# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Srebrata, Goswami' 'Chayan, Das' 'Gene-Hsiang, Lee' 'Shie-Ming, Peng' _publ_contact_author_name 'Dr Goswami Srebrata' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'icsg@mahendra.iacs.res.in' _publ_section_title ; Osmium(II) complexes of 2-[arylamido)phenylazo]pyridines. New examples of deamination reactions X-ray structure and redox properties ; data_ic7581 _database_code_CSD 157836 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H27 Br N8 Os' _chemical_formula_weight 817.75 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0940(2) _cell_length_b 19.9527(3) _cell_length_c 14.5400(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.873(1) _cell_angle_gamma 90.00 _cell_volume 3007.28(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method ? _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 5.608 _exptl_absorpt_correction_type 'empirical used sadabs' _exptl_absorpt_correction_T_min 0.3159 _exptl_absorpt_correction_T_max 0.4929 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART 1K CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21518 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6877 _reflns_number_observed 6257 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+2.8083P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6877 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_obs 0.0227 _refine_ls_wR_factor_all 0.0499 _refine_ls_wR_factor_obs 0.0482 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.098 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os Os 0.767022(9) 0.366931(5) 0.776104(7) 0.01485(4) Uani 1 d . . Br Br 1.00438(2) 0.374157(15) 0.87995(2) 0.02291(7) Uani 1 d . . N1 N 0.7936(2) 0.40746(11) 0.6533(2) 0.0182(5) Uani 1 d . . N2 N 0.5719(2) 0.42440(12) 0.6043(2) 0.0216(5) Uani 1 d . . N3 N 0.5942(2) 0.38941(12) 0.6870(2) 0.0171(4) Uani 1 d . . N4 N 0.4840(2) 0.26539(13) 0.6873(2) 0.0260(5) Uani 1 d . . H4A H 0.5382(2) 0.27533(13) 0.6575(2) 0.031 Uiso 1 calc R . N5 N 0.7424(2) 0.44623(11) 0.8614(2) 0.0177(5) Uani 1 d . . N6 N 0.6864(2) 0.35569(12) 0.9442(2) 0.0196(5) Uani 1 d . . N7 N 0.7258(2) 0.32304(11) 0.8813(2) 0.0169(4) Uani 1 d . . N8 N 0.7976(2) 0.27017(11) 0.7468(2) 0.0202(5) Uani 1 d . . C1 C 0.9031(3) 0.40896(15) 0.6311(2) 0.0231(6) Uani 1 d . . H1A H 0.9805(3) 0.39124(15) 0.6773(2) 0.028 Uiso 1 calc R . C2 C 0.9053(3) 0.4351(2) 0.5448(2) 0.0288(7) Uani 1 d . . H2A H 0.9829(3) 0.4348(2) 0.5311(2) 0.035 Uiso 1 calc R . C3 C 0.7926(3) 0.4622(2) 0.4768(2) 0.0311(7) Uani 1 d . . H3A H 0.7938(3) 0.4821(2) 0.4178(2) 0.037 Uiso 1 calc R . C4 C 0.6808(3) 0.4598(2) 0.4959(2) 0.0274(6) Uani 1 d . . H4B H 0.6031(3) 0.4775(2) 0.4501(2) 0.033 Uiso 1 calc R . C5 C 0.6824(3) 0.43063(14) 0.5847(2) 0.0202(6) Uani 1 d . . C6 C 0.4817(2) 0.38370(15) 0.7144(2) 0.0204(6) Uani 1 d . . C7 C 0.4273(3) 0.4412(2) 0.7368(2) 0.0253(6) Uani 1 d . . H7A H 0.4623(3) 0.4839(2) 0.7319(2) 0.030 Uiso 1 calc R . C8 C 0.3219(3) 0.4362(2) 0.7663(2) 0.0328(8) Uani 1 d . . H8A H 0.2854(3) 0.4753(2) 0.7832(2) 0.039 Uiso 1 calc R . C9 C 0.2705(3) 0.3737(2) 0.7709(2) 0.0345(8) Uani 1 d . . H9A H 0.1983(3) 0.3701(2) 0.7911(2) 0.041 Uiso 1 calc R . C10 C 0.3226(3) 0.3161(2) 0.7465(2) 0.0308(7) Uani 1 d . . H10A H 0.2848(3) 0.2738(2) 0.7493(2) 0.037 Uiso 1 calc R . C11 C 0.4306(3) 0.3197(2) 0.7179(2) 0.0230(6) Uani 1 d . . C12 C 0.4642(3) 0.1966(2) 0.6970(2) 0.0250(6) Uani 1 d . . C13 C 0.4445(3) 0.1692(2) 0.7789(2) 0.0332(7) Uani 1 d . . H13A H 0.4385(3) 0.1976(2) 0.8296(2) 0.040 Uiso 1 calc R . C14 C 0.4337(4) 0.0997(2) 0.7855(3) 0.0412(8) Uani 1 d . . H14A H 0.4201(4) 0.0809(2) 0.8410(3) 0.049 Uiso 1 calc R . C15 C 0.4426(3) 0.0584(2) 0.7130(3) 0.0367(8) Uani 1 d . . H15A H 0.4349(3) 0.0112(2) 0.7183(3) 0.044 Uiso 1 calc R . C16 C 0.4628(3) 0.0854(2) 0.6322(3) 0.0319(7) Uani 1 d . . H16A H 0.4693(3) 0.0568(2) 0.5820(3) 0.038 Uiso 1 calc R . C17 C 0.4736(3) 0.1541(2) 0.6240(2) 0.0275(6) Uani 1 d . . H17A H 0.4876(3) 0.1723(2) 0.5683(2) 0.033 Uiso 1 calc R . C18 C 0.7581(3) 0.51263(14) 0.8537(2) 0.0218(6) Uani 1 d . . H18A H 0.7930(3) 0.52821(14) 0.8067(2) 0.026 Uiso 1 calc R . C19 C 0.7255(3) 0.5588(2) 0.9111(2) 0.0272(6) Uani 1 d . . H19A H 0.7379(3) 0.6053(2) 0.9038(2) 0.033 Uiso 1 calc R . C20 C 0.6741(3) 0.5363(2) 0.9800(2) 0.0281(7) Uani 1 d . . H20A H 0.6500(3) 0.5675(2) 1.0198(2) 0.034 Uiso 1 calc R . C21 C 0.6585(3) 0.4686(2) 0.9902(2) 0.0244(6) Uani 1 d . . H21A H 0.6236(3) 0.4526(2) 1.0371(2) 0.029 Uiso 1 calc R . C22 C 0.6945(2) 0.42372(14) 0.9308(2) 0.0189(5) Uani 1 d . . C23 C 0.7454(3) 0.25438(14) 0.8906(2) 0.0200(6) Uani 1 d . . C24 C 0.7304(3) 0.21514(15) 0.9657(2) 0.0257(6) Uani 1 d . . H24A H 0.7026(3) 0.23490(15) 1.0142(2) 0.031 Uiso 1 calc R . C25 C 0.7565(3) 0.1476(2) 0.9684(2) 0.0323(7) Uani 1 d . . H25A H 0.7477(3) 0.1203(2) 1.0192(2) 0.039 Uiso 1 calc R . C26 C 0.7964(4) 0.1194(2) 0.8949(3) 0.0373(8) Uani 1 d . . H26A H 0.8133(4) 0.0726(2) 0.8967(3) 0.045 Uiso 1 calc R . C27 C 0.8115(3) 0.1571(2) 0.8209(2) 0.0297(7) Uani 1 d . . H27A H 0.8385(3) 0.1364(2) 0.7727(2) 0.036 Uiso 1 calc R . C28 C 0.7869(3) 0.22682(14) 0.8165(2) 0.0213(6) Uani 1 d . . C29 C 0.8515(3) 0.24778(14) 0.6755(2) 0.0239(6) Uani 1 d . . C30 C 0.9759(3) 0.2229(2) 0.7030(3) 0.0329(7) Uani 1 d . . H30A H 1.0285(3) 0.2197(2) 0.7706(3) 0.040 Uiso 1 calc R . C31 C 1.0238(3) 0.2025(2) 0.6296(3) 0.0406(9) Uani 1 d . . H31A H 1.1086(3) 0.1846(2) 0.6480(3) 0.049 Uiso 1 calc R . C32 C 0.9488(4) 0.2082(2) 0.5320(3) 0.0397(9) Uani 1 d . . H32A H 0.9820(4) 0.1947(2) 0.4830(3) 0.048 Uiso 1 calc R . C33 C 0.8255(4) 0.2333(2) 0.5046(3) 0.0371(8) Uani 1 d . . H33A H 0.7737(4) 0.2368(2) 0.4368(3) 0.045 Uiso 1 calc R . C34 C 0.7766(3) 0.2538(2) 0.5758(2) 0.0277(6) Uani 1 d . . H34A H 0.6919(3) 0.2718(2) 0.5565(2) 0.033 Uiso 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 Os 0.01315(5) 0.01927(6) 0.01401(6) 0.00094(4) 0.00716(4) 0.00124(4) Br 0.01397(12) 0.0362(2) 0.01920(13) 0.00082(12) 0.00668(10) 0.00073(11) N1 0.0201(11) 0.0205(12) 0.0164(11) 0.0016(9) 0.0094(9) 0.0012(9) N2 0.0211(12) 0.0290(13) 0.0167(12) 0.0040(10) 0.0091(9) 0.0045(10) N3 0.0165(10) 0.0223(11) 0.0144(11) -0.0014(9) 0.0076(8) 0.0018(9) N4 0.0246(12) 0.0307(14) 0.0282(14) -0.0012(11) 0.0162(11) -0.0047(10) N5 0.0151(11) 0.0201(11) 0.0180(11) 0.0018(9) 0.0061(9) 0.0012(9) N6 0.0194(11) 0.0250(13) 0.0162(11) 0.0000(9) 0.0087(9) 0.0009(9) N7 0.0142(10) 0.0213(12) 0.0148(11) 0.0004(9) 0.0045(9) 0.0009(9) N8 0.0209(12) 0.0211(12) 0.0207(12) -0.0013(10) 0.0100(10) 0.0017(9) C1 0.0201(13) 0.030(2) 0.0243(15) 0.0011(12) 0.0136(12) 0.0012(11) C2 0.028(2) 0.037(2) 0.029(2) 0.0039(14) 0.0189(13) 0.0010(13) C3 0.039(2) 0.036(2) 0.025(2) 0.0097(14) 0.0197(14) 0.0056(14) C4 0.033(2) 0.031(2) 0.0212(15) 0.0085(13) 0.0125(13) 0.0088(13) C5 0.0218(13) 0.0216(14) 0.0186(13) 0.0012(11) 0.0089(11) 0.0046(11) C6 0.0139(12) 0.035(2) 0.0126(12) 0.0025(11) 0.0049(10) 0.0045(11) C7 0.0199(14) 0.037(2) 0.0185(14) 0.0031(13) 0.0064(11) 0.0079(12) C8 0.025(2) 0.052(2) 0.025(2) 0.0049(15) 0.0127(13) 0.0176(15) C9 0.0177(14) 0.065(2) 0.024(2) 0.006(2) 0.0112(12) 0.0092(15) C10 0.0195(14) 0.050(2) 0.024(2) 0.0031(15) 0.0092(12) -0.0051(13) C11 0.0162(13) 0.035(2) 0.0172(14) 0.0017(12) 0.0053(11) -0.0006(11) C12 0.0168(13) 0.034(2) 0.0232(15) 0.0013(13) 0.0054(11) -0.0054(11) C13 0.036(2) 0.041(2) 0.026(2) -0.0012(15) 0.0141(14) -0.0099(15) C14 0.044(2) 0.044(2) 0.039(2) 0.009(2) 0.020(2) -0.009(2) C15 0.030(2) 0.032(2) 0.046(2) 0.000(2) 0.012(2) -0.0074(14) C16 0.0213(14) 0.037(2) 0.034(2) -0.0046(14) 0.0061(13) -0.0009(13) C17 0.0234(14) 0.034(2) 0.025(2) -0.0018(13) 0.0091(12) -0.0012(12) C18 0.0200(13) 0.0263(15) 0.0195(14) 0.0017(12) 0.0077(11) -0.0001(11) C19 0.033(2) 0.0214(15) 0.025(2) -0.0010(12) 0.0075(13) 0.0026(12) C20 0.032(2) 0.030(2) 0.022(2) -0.0041(13) 0.0090(13) 0.0082(13) C21 0.0245(14) 0.032(2) 0.0193(14) 0.0011(12) 0.0115(12) 0.0042(12) C22 0.0164(12) 0.0247(14) 0.0159(13) 0.0016(11) 0.0061(10) 0.0022(10) C23 0.0187(13) 0.0221(14) 0.0177(13) 0.0009(11) 0.0045(11) 0.0001(10) C24 0.030(2) 0.027(2) 0.0200(15) 0.0019(12) 0.0085(12) -0.0024(12) C25 0.043(2) 0.026(2) 0.025(2) 0.0062(13) 0.0084(14) -0.0026(13) C26 0.052(2) 0.023(2) 0.032(2) 0.0020(14) 0.009(2) 0.0023(14) C27 0.038(2) 0.0220(14) 0.029(2) -0.0011(13) 0.0116(14) 0.0041(13) C28 0.0192(13) 0.0238(14) 0.0194(14) -0.0005(12) 0.0050(11) 0.0003(11) C29 0.0258(14) 0.0206(14) 0.030(2) -0.0039(12) 0.0159(13) -0.0026(11) C30 0.026(2) 0.032(2) 0.042(2) -0.0103(15) 0.0130(14) 0.0001(13) C31 0.030(2) 0.036(2) 0.065(3) -0.016(2) 0.029(2) -0.0055(14) C32 0.046(2) 0.036(2) 0.053(2) -0.015(2) 0.036(2) -0.012(2) C33 0.053(2) 0.034(2) 0.034(2) -0.0071(15) 0.028(2) -0.008(2) C34 0.032(2) 0.029(2) 0.027(2) -0.0003(13) 0.0161(13) -0.0008(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os N3 1.946(2) . ? Os N7 1.953(2) . ? Os N8 2.031(2) . ? Os N1 2.074(2) . ? Os N5 2.088(2) . ? Os Br 2.5301(3) . ? N1 C5 1.361(3) . ? N1 C1 1.364(3) . ? N2 N3 1.336(3) . ? N2 C5 1.360(3) . ? N3 C6 1.443(3) . ? N4 C11 1.383(4) . ? N4 C12 1.406(4) . ? N5 C18 1.346(4) . ? N5 C22 1.372(3) . ? N6 N7 1.319(3) . ? N6 C22 1.379(3) . ? N7 C23 1.386(3) . ? N8 C28 1.369(4) . ? N8 C29 1.440(4) . ? C1 C2 1.368(4) . ? C2 C3 1.397(4) . ? C3 C4 1.365(4) . ? C4 C5 1.410(4) . ? C6 C7 1.388(4) . ? C6 C11 1.405(4) . ? C7 C8 1.385(4) . ? C8 C9 1.384(5) . ? C9 C10 1.387(5) . ? C10 C11 1.404(4) . ? C12 C17 1.390(4) . ? C12 C13 1.397(4) . ? C13 C14 1.398(5) . ? C14 C15 1.369(5) . ? C15 C16 1.382(5) . ? C16 C17 1.384(5) . ? C18 C19 1.375(4) . ? C19 C20 1.392(4) . ? C20 C21 1.376(4) . ? C21 C22 1.398(4) . ? C23 C24 1.401(4) . ? C23 C28 1.425(4) . ? C24 C25 1.375(4) . ? C25 C26 1.412(5) . ? C26 C27 1.371(5) . ? C27 C28 1.414(4) . ? C29 C30 1.385(4) . ? C29 C34 1.396(4) . ? C30 C31 1.412(5) . ? C31 C32 1.371(6) . ? C32 C33 1.376(5) . ? C33 C34 1.390(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Os N7 100.05(9) . . ? N3 Os N8 106.15(9) . . ? N7 Os N8 80.86(9) . . ? N3 Os N1 75.26(9) . . ? N7 Os N1 173.49(9) . . ? N8 Os N1 96.00(9) . . ? N3 Os N5 85.08(9) . . ? N7 Os N5 75.98(9) . . ? N8 Os N5 155.75(9) . . ? N1 Os N5 107.76(9) . . ? N3 Os Br 162.44(7) . . ? N7 Os Br 92.43(6) . . ? N8 Os Br 87.89(7) . . ? N1 Os Br 93.14(6) . . ? N5 Os Br 86.04(6) . . ? C5 N1 C1 118.0(2) . . ? C5 N1 Os 113.2(2) . . ? C1 N1 Os 128.6(2) . . ? N3 N2 C5 110.2(2) . . ? N2 N3 C6 112.9(2) . . ? N2 N3 Os 122.9(2) . . ? C6 N3 Os 122.8(2) . . ? C11 N4 C12 129.3(2) . . ? C18 N5 C22 118.6(2) . . ? C18 N5 Os 130.4(2) . . ? C22 N5 Os 110.8(2) . . ? N7 N6 C22 109.5(2) . . ? N6 N7 C23 120.0(2) . . ? N6 N7 Os 123.4(2) . . ? C23 N7 Os 116.6(2) . . ? C28 N8 C29 120.3(2) . . ? C28 N8 Os 112.4(2) . . ? C29 N8 Os 126.1(2) . . ? N1 C1 C2 122.3(3) . . ? C1 C2 C3 119.5(3) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C5 119.0(3) . . ? N2 C5 N1 117.7(2) . . ? N2 C5 C4 120.7(3) . . ? N1 C5 C4 121.6(3) . . ? C7 C6 C11 121.9(3) . . ? C7 C6 N3 119.4(3) . . ? C11 C6 N3 118.8(2) . . ? C8 C7 C6 119.9(3) . . ? C9 C8 C7 119.2(3) . . ? C8 C9 C10 121.2(3) . . ? C9 C10 C11 120.7(3) . . ? N4 C11 C10 124.3(3) . . ? N4 C11 C6 118.4(2) . . ? C10 C11 C6 117.1(3) . . ? C17 C12 C13 119.4(3) . . ? C17 C12 N4 117.5(3) . . ? C13 C12 N4 123.0(3) . . ? C12 C13 C14 119.2(3) . . ? C15 C14 C13 121.0(3) . . ? C14 C15 C16 119.7(3) . . ? C15 C16 C17 120.4(3) . . ? C16 C17 C12 120.3(3) . . ? N5 C18 C19 122.6(3) . . ? C18 C19 C20 119.0(3) . . ? C21 C20 C19 119.6(3) . . ? C20 C21 C22 119.1(3) . . ? N5 C22 N6 119.2(2) . . ? N5 C22 C21 121.0(3) . . ? N6 C22 C21 119.7(2) . . ? N7 C23 C24 124.8(3) . . ? N7 C23 C28 112.9(2) . . ? C24 C23 C28 122.3(3) . . ? C25 C24 C23 119.2(3) . . ? C24 C25 C26 119.3(3) . . ? C27 C26 C25 122.2(3) . . ? C26 C27 C28 120.1(3) . . ? N8 C28 C27 126.1(3) . . ? N8 C28 C23 116.9(2) . . ? C27 C28 C23 117.0(3) . . ? C30 C29 C34 119.5(3) . . ? C30 C29 N8 122.0(3) . . ? C34 C29 N8 118.4(3) . . ? C29 C30 C31 119.4(3) . . ? C32 C31 C30 120.3(3) . . ? C31 C32 C33 120.3(3) . . ? C32 C33 C34 120.2(3) . . ? C33 C34 C29 120.2(3) . . ? _refine_diff_density_max 1.651 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.089 #CIF for Os[(La)(PaP)Br], 2a data_ic7676 _database_code_CSD 157837 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Br N7 Os' _chemical_formula_weight 726.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.643(2) _cell_length_b 14.1915(18) _cell_length_c 13.850(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.36(2) _cell_angle_gamma 90.00 _cell_volume 2680.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.26 _cell_measurement_theta_max 12.00 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 6.278 _exptl_absorpt_correction_type 'empirical used psi-scan' _exptl_absorpt_correction_T_min 0.2181 _exptl_absorpt_correction_T_max 0.5687 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4731 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4731 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0281P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4731 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 0.007254(19) 0.293133(18) 0.71530(2) 0.05351(11) Uani 1 1 d . . . Br Br -0.06032(6) 0.44792(5) 0.77569(6) 0.0808(3) Uani 1 1 d . . . N1 N -0.0580(4) 0.3306(3) 0.5836(4) 0.0573(16) Uani 1 1 d . . . N2 N 0.1064(4) 0.3768(4) 0.5569(4) 0.0562(15) Uani 1 1 d . . . N3 N 0.1142(4) 0.3527(3) 0.6483(4) 0.0491(14) Uani 1 1 d . . . N4 N 0.1057(4) 0.3018(3) 0.8241(4) 0.0617(16) Uani 1 1 d . . . N5 N -0.1016(4) 0.2141(4) 0.7806(4) 0.0606(15) Uani 1 1 d . . . N6 N -0.0295(4) 0.0928(3) 0.6936(4) 0.0582(15) Uani 1 1 d . . . N7 N 0.0303(4) 0.1650(3) 0.6730(4) 0.0525(14) Uani 1 1 d . . . C1 C -0.1513(6) 0.3289(5) 0.5515(7) 0.080(3) Uani 1 1 d . . . H1A H -0.1995 0.3076 0.5926 0.096 Uiso 1 1 calc R . . C2 C -0.1781(7) 0.3573(6) 0.4605(8) 0.089(3) Uani 1 1 d . . . H2A H -0.2436 0.3546 0.4405 0.106 Uiso 1 1 calc R . . C3 C -0.1082(6) 0.3901(5) 0.3979(7) 0.084(3) Uani 1 1 d . . . H3A H -0.1256 0.4104 0.3360 0.100 Uiso 1 1 calc R . . C4 C -0.0130(6) 0.3918(5) 0.4301(6) 0.072(2) Uani 1 1 d . . . H4A H 0.0354 0.4117 0.3886 0.086 Uiso 1 1 calc R . . C5 C 0.0132(5) 0.3645(4) 0.5237(5) 0.0548(18) Uani 1 1 d . . . C6 C 0.1979(4) 0.3714(4) 0.7014(5) 0.0505(17) Uani 1 1 d . . . C7 C 0.2818(5) 0.4118(4) 0.6636(6) 0.062(2) Uani 1 1 d . . . H7A H 0.2836 0.4278 0.5986 0.074 Uiso 1 1 calc R . . C8 C 0.3601(5) 0.4274(5) 0.7221(6) 0.069(2) Uani 1 1 d . . . H8A H 0.4160 0.4554 0.6978 0.083 Uiso 1 1 calc R . . C9 C 0.3575(5) 0.4021(5) 0.8180(6) 0.069(2) Uani 1 1 d . . . H9A H 0.4128 0.4127 0.8572 0.082 Uiso 1 1 calc R . . C10 C 0.2759(5) 0.3616(4) 0.8582(5) 0.064(2) Uani 1 1 d . . . H10A H 0.2760 0.3454 0.9233 0.077 Uiso 1 1 calc R . . C11 C 0.1931(5) 0.3454(4) 0.7992(6) 0.0557(18) Uani 1 1 d . . . C12 C 0.0896(5) 0.2799(5) 0.9230(6) 0.065(2) Uani 1 1 d . . . C13 C 0.0947(6) 0.3467(6) 0.9952(7) 0.097(3) Uani 1 1 d . . . H13A H 0.1105 0.4088 0.9808 0.117 Uiso 1 1 calc R . . C14 C 0.0760(8) 0.3205(7) 1.0900(7) 0.121(4) Uani 1 1 d . . . H14A H 0.0796 0.3652 1.1390 0.145 Uiso 1 1 calc R . . C15 C 0.0522(7) 0.2290(9) 1.1112(7) 0.118(4) Uani 1 1 d . . . H15A H 0.0412 0.2114 1.1747 0.141 Uiso 1 1 calc R . . C16 C 0.0448(6) 0.1642(6) 1.0392(7) 0.094(3) Uani 1 1 d . . . H16A H 0.0262 0.1029 1.0536 0.112 Uiso 1 1 calc R . . C17 C 0.0642(5) 0.1877(5) 0.9462(6) 0.075(2) Uani 1 1 d . . . H17A H 0.0604 0.1421 0.8981 0.090 Uiso 1 1 calc R . . C18 C -0.1677(5) 0.2412(6) 0.8460(6) 0.087(3) Uani 1 1 d . . . H18A H -0.1687 0.3040 0.8652 0.104 Uiso 1 1 calc R . . C19 C -0.2328(6) 0.1809(6) 0.8846(7) 0.092(3) Uani 1 1 d . . . H19A H -0.2778 0.2026 0.9288 0.110 Uiso 1 1 calc R . . C20 C -0.2322(6) 0.0875(6) 0.8585(6) 0.083(3) Uani 1 1 d . . . H20A H -0.2763 0.0453 0.8849 0.099 Uiso 1 1 calc R . . C21 C -0.1663(5) 0.0582(5) 0.7937(6) 0.072(2) Uani 1 1 d . . . H21A H -0.1651 -0.0047 0.7751 0.086 Uiso 1 1 calc R . . C22 C -0.1001(5) 0.1214(5) 0.7546(5) 0.0579(18) Uani 1 1 d . . . C23 C 0.1086(5) 0.1368(4) 0.6122(5) 0.0480(16) Uani 1 1 d . . . C24 C 0.0874(6) 0.1005(5) 0.5238(6) 0.082(2) Uani 1 1 d . . . H24A H 0.0228 0.0959 0.5013 0.099 Uiso 1 1 calc R . . C25 C 0.1638(9) 0.0703(6) 0.4674(7) 0.106(4) Uani 1 1 d . . . H25A H 0.1503 0.0435 0.4073 0.127 Uiso 1 1 calc R . . C26 C 0.2572(8) 0.0796(6) 0.4989(8) 0.110(4) Uani 1 1 d . . . H26A H 0.3080 0.0606 0.4598 0.132 Uiso 1 1 calc R . . C27 C 0.2778(6) 0.1162(6) 0.5871(8) 0.098(3) Uani 1 1 d . . . H27A H 0.3426 0.1213 0.6087 0.118 Uiso 1 1 calc R . . C28 C 0.2029(5) 0.1460(5) 0.6452(6) 0.069(2) Uani 1 1 d . . . H28A H 0.2166 0.1719 0.7057 0.083 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 Os 0.04657(16) 0.04216(14) 0.0727(2) -0.00470(16) 0.02084(12) -0.00324(14) Br 0.0920(6) 0.0501(4) 0.1024(7) -0.0067(4) 0.0444(5) 0.0077(4) N1 0.043(3) 0.048(3) 0.081(5) -0.015(3) 0.018(3) -0.004(3) N2 0.047(4) 0.057(3) 0.065(4) 0.002(3) 0.011(3) -0.002(3) N3 0.048(3) 0.041(3) 0.059(4) -0.008(3) 0.014(3) -0.005(2) N4 0.074(4) 0.040(3) 0.072(4) -0.005(3) 0.030(3) -0.006(3) N5 0.048(3) 0.053(3) 0.082(4) -0.002(3) 0.025(3) -0.005(3) N6 0.062(4) 0.045(3) 0.069(4) -0.009(3) 0.010(3) -0.011(3) N7 0.050(3) 0.039(3) 0.069(4) 0.001(3) 0.007(3) 0.000(2) C1 0.052(5) 0.067(5) 0.120(8) -0.009(5) 0.015(5) -0.004(4) C2 0.077(6) 0.070(6) 0.117(9) -0.015(6) -0.016(6) -0.003(5) C3 0.080(6) 0.065(5) 0.104(8) -0.001(5) -0.025(6) -0.005(5) C4 0.069(6) 0.063(5) 0.083(7) -0.002(4) 0.002(5) -0.008(4) C5 0.055(5) 0.044(4) 0.065(5) -0.009(4) 0.004(4) 0.005(3) C6 0.039(4) 0.039(3) 0.074(5) -0.005(4) 0.002(4) -0.006(3) C7 0.056(5) 0.056(4) 0.073(6) -0.004(4) 0.012(4) -0.005(3) C8 0.053(5) 0.075(5) 0.081(6) -0.009(5) 0.017(4) -0.014(4) C9 0.056(5) 0.069(5) 0.080(6) -0.023(4) -0.004(4) -0.007(4) C10 0.075(5) 0.054(4) 0.065(5) -0.002(4) -0.006(4) -0.003(4) C11 0.057(5) 0.038(4) 0.072(6) -0.008(4) 0.006(4) 0.000(3) C12 0.063(5) 0.062(5) 0.072(6) -0.010(4) 0.015(4) -0.004(4) C13 0.142(9) 0.067(6) 0.085(7) -0.014(5) 0.040(6) -0.017(5) C14 0.181(11) 0.104(8) 0.080(8) -0.023(6) 0.047(7) -0.005(7) C15 0.138(9) 0.147(10) 0.070(7) 0.017(7) 0.036(6) -0.021(8) C16 0.106(7) 0.082(6) 0.094(8) 0.006(6) 0.030(6) -0.021(5) C17 0.081(6) 0.068(6) 0.078(6) 0.003(4) 0.017(4) -0.020(4) C18 0.070(5) 0.074(5) 0.118(7) -0.019(5) 0.054(5) -0.011(4) C19 0.067(5) 0.086(6) 0.125(8) -0.008(5) 0.043(5) -0.020(4) C20 0.069(5) 0.079(6) 0.102(7) 0.009(5) 0.029(5) -0.028(4) C21 0.058(5) 0.066(5) 0.092(6) -0.005(4) 0.009(4) -0.025(4) C22 0.049(4) 0.058(4) 0.067(5) -0.006(4) 0.016(4) -0.010(3) C23 0.060(5) 0.033(3) 0.051(5) -0.003(3) 0.016(4) -0.001(3) C24 0.104(7) 0.074(6) 0.069(6) -0.001(5) 0.004(5) 0.011(5) C25 0.180(11) 0.079(6) 0.060(7) -0.010(5) 0.036(8) 0.005(8) C26 0.146(10) 0.060(6) 0.128(11) 0.015(6) 0.094(9) 0.020(6) C27 0.066(6) 0.071(6) 0.159(10) 0.004(6) 0.046(6) 0.005(4) C28 0.058(5) 0.056(4) 0.094(6) -0.009(4) 0.016(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os N7 1.938(5) . ? Os N3 1.941(5) . ? Os N4 1.998(6) . ? Os N1 2.079(6) . ? Os N5 2.084(5) . ? Os Br 2.5321(8) . ? N1 C1 1.340(9) . ? N1 C5 1.378(8) . ? N2 N3 1.313(7) . ? N2 C5 1.353(7) . ? N3 C6 1.369(7) . ? N4 C11 1.395(8) . ? N4 C12 1.426(9) . ? N5 C18 1.349(8) . ? N5 C22 1.364(8) . ? N6 N7 1.345(6) . ? N6 C22 1.359(7) . ? N7 C23 1.433(7) . ? C1 C2 1.364(11) . ? C2 C3 1.385(11) . ? C3 C4 1.363(9) . ? C4 C5 1.392(9) . ? C6 C7 1.394(8) . ? C6 C11 1.406(9) . ? C7 C8 1.343(9) . ? C8 C9 1.378(9) . ? C9 C10 1.383(9) . ? C10 C11 1.398(9) . ? C12 C13 1.379(10) . ? C12 C17 1.393(9) . ? C13 C14 1.393(11) . ? C14 C15 1.372(12) . ? C15 C16 1.358(12) . ? C16 C17 1.362(10) . ? C18 C19 1.353(9) . ? C19 C20 1.374(10) . ? C20 C21 1.351(9) . ? C21 C22 1.392(8) . ? C23 C24 1.354(9) . ? C23 C28 1.360(9) . ? C24 C25 1.385(11) . ? C25 C26 1.344(13) . ? C26 C27 1.350(12) . ? C27 C28 1.383(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 N7 Os N3 97.7(2) . . ? N7 Os N4 100.1(2) . . ? N3 Os N4 80.5(2) . . ? N7 Os N1 92.5(2) . . ? N3 Os N1 77.3(2) . . ? N4 Os N1 155.7(2) . . ? N7 Os N5 75.5(2) . . ? N3 Os N5 173.2(2) . . ? N4 Os N5 100.3(2) . . ? N1 Os N5 102.9(2) . . ? N7 Os Br 167.59(15) . . ? N3 Os Br 93.67(14) . . ? N4 Os Br 86.63(14) . . ? N1 Os Br 85.19(13) . . ? N5 Os Br 93.12(15) . . ? C1 N1 C5 118.9(7) . . ? C1 N1 Os 132.1(6) . . ? C5 N1 Os 108.9(5) . . ? N3 N2 C5 110.4(5) . . ? N2 N3 C6 121.0(5) . . ? N2 N3 Os 122.0(4) . . ? C6 N3 Os 117.0(5) . . ? C11 N4 C12 119.1(6) . . ? C11 N4 Os 113.8(5) . . ? C12 N4 Os 126.5(4) . . ? C18 N5 C22 117.8(6) . . ? C18 N5 Os 129.3(5) . . ? C22 N5 Os 112.9(4) . . ? N7 N6 C22 110.3(5) . . ? N6 N7 C23 112.1(5) . . ? N6 N7 Os 123.2(4) . . ? C23 N7 Os 124.6(4) . . ? N1 C1 C2 122.2(8) . . ? C1 C2 C3 120.3(9) . . ? C4 C3 C2 117.8(8) . . ? C3 C4 C5 121.4(8) . . ? N2 C5 N1 120.6(7) . . ? N2 C5 C4 120.0(7) . . ? N1 C5 C4 119.3(7) . . ? N3 C6 C7 124.1(7) . . ? N3 C6 C11 114.2(6) . . ? C7 C6 C11 121.7(6) . . ? C8 C7 C6 119.4(7) . . ? C7 C8 C9 120.0(7) . . ? C8 C9 C10 122.4(7) . . ? C9 C10 C11 118.7(7) . . ? N4 C11 C10 127.7(7) . . ? N4 C11 C6 114.4(6) . . ? C10 C11 C6 117.8(6) . . ? C13 C12 C17 119.1(7) . . ? C13 C12 N4 122.8(7) . . ? C17 C12 N4 118.1(7) . . ? C12 C13 C14 119.5(8) . . ? C15 C14 C13 120.2(9) . . ? C16 C15 C14 119.8(9) . . ? C15 C16 C17 121.0(8) . . ? C16 C17 C12 120.2(8) . . ? N5 C18 C19 122.7(7) . . ? C18 C19 C20 119.9(8) . . ? C21 C20 C19 118.6(7) . . ? C20 C21 C22 120.6(7) . . ? N6 C22 N5 117.9(5) . . ? N6 C22 C21 121.7(6) . . ? N5 C22 C21 120.3(6) . . ? C24 C23 C28 121.4(7) . . ? C24 C23 N7 119.4(7) . . ? C28 C23 N7 119.2(6) . . ? C23 C24 C25 118.7(9) . . ? C26 C25 C24 120.5(10) . . ? C25 C26 C27 120.5(9) . . ? C26 C27 C28 120.2(9) . . ? C23 C28 C27 118.7(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.938 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.110 #CIF For Os[(HLa)(PaP)Br2], 4a data_ic7582 _database_code_CSD 157838 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H23 Br2 N7 Os' _chemical_formula_weight 807.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 38.4934(7) _cell_length_b 38.4934(7) _cell_length_c 9.7379(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12495.9(4) _cell_formula_units_Z 18 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method ? _exptl_crystal_F_000 6948 _exptl_absorpt_coefficient_mu 7.501 _exptl_absorpt_correction_type ' empirical used sadabs' _exptl_absorpt_correction_T_min 0.1520 _exptl_absorpt_correction_T_max 0.4929 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART 1K CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24176 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6362 _reflns_number_observed 5588 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0363P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000176(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6362 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_obs 0.0285 _refine_ls_wR_factor_all 0.0726 _refine_ls_wR_factor_obs 0.0611 _refine_ls_goodness_of_fit_all 1.150 _refine_ls_goodness_of_fit_obs 1.035 _refine_ls_restrained_S_all 1.150 _refine_ls_restrained_S_obs 1.035 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os Os 0.602546(4) 0.065347(4) 0.123677(15) 0.01725(6) Uani 1 d . . Br1 Br 0.652015(12) 0.136633(12) 0.04585(5) 0.02807(11) Uani 1 d . . Br2 Br 0.659546(13) 0.059817(14) 0.23391(5) 0.03117(11) Uani 1 d . . N1 N 0.61285(9) 0.05048(9) -0.0723(3) 0.0195(7) Uani 1 d . . N2 N 0.56236(10) 0.06534(10) -0.1265(3) 0.0237(7) Uani 1 d . . N3 N 0.56200(9) 0.06757(9) 0.0078(3) 0.0201(7) Uani 1 d . . N4 N 0.56662(12) 0.14221(11) -0.0286(5) 0.0425(11) Uani 1 d . . H4A H 0.58092(12) 0.13571(11) -0.0821(5) 0.051 Uiso 1 calc R . N5 N 0.56666(9) 0.00945(9) 0.2046(3) 0.0197(7) Uani 1 d . . N6 N 0.55834(11) 0.04678(11) 0.3787(3) 0.0262(8) Uani 1 d . . N7 N 0.58316(10) 0.07612(10) 0.2992(3) 0.0207(7) Uani 1 d . . C1 C 0.63914(12) 0.03876(12) -0.1147(5) 0.0271(9) Uani 1 d . . H1A H 0.65445(12) 0.03425(12) -0.0480(5) 0.033 Uiso 1 calc R . C2 C 0.64425(13) 0.03322(13) -0.2516(5) 0.0314(10) Uani 1 d . . H2A H 0.66240(13) 0.02443(13) -0.2775(5) 0.038 Uiso 1 calc R . C3 C 0.62295(14) 0.04044(13) -0.3516(5) 0.0345(11) Uani 1 d . . H3A H 0.62660(14) 0.03710(13) -0.4462(5) 0.041 Uiso 1 calc R . C4 C 0.59634(13) 0.05260(13) -0.3106(4) 0.0307(10) Uani 1 d . . H4B H 0.58166(13) 0.05817(13) -0.3768(4) 0.037 Uiso 1 calc R . C5 C 0.59124(12) 0.05663(12) -0.1702(4) 0.0218(8) Uani 1 d . . C6 C 0.53018(11) 0.07397(12) 0.0582(4) 0.0201(8) Uani 1 d . . C7 C 0.49816(12) 0.04352(12) 0.1292(4) 0.0249(9) Uani 1 d . . H7A H 0.49681(12) 0.01842(12) 0.1425(4) 0.030 Uiso 1 calc R . C8 C 0.46799(12) 0.04982(13) 0.1810(5) 0.0299(10) Uani 1 d . . H8A H 0.44633(12) 0.02931(13) 0.2315(5) 0.036 Uiso 1 calc R . C9 C 0.46987(12) 0.08633(13) 0.1580(5) 0.0302(10) Uani 1 d . . H9A H 0.44896(12) 0.09043(13) 0.1909(5) 0.036 Uiso 1 calc R . C10 C 0.50208(13) 0.11707(13) 0.0872(5) 0.0291(10) Uani 1 d . . H10A H 0.50271(13) 0.14175(13) 0.0719(5) 0.035 Uiso 1 calc R . C11 C 0.53346(12) 0.11203(12) 0.0383(4) 0.0258(9) Uani 1 d . . C12 C 0.57830(13) 0.18350(13) -0.0135(5) 0.0296(10) Uani 1 d . . C13 C 0.56237(15) 0.2007(2) -0.0985(5) 0.0403(12) Uani 1 d . . H13A H 0.54258(15) 0.1849(2) -0.1646(5) 0.048 Uiso 1 calc R . C14 C 0.5756(2) 0.2416(2) -0.0865(6) 0.0499(15) Uani 1 d . . H14A H 0.5642(2) 0.2535(2) -0.1430(6) 0.060 Uiso 1 calc R . C15 C 0.6048(2) 0.2647(2) 0.0063(6) 0.0500(15) Uani 1 d . . H15A H 0.6143(2) 0.2926(2) 0.0120(6) 0.060 Uiso 1 calc R . C16 C 0.6203(2) 0.2476(2) 0.0905(6) 0.055(2) Uani 1 d . . H16A H 0.6402(2) 0.2636(2) 0.1560(6) 0.066 Uiso 1 calc R . C17 C 0.6071(2) 0.2071(2) 0.0809(5) 0.0436(12) Uani 1 d . . H17A H 0.6181(2) 0.1954(2) 0.1401(5) 0.052 Uiso 1 calc R . C18 C 0.56046(12) -0.02597(12) 0.1547(4) 0.0229(8) Uani 1 d . . H18A H 0.57205(12) -0.02635(12) 0.0690(4) 0.027 Uiso 1 calc R . C19 C 0.53797(13) -0.06140(13) 0.2239(5) 0.0303(10) Uani 1 d . . H19A H 0.53420(13) -0.08587(13) 0.1868(5) 0.036 Uiso 1 calc R . C20 C 0.52064(15) -0.06101(14) 0.3500(5) 0.0384(12) Uani 1 d . . H20A H 0.50484(15) -0.08527(14) 0.3991(5) 0.046 Uiso 1 calc R . C21 C 0.52670(14) -0.02529(14) 0.4019(5) 0.0341(10) Uani 1 d . . H21A H 0.51499(14) -0.02449(14) 0.4869(5) 0.041 Uiso 1 calc R . C22 C 0.55045(12) 0.01002(13) 0.3276(4) 0.0244(9) Uani 1 d . . C23 C 0.59036(12) 0.11435(12) 0.3509(4) 0.0225(8) Uani 1 d . . C24 C 0.55740(13) 0.11886(13) 0.3828(4) 0.0268(9) Uani 1 d . . H24A H 0.53087(13) 0.09733(13) 0.3686(4) 0.032 Uiso 1 calc R . C25 C 0.56393(14) 0.15524(14) 0.4355(5) 0.0347(11) Uani 1 d . . H25A H 0.54176(14) 0.15874(14) 0.4564(5) 0.042 Uiso 1 calc R . C26 C 0.6027(2) 0.18640(14) 0.4577(5) 0.0386(12) Uani 1 d . . H26A H 0.6070(2) 0.21108(14) 0.4947(5) 0.046 Uiso 1 calc R . C27 C 0.63531(15) 0.18158(14) 0.4259(5) 0.0372(11) Uani 1 d . . H27A H 0.66182(15) 0.20296(14) 0.4417(5) 0.045 Uiso 1 calc R . C28 C 0.62920(13) 0.14550(13) 0.3708(4) 0.0292(9) Uani 1 d . . H28A H 0.65141(13) 0.14233(13) 0.3472(4) 0.035 Uiso 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 Os 0.01864(9) 0.01871(9) 0.01550(9) -0.00081(6) -0.00028(6) 0.01016(6) Br1 0.0230(2) 0.0215(2) 0.0363(3) 0.0009(2) 0.0048(2) 0.0086(2) Br2 0.0298(2) 0.0396(3) 0.0311(2) -0.0058(2) -0.0093(2) 0.0226(2) N1 0.021(2) 0.018(2) 0.019(2) -0.0006(13) 0.0018(13) 0.0091(14) N2 0.027(2) 0.027(2) 0.019(2) -0.0013(14) -0.0027(14) 0.014(2) N3 0.020(2) 0.018(2) 0.020(2) 0.0010(13) -0.0017(13) 0.0083(14) N4 0.039(2) 0.027(2) 0.067(3) 0.012(2) 0.027(2) 0.020(2) N5 0.023(2) 0.022(2) 0.016(2) -0.0003(13) -0.0032(13) 0.0122(14) N6 0.035(2) 0.031(2) 0.018(2) 0.0021(15) 0.0037(15) 0.020(2) N7 0.023(2) 0.024(2) 0.017(2) -0.0032(14) -0.0043(13) 0.0139(14) C1 0.022(2) 0.025(2) 0.031(2) 0.000(2) 0.003(2) 0.009(2) C2 0.027(2) 0.030(2) 0.035(3) -0.006(2) 0.009(2) 0.012(2) C3 0.040(3) 0.034(2) 0.022(2) -0.004(2) 0.009(2) 0.013(2) C4 0.038(3) 0.033(2) 0.020(2) 0.000(2) 0.000(2) 0.017(2) C5 0.025(2) 0.020(2) 0.017(2) 0.000(2) 0.000(2) 0.008(2) C6 0.018(2) 0.026(2) 0.017(2) -0.002(2) -0.0017(15) 0.012(2) C7 0.026(2) 0.022(2) 0.023(2) -0.002(2) -0.004(2) 0.009(2) C8 0.019(2) 0.028(2) 0.035(3) 0.002(2) 0.003(2) 0.006(2) C9 0.021(2) 0.035(2) 0.035(3) -0.008(2) 0.000(2) 0.015(2) C10 0.026(2) 0.030(2) 0.035(3) -0.002(2) 0.002(2) 0.017(2) C11 0.026(2) 0.027(2) 0.027(2) 0.000(2) 0.001(2) 0.014(2) C12 0.026(2) 0.026(2) 0.039(3) 0.009(2) 0.011(2) 0.015(2) C13 0.033(3) 0.043(3) 0.048(3) 0.005(2) -0.001(2) 0.021(2) C14 0.058(4) 0.047(3) 0.061(4) 0.027(3) 0.018(3) 0.039(3) C15 0.050(3) 0.025(2) 0.071(4) 0.005(3) 0.024(3) 0.016(2) C16 0.045(3) 0.056(4) 0.061(4) -0.019(3) -0.002(3) 0.023(3) C17 0.050(3) 0.055(3) 0.036(3) 0.002(2) 0.001(2) 0.034(3) C18 0.028(2) 0.023(2) 0.021(2) -0.001(2) -0.001(2) 0.016(2) C19 0.033(2) 0.023(2) 0.035(3) -0.001(2) -0.003(2) 0.014(2) C20 0.046(3) 0.031(2) 0.042(3) 0.016(2) 0.014(2) 0.022(2) C21 0.043(3) 0.033(2) 0.029(2) 0.011(2) 0.015(2) 0.021(2) C22 0.028(2) 0.029(2) 0.020(2) 0.004(2) 0.002(2) 0.017(2) C23 0.028(2) 0.023(2) 0.018(2) -0.004(2) -0.004(2) 0.013(2) C24 0.028(2) 0.031(2) 0.026(2) -0.005(2) -0.002(2) 0.019(2) C25 0.039(3) 0.040(3) 0.035(3) -0.007(2) 0.000(2) 0.028(2) C26 0.049(3) 0.031(2) 0.043(3) -0.015(2) -0.009(2) 0.025(2) C27 0.034(3) 0.033(2) 0.042(3) -0.013(2) -0.011(2) 0.015(2) C28 0.029(2) 0.035(2) 0.027(2) -0.008(2) -0.006(2) 0.018(2) _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 Os N3 1.962(3) . ? Os N7 1.990(3) . ? Os N5 2.046(3) . ? Os N1 2.086(3) . ? Os Br2 2.5454(4) . ? Os Br1 2.5505(4) . ? N1 C5 1.362(5) . ? N1 C1 1.362(5) . ? N2 N3 1.311(4) . ? N2 C5 1.379(5) . ? N3 C6 1.450(5) . ? N4 C11 1.386(5) . ? N4 C12 1.427(5) . ? N5 C18 1.352(5) . ? N5 C22 1.356(5) . ? N6 N7 1.307(5) . ? N6 C22 1.383(5) . ? N7 C23 1.445(5) . ? C1 C2 1.379(6) . ? C2 C3 1.388(7) . ? C3 C4 1.381(6) . ? C4 C5 1.400(6) . ? C6 C7 1.388(5) . ? C6 C11 1.419(6) . ? C7 C8 1.394(6) . ? C8 C9 1.389(6) . ? C9 C10 1.395(6) . ? C10 C11 1.399(6) . ? C12 C17 1.376(7) . ? C12 C13 1.382(6) . ? C13 C14 1.397(7) . ? C14 C15 1.368(8) . ? C15 C16 1.362(8) . ? C16 C17 1.380(8) . ? C18 C19 1.372(6) . ? C19 C20 1.401(6) . ? C20 C21 1.371(6) . ? C21 C22 1.401(6) . ? C23 C28 1.385(6) . ? C23 C24 1.399(5) . ? C24 C25 1.391(6) . ? C25 C26 1.386(7) . ? C26 C27 1.393(6) . ? C27 C28 1.395(6) . ? 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 N3 Os N7 95.46(13) . . ? N3 Os N5 97.69(13) . . ? N7 Os N5 76.23(13) . . ? N3 Os N1 75.57(13) . . ? N7 Os N1 170.16(12) . . ? N5 Os N1 100.65(12) . . ? N3 Os Br2 169.71(10) . . ? N7 Os Br2 94.82(9) . . ? N5 Os Br2 84.64(9) . . ? N1 Os Br2 94.16(9) . . ? N3 Os Br1 87.96(9) . . ? N7 Os Br1 100.78(9) . . ? N5 Os Br1 173.80(9) . . ? N1 Os Br1 83.18(9) . . ? Br2 Os Br1 90.24(2) . . ? C5 N1 C1 117.7(3) . . ? C5 N1 Os 112.1(2) . . ? C1 N1 Os 130.0(3) . . ? N3 N2 C5 111.1(3) . . ? N2 N3 C6 112.7(3) . . ? N2 N3 Os 122.4(3) . . ? C6 N3 Os 124.8(3) . . ? C11 N4 C12 122.0(4) . . ? C18 N5 C22 118.9(3) . . ? C18 N5 Os 127.5(3) . . ? C22 N5 Os 113.4(3) . . ? N7 N6 C22 111.2(3) . . ? N6 N7 C23 111.0(3) . . ? N6 N7 Os 121.2(3) . . ? C23 N7 Os 127.6(3) . . ? N1 C1 C2 122.1(4) . . ? C1 C2 C3 120.2(4) . . ? C4 C3 C2 118.5(4) . . ? C3 C4 C5 119.3(4) . . ? N1 C5 N2 117.6(3) . . ? N1 C5 C4 122.2(4) . . ? N2 C5 C4 120.2(4) . . ? C7 C6 C11 121.5(4) . . ? C7 C6 N3 119.6(3) . . ? C11 C6 N3 118.8(3) . . ? C6 C7 C8 119.9(4) . . ? C9 C8 C7 119.4(4) . . ? C8 C9 C10 120.8(4) . . ? C11 C10 C9 120.9(4) . . ? N4 C11 C10 122.7(4) . . ? N4 C11 C6 119.9(4) . . ? C10 C11 C6 117.3(4) . . ? C17 C12 C13 119.3(4) . . ? C17 C12 N4 120.3(4) . . ? C13 C12 N4 120.3(4) . . ? C12 C13 C14 119.5(5) . . ? C15 C14 C13 120.3(5) . . ? C14 C15 C16 120.1(5) . . ? C15 C16 C17 120.2(5) . . ? C16 C17 C12 120.6(5) . . ? N5 C18 C19 122.1(4) . . ? C18 C19 C20 119.1(4) . . ? C21 C20 C19 119.4(4) . . ? C20 C21 C22 118.9(4) . . ? N5 C22 N6 117.8(4) . . ? N5 C22 C21 121.5(4) . . ? N6 C22 C21 120.6(4) . . ? C28 C23 C24 121.0(4) . . ? C28 C23 N7 120.3(4) . . ? C24 C23 N7 118.7(4) . . ? C25 C24 C23 119.2(4) . . ? C26 C25 C24 120.2(4) . . ? C25 C26 C27 120.1(4) . . ? C26 C27 C28 120.2(4) . . ? C23 C28 C27 119.2(4) . . ? _refine_diff_density_max 1.630 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.208