) . . ? C23 C24 C25 120.2(10) . . ? C24 C25 C26 119.3(10) . . ? C21 C26 C25 120.1(9) . . ? C2 N3 N2 104.7(6) . . ? N3 C2 N1 109.8(7) . . ? N3 C2 C31 125.1(7) . . ? N1 C2 C31 125.1(7) . . ? C36 C31 C32 118.4(8) . . ? C36 C31 C2 122.2(8) . . ? C32 C31 C2 119.5(8) . . ? C33 C32 C31 119.9(10) . . ? C34 C33 C32 120.5(10) . . ? C33 C34 C35 120.6(10) . . ? C36 C35 C34 119.4(10) . . ? C35 C36 C31 121.3(9) . . ? N5 C3 N4 102.7(6) . . ? N5 C3 Re1 115.4(5) . . ? N4 C3 Re1 141.9(6) . . ? C3 N4 C4 109.3(6) . . ? C3 N4 C41 125.0(7) . . ? C4 N4 C41 125.6(7) . . ? C42 C41 C46 122.3(10) . . ? C42 C41 N4 119.6(9) . . ? C46 C41 N4 118.1(9) . . ? C41 C42 C43 119.0(13) . . ? C44 C43 C42 121.4(16) . . ? C43 C44 C45 119.9(14) . . ? C44 C45 C46 121.6(15) . . ? C45 C46 C41 115.7(13) . . ? C3 N5 N6 114.9(6) . . ? C3 N5 C51 119.9(7) . . ? N6 N5 C51 125.1(6) . . ? C52 C51 C56 126.5(8) . . ? C52 C51 N5 121.2(8) . . ? C56 C51 N5 112.2(7) . . ? C51 C52 C53 116.6(9) . . ? C52 C53 C54 120.4(9) . . ? C55 C54 C53 120.4(9) . . ? C54 C55 C56 122.7(9) . . ? C51 C56 C55 113.4(8) . . ? C51 C56 Re1 115.7(6) . . ? C55 C56 Re1 130.9(7) . . ? C4 N6 N5 103.3(6) . . ? N6 C4 N4 109.8(7) . . ? N6 C4 C61 123.1(7) . . ? N4 C4 C61 127.1(7) . . ? C62 C61 C66 119.1(9) . . ? C62 C61 C4 121.5(8) . . ? C66 C61 C4 119.0(8) . . ? C61 C62 C63 119.2(11) . . ? C64 C63 C62 121.6(12) . . ? C63 C64 C65 119.3(11) . . ? C64 C65 C66 120.7(12) . . ? C61 C66 C65 120.0(12) . . ? C20 N20 Re1 168.6(8) . . ? N20 C20 S20 178.9(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.201 _refine_diff_density_min -2.774 _refine_diff_density_rms 0.188 #----END