Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Minna Jakonen' 'Pipsa Hirva' 'Matti Haukka' 'Sylvie Chardon-Noblat' 'Frederic Lafolet' 'Jerome Chauvin' 'Alain Deronzier' _publ_contact_author_name 'Matti Haukka' _publ_contact_author_address ; Department of Chemistry University of Joensuu P.O.Box 111 Joensuu FI-80101 FINLAND ; _publ_contact_author_email MATTI.HAUKKA@JOENSUU.FI _publ_section_title ;An Alternative Synthesis Method for [Os(NN)(CO)2Cl2] Complexes (NN = 2,2-bipyridine, 4,4-dimethyl-2,2-bipyridine; X = Cl, Br, I). Electrochemical and Photochemical Properties and Behavior. ; # Attachment 'B704931E.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 642573' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Cl2 N2 O2 Os' _chemical_formula_sum 'C12 H8 Cl2 N2 O2 Os' _chemical_formula_weight 473.30 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' O O 0.0106 0.0060 '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' 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 'P n' _symmetry_space_group_name_Hall 'P -2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.1820(6) _cell_length_b 6.8180(3) _cell_length_c 12.4450(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.171(3) _cell_angle_gamma 90.00 _cell_volume 673.12(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1916 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 9.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4183 _exptl_absorpt_correction_T_max 0.6129 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H atoms were positioned geometrically and allowed to ride on their parent atoms, with C---H = 0.95 \%A, and U~iso~ = 1.2 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5285 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2498 _reflns_number_gt 2344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _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^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(13) _chemical_absolute_configuration unk _refine_ls_number_reflns 2498 _refine_ls_number_parameters 172 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.108 _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 Os1 Os 0.96217(6) 0.78237(4) 0.09967(6) 0.02121(9) Uani 1 1 d . . . Cl1 Cl 1.1280(3) 0.5921(3) 0.24842(18) 0.0302(5) Uani 1 1 d . . . Cl2 Cl 0.8220(3) 0.9627(3) -0.06130(17) 0.0289(5) Uani 1 1 d . . . O1 O 0.8452(9) 1.0632(11) 0.2514(6) 0.0425(17) Uani 1 1 d . . . O2 O 0.6599(11) 0.5348(11) 0.0905(6) 0.0475(19) Uani 1 1 d . . . N1 N 1.0683(9) 0.6101(10) -0.0067(5) 0.0228(15) Uani 1 1 d . . . N2 N 1.1837(9) 0.9406(10) 0.0970(5) 0.0225(15) Uani 1 1 d . . . C1 C 0.8856(11) 0.9591(13) 0.1970(7) 0.0250(19) Uani 1 1 d . . . C2 C 0.7671(12) 0.6213(15) 0.0927(7) 0.0259(19) Uani 1 1 d . . . C10 C 1.0053(11) 0.4423(12) -0.0551(6) 0.0254(19) Uani 1 1 d . . . H10 H 0.9015 0.3959 -0.0435 0.030 Uiso 1 1 calc R . . C11 C 1.0858(12) 0.3313(13) -0.1225(7) 0.030(2) Uani 1 1 d . . . H11 H 1.0387 0.2124 -0.1562 0.036 Uiso 1 1 calc R . . C12 C 1.2364(13) 0.4030(13) -0.1375(8) 0.031(2) Uani 1 1 d . . . H12 H 1.2960 0.3311 -0.1811 0.037 Uiso 1 1 calc R . . C13 C 1.3004(12) 0.5757(13) -0.0905(7) 0.030(2) Uani 1 1 d . . . H13 H 1.4022 0.6260 -0.1033 0.036 Uiso 1 1 calc R . . C14 C 1.2177(11) 0.6768(12) -0.0245(7) 0.0231(18) Uani 1 1 d . . . C15 C 1.2800(11) 0.8636(13) 0.0326(7) 0.0259(18) Uani 1 1 d . . . C16 C 1.4261(10) 0.9530(13) 0.0231(8) 0.029(2) Uani 1 1 d . . . H16 H 1.4927 0.8958 -0.0214 0.034 Uiso 1 1 calc R . . C17 C 1.4749(17) 1.1250(14) 0.0779(9) 0.034(3) Uani 1 1 d . . . H17 H 1.5737 1.1904 0.0698 0.041 Uiso 1 1 calc R . . C18 C 1.3805(13) 1.2030(14) 0.1449(8) 0.032(2) Uani 1 1 d . . . H18 H 1.4148 1.3202 0.1854 0.039 Uiso 1 1 calc R . . C19 C 1.2351(12) 1.1075(13) 0.1522(7) 0.030(2) Uani 1 1 d . . . H19 H 1.1690 1.1617 0.1978 0.036 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 Os1 0.01989(14) 0.02115(14) 0.02328(14) -0.0005(4) 0.00658(9) -0.0027(4) Cl1 0.0299(12) 0.0298(12) 0.0300(11) 0.0046(8) 0.0054(9) 0.0038(9) Cl2 0.0266(12) 0.0317(12) 0.0279(10) 0.0042(9) 0.0056(9) -0.0026(9) O1 0.040(5) 0.047(5) 0.043(4) -0.002(3) 0.013(3) 0.010(3) O2 0.056(6) 0.040(5) 0.043(4) -0.002(3) 0.005(4) -0.001(4) N1 0.022(4) 0.022(4) 0.023(4) 0.003(3) 0.002(3) 0.000(3) N2 0.019(4) 0.026(4) 0.022(4) 0.000(3) 0.004(3) -0.002(3) C1 0.019(5) 0.023(5) 0.034(5) 0.009(4) 0.007(4) -0.006(3) C2 0.024(5) 0.038(6) 0.019(4) 0.013(4) 0.012(4) 0.013(4) C10 0.025(5) 0.027(5) 0.024(4) -0.001(3) 0.005(4) -0.002(4) C11 0.037(5) 0.023(5) 0.031(5) -0.005(3) 0.011(4) 0.003(4) C12 0.035(6) 0.028(5) 0.033(5) 0.006(4) 0.017(4) 0.004(4) C13 0.030(5) 0.027(5) 0.039(5) 0.007(4) 0.021(5) 0.001(4) C14 0.027(5) 0.021(5) 0.022(4) 0.005(3) 0.008(3) 0.004(3) C15 0.022(5) 0.026(5) 0.030(4) 0.005(3) 0.006(4) 0.004(3) C16 0.013(5) 0.034(5) 0.040(5) 0.004(4) 0.008(4) 0.002(3) C17 0.026(6) 0.026(5) 0.048(9) 0.006(5) 0.006(5) -0.005(5) C18 0.029(6) 0.026(5) 0.039(6) 0.000(4) 0.001(4) -0.004(4) C19 0.030(5) 0.033(5) 0.026(5) 0.001(4) 0.003(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 Os1 C1 1.919(10) . yes Os1 C2 1.922(11) . yes Os1 N1 2.109(7) . yes Os1 N2 2.117(7) . yes Os1 Cl2 2.391(2) . yes Os1 Cl1 2.392(2) . yes O1 C1 1.087(11) . ? O2 C2 1.052(11) . ? N1 C10 1.336(11) . ? N1 C14 1.373(11) . ? N2 C19 1.342(11) . ? N2 C15 1.359(11) . ? C10 C11 1.408(12) . ? C10 H10 0.9500 . ? C11 C12 1.379(13) . ? C11 H11 0.9500 . ? C12 C13 1.361(13) . ? C12 H12 0.9500 . ? C13 C14 1.371(12) . ? C13 H13 0.9500 . ? C14 C15 1.487(12) . ? C15 C16 1.373(12) . ? C16 C17 1.366(14) . ? C16 H16 0.9500 . ? C17 C18 1.374(15) . ? C17 H17 0.9500 . ? C18 C19 1.379(14) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Os1 C2 89.5(4) . . yes C1 Os1 N1 173.7(3) . . ? C2 Os1 N1 96.8(3) . . ? C1 Os1 N2 95.9(3) . . ? C2 Os1 N2 174.6(3) . . ? N1 Os1 N2 77.8(3) . . yes C1 Os1 Cl2 92.4(2) . . ? C2 Os1 Cl2 91.9(2) . . ? N1 Os1 Cl2 86.98(19) . . ? N2 Os1 Cl2 87.81(18) . . ? C1 Os1 Cl1 93.6(3) . . ? C2 Os1 Cl1 91.9(2) . . ? N1 Os1 Cl1 86.61(18) . . ? N2 Os1 Cl1 87.87(19) . . ? Cl2 Os1 Cl1 172.91(8) . . yes C10 N1 C14 118.1(7) . . ? C10 N1 Os1 126.0(6) . . ? C14 N1 Os1 115.9(5) . . ? C19 N2 C15 118.4(8) . . ? C19 N2 Os1 125.9(6) . . ? C15 N2 Os1 115.7(6) . . ? O1 C1 Os1 178.0(8) . . ? O2 C2 Os1 178.7(9) . . ? N1 C10 C11 123.0(8) . . ? N1 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C12 C11 C10 117.0(8) . . ? C12 C11 H11 121.5 . . ? C10 C11 H11 121.5 . . ? C13 C12 C11 120.7(8) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.9(8) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 N1 121.3(8) . . ? C13 C14 C15 123.8(8) . . ? N1 C14 C15 114.9(7) . . ? N2 C15 C16 121.5(8) . . ? N2 C15 C14 115.7(7) . . ? C16 C15 C14 122.9(8) . . ? C17 C16 C15 119.5(9) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 119.7(10) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C19 118.6(9) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? N2 C19 C18 122.3(9) . . ? N2 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.065 _refine_diff_density_min -1.482 _refine_diff_density_rms 0.186 #===END======================================================================== data_1B _database_code_depnum_ccdc_archive 'CCDC 642574' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Cl2 N2 O2 Os' _chemical_formula_sum 'C12 H8 Cl2 N2 O2 Os' _chemical_formula_weight 473.30 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' O O 0.0106 0.0060 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 8.0674(16) _cell_length_b 15.938(3) _cell_length_c 10.325(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.20(3) _cell_angle_gamma 90.00 _cell_volume 1302.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3506 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 10.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3262 _exptl_absorpt_correction_T_max 0.6665 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; The H atoms were positioned geometrically and allowed to ride on their parent atoms, with C---H = 0.95 \%A, and U~iso~ = 1.2 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9208 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2978 _reflns_number_gt 2130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _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^)+(0.0124P)^2^+0.5607P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2978 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 Os1 Os 0.73001(3) 0.155737(15) 0.71859(2) 0.01664(7) Uani 1 1 d . . . Cl1 Cl 0.65308(16) 0.01131(9) 0.69540(13) 0.0227(3) Uani 1 1 d . . . Cl2 Cl 0.84512(17) 0.29338(10) 0.72904(14) 0.0262(3) Uani 1 1 d . . . O1 O 0.6179(5) 0.1624(3) 0.9794(4) 0.0316(10) Uani 1 1 d . . . O2 O 0.3902(5) 0.2183(3) 0.5853(4) 0.0313(11) Uani 1 1 d . . . N1 N 0.8248(5) 0.1429(3) 0.5437(4) 0.0167(11) Uani 1 1 d . . . N2 N 0.9795(5) 0.1123(3) 0.7864(4) 0.0183(10) Uani 1 1 d . . . C1 C 0.6620(6) 0.1617(4) 0.8830(6) 0.0228(13) Uani 1 1 d . . . C2 C 0.5152(7) 0.1945(4) 0.6358(5) 0.0197(13) Uani 1 1 d . . . C10 C 0.7395(7) 0.1616(4) 0.4237(5) 0.0225(13) Uani 1 1 d . . . H10 H 0.6258 0.1800 0.4140 0.027 Uiso 1 1 calc R . . C11 C 0.8098(7) 0.1553(4) 0.3136(5) 0.0246(13) Uani 1 1 d . . . H11 H 0.7456 0.1692 0.2291 0.030 Uiso 1 1 calc R . . C12 C 0.9733(7) 0.1290(4) 0.3264(5) 0.0239(14) Uani 1 1 d . . . H12 H 1.0244 0.1246 0.2512 0.029 Uiso 1 1 calc R . . C13 C 1.0623(7) 0.1089(4) 0.4494(5) 0.0198(13) Uani 1 1 d . . . H13 H 1.1762 0.0906 0.4601 0.024 Uiso 1 1 calc R . . C14 C 0.9862(6) 0.1155(4) 0.5574(5) 0.0165(12) Uani 1 1 d . . . C15 C 1.0692(6) 0.0951(4) 0.6927(5) 0.0177(13) Uani 1 1 d . . . C16 C 1.2286(7) 0.0600(4) 0.7256(6) 0.0248(13) Uani 1 1 d . . . H16 H 1.2909 0.0476 0.6587 0.030 Uiso 1 1 calc R . . C17 C 1.2964(7) 0.0432(4) 0.8561(6) 0.0264(15) Uani 1 1 d . . . H17 H 1.4049 0.0181 0.8797 0.032 Uiso 1 1 calc R . . C18 C 1.2080(6) 0.0627(4) 0.9497(5) 0.0244(14) Uani 1 1 d . . . H18 H 1.2544 0.0526 1.0401 0.029 Uiso 1 1 calc R . . C19 C 1.0495(7) 0.0975(4) 0.9132(5) 0.0239(14) Uani 1 1 d . . . H19 H 0.9878 0.1114 0.9799 0.029 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 Os1 0.01360(10) 0.02191(13) 0.01445(10) 0.00061(12) 0.00283(8) 0.00158(12) Cl1 0.0216(7) 0.0216(8) 0.0257(7) -0.0002(6) 0.0064(6) 0.0002(6) Cl2 0.0240(7) 0.0270(9) 0.0270(8) -0.0009(7) 0.0032(7) -0.0032(7) O1 0.030(2) 0.048(3) 0.019(2) -0.007(2) 0.0085(18) -0.011(2) O2 0.023(2) 0.041(3) 0.028(2) -0.001(2) 0.001(2) 0.009(2) N1 0.015(2) 0.017(3) 0.017(2) 0.003(2) 0.0025(19) 0.002(2) N2 0.013(2) 0.023(3) 0.018(2) 0.001(2) 0.002(2) -0.002(2) C1 0.015(3) 0.024(4) 0.028(3) -0.002(3) 0.000(3) 0.005(3) C2 0.027(3) 0.014(3) 0.020(3) -0.003(3) 0.009(3) -0.006(3) C10 0.021(3) 0.026(4) 0.021(3) 0.000(3) 0.002(2) 0.001(3) C11 0.024(3) 0.030(3) 0.022(3) -0.003(3) 0.008(2) -0.003(3) C12 0.031(3) 0.023(4) 0.022(3) -0.008(3) 0.015(3) -0.011(3) C13 0.017(3) 0.019(3) 0.024(3) -0.001(3) 0.007(3) -0.001(3) C14 0.015(3) 0.019(3) 0.016(3) -0.001(3) 0.002(2) -0.006(2) C15 0.009(3) 0.025(4) 0.018(3) 0.003(2) 0.000(2) -0.004(2) C16 0.016(3) 0.026(3) 0.034(3) -0.003(3) 0.007(2) -0.003(3) C17 0.012(3) 0.029(4) 0.034(4) 0.008(3) -0.005(3) -0.003(3) C18 0.016(3) 0.036(4) 0.018(3) 0.010(3) -0.003(3) 0.001(3) C19 0.021(3) 0.035(4) 0.015(3) 0.005(3) 0.002(3) -0.003(3) _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 Os1 C2 1.882(6) . yes Os1 C1 1.885(6) . yes Os1 N1 2.104(4) . yes Os1 N2 2.114(4) . yes Os1 Cl2 2.3764(16) . yes Os1 Cl1 2.3839(15) . yes O1 C1 1.120(6) . ? O2 C2 1.109(6) . ? N1 C10 1.329(6) . ? N1 C14 1.354(6) . ? N2 C19 1.343(6) . ? N2 C15 1.343(7) . ? C10 C11 1.369(7) . ? C10 H10 0.9500 . ? C11 C12 1.365(8) . ? C11 H11 0.9500 . ? C12 C13 1.369(7) . ? C12 H12 0.9500 . ? C13 C14 1.378(7) . ? C13 H13 0.9500 . ? C14 C15 1.464(7) . ? C15 C16 1.384(7) . ? C16 C17 1.378(7) . ? C16 H16 0.9500 . ? C17 C18 1.344(8) . ? C17 H17 0.9500 . ? C18 C19 1.377(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Os1 C1 89.4(2) . . yes C2 Os1 N1 95.6(2) . . ? C1 Os1 N1 174.9(2) . . ? C2 Os1 N2 172.4(2) . . ? C1 Os1 N2 98.23(19) . . ? N1 Os1 N2 76.77(16) . . yes C2 Os1 Cl2 91.99(17) . . ? C1 Os1 Cl2 95.29(19) . . ? N1 Os1 Cl2 85.69(13) . . ? N2 Os1 Cl2 87.06(13) . . ? C2 Os1 Cl1 94.16(17) . . ? C1 Os1 Cl1 91.34(19) . . ? N1 Os1 Cl1 87.17(13) . . ? N2 Os1 Cl1 85.97(13) . . ? Cl2 Os1 Cl1 171.00(5) . . yes C10 N1 C14 118.9(4) . . ? C10 N1 Os1 124.8(3) . . ? C14 N1 Os1 116.4(3) . . ? C19 N2 C15 118.9(4) . . ? C19 N2 Os1 125.0(4) . . ? C15 N2 Os1 116.1(3) . . ? O1 C1 Os1 177.2(6) . . ? O2 C2 Os1 178.5(5) . . ? N1 C10 C11 122.3(5) . . ? N1 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 119.3(5) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 119.0(5) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C12 C13 C14 119.8(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? N1 C14 C13 120.7(5) . . ? N1 C14 C15 115.0(4) . . ? C13 C14 C15 124.2(5) . . ? N2 C15 C16 120.8(5) . . ? N2 C15 C14 115.6(4) . . ? C16 C15 C14 123.7(5) . . ? C17 C16 C15 119.4(6) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.4(5) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? N2 C19 C18 122.0(5) . . ? N2 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.230 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.222 #===END======================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 642575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H12 Cl2 N2 O2 Os' _chemical_formula_sum 'C14 H12 Cl2 N2 O2 Os' _chemical_formula_weight 501.36 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' O O 0.0106 0.0060 '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' 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 6.3432(3) _cell_length_b 18.1482(9) _cell_length_c 13.4114(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.766(3) _cell_angle_gamma 90.00 _cell_volume 1511.45(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5644 _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 8.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3483 _exptl_absorpt_correction_T_max 0.8369 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; Hydrogens were positioned geometrically and were constrained to ride on their parent atoms, with C---H =0.95-0.98 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5644 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1733 _reflns_number_gt 1587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _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^)+(0.0174P)^2^+1.9241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1733 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.5000 -0.106072(9) 0.2500 0.01647(8) Uani 1 2 d S . . Cl1 Cl 0.42015(13) -0.09814(4) 0.41743(7) 0.02212(19) Uani 1 1 d . . . O1 O 0.8344(4) -0.22483(14) 0.3100(2) 0.0320(6) Uani 1 1 d . . . N1 N 0.7048(4) -0.01405(15) 0.2969(2) 0.0162(6) Uani 1 1 d . . . C1 C 0.7071(5) -0.17992(19) 0.2880(3) 0.0210(7) Uani 1 1 d . . . C10 C 0.9084(5) -0.01681(19) 0.3507(2) 0.0181(7) Uani 1 1 d . . . H10 H 0.9789 -0.0632 0.3599 0.022 Uiso 1 1 calc R . . C11 C 1.0189(5) 0.04463(19) 0.3930(3) 0.0199(7) Uani 1 1 d . . . H11 H 1.1640 0.0402 0.4286 0.024 Uiso 1 1 calc R . . C12 C 0.9193(5) 0.11303(17) 0.3838(3) 0.0196(7) Uani 1 1 d . . . C13 C 0.7100(5) 0.11588(17) 0.3248(3) 0.0196(7) Uani 1 1 d . . . H13 H 0.6366 0.1618 0.3147 0.024 Uiso 1 1 calc R . . C14 C 0.6096(5) 0.05326(17) 0.2815(2) 0.0162(7) Uani 1 1 d . . . C15 C 1.0211(6) 0.1797(2) 0.4385(3) 0.0317(9) Uani 1 1 d . . . H15A H 0.9741 0.1848 0.5034 0.048 Uiso 1 1 calc R . . H15B H 0.9779 0.2235 0.3966 0.048 Uiso 1 1 calc R . . H15C H 1.1781 0.1747 0.4515 0.048 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 Os1 0.01323(11) 0.01739(11) 0.01865(12) 0.000 0.00289(8) 0.000 Cl1 0.0194(4) 0.0274(4) 0.0203(5) 0.0027(3) 0.0058(4) 0.0042(3) O1 0.0258(14) 0.0298(14) 0.0394(17) -0.0003(13) 0.0045(12) 0.0106(12) N1 0.0112(12) 0.0207(14) 0.0170(15) 0.0004(12) 0.0035(11) 0.0016(11) C1 0.0208(17) 0.0233(17) 0.0192(18) -0.0029(15) 0.0048(14) -0.0041(15) C10 0.0147(15) 0.0249(17) 0.0150(17) 0.0020(14) 0.0039(13) 0.0020(14) C11 0.0137(16) 0.0278(18) 0.0179(19) 0.0039(15) 0.0025(14) -0.0003(14) C12 0.0169(17) 0.0256(18) 0.0161(18) 0.0010(14) 0.0031(14) -0.0053(14) C13 0.0195(17) 0.0184(16) 0.0200(19) 0.0023(14) 0.0017(15) 0.0003(13) C14 0.0137(15) 0.0212(16) 0.0137(17) -0.0010(14) 0.0031(13) 0.0001(13) C15 0.030(2) 0.0258(19) 0.034(2) 0.0012(18) -0.0060(17) -0.0096(16) _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 Os1 C1 1.873(4) . yes Os1 C1 1.873(4) 2_655 ? Os1 N1 2.131(3) 2_655 ? Os1 N1 2.131(3) . yes Os1 Cl1 2.4048(9) 2_655 ? Os1 Cl1 2.4048(9) . yes O1 C1 1.143(4) . ? N1 C10 1.345(4) . ? N1 C14 1.360(4) . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 C13 1.400(5) . ? C12 C15 1.493(5) . yes C13 C14 1.373(4) . ? C13 H13 0.9500 . ? C14 C14 1.472(6) 2_655 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Os1 C1 88.6(2) . 2_655 yes C1 Os1 N1 173.11(11) . 2_655 ? C1 Os1 N1 97.40(13) 2_655 2_655 ? C1 Os1 N1 97.39(13) . . ? C1 Os1 N1 173.11(11) 2_655 . ? N1 Os1 N1 76.78(14) 2_655 . yes C1 Os1 Cl1 91.58(10) . 2_655 ? C1 Os1 Cl1 93.33(10) 2_655 2_655 ? N1 Os1 Cl1 84.80(7) 2_655 2_655 ? N1 Os1 Cl1 89.82(7) . 2_655 ? C1 Os1 Cl1 93.33(10) . . ? C1 Os1 Cl1 91.58(10) 2_655 . ? N1 Os1 Cl1 89.82(7) 2_655 . ? N1 Os1 Cl1 84.80(7) . . ? Cl1 Os1 Cl1 173.14(4) 2_655 . yes C10 N1 C14 117.6(3) . . ? C10 N1 Os1 126.2(2) . . ? C14 N1 Os1 115.7(2) . . ? O1 C1 Os1 179.0(3) . . ? N1 C10 C11 122.9(3) . . ? N1 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 116.5(3) . . ? C11 C12 C15 122.6(3) . . ? C13 C12 C15 120.9(3) . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? N1 C14 C13 121.7(3) . . ? N1 C14 C14 115.18(18) . 2_655 ? C13 C14 C14 123.05(19) . 2_655 ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.459 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.146 #===END======================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 642576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 Br2 N2 O2 Os' _chemical_formula_sum 'C12 H8 Br2 N2 O2 Os' _chemical_formula_weight 562.22 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' O O 0.0106 0.0060 '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 'P n' _symmetry_space_group_name_Hall 'P -2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.2462(4) _cell_length_b 6.9197(2) _cell_length_c 12.6228(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.933(3) _cell_angle_gamma 90.00 _cell_volume 702.00(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2059 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 14.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1827 _exptl_absorpt_correction_T_max 0.3069 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; Hydrogens were positioned geometrically and were constrained to ride on their parent atoms, with C---H =0.95 \%A, and U~iso~ = 1.2 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5810 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2972 _reflns_number_gt 2798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(12) _chemical_absolute_configuration unk _refine_ls_number_reflns 2972 _refine_ls_number_parameters 172 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _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 Os1 Os 0.20091(4) 0.21953(3) 0.87606(3) 0.01025(6) Uani 1 1 d . . . Br1 Br 0.02972(8) 0.41349(10) 0.72127(6) 0.01903(15) Uani 1 1 d . . . Br2 Br 0.34515(7) 0.03540(9) 1.04295(5) 0.01845(16) Uani 1 1 d . . . O1 O 0.5013(6) 0.4667(7) 0.8854(4) 0.0241(12) Uani 1 1 d . . . O2 O 0.3248(6) -0.0546(7) 0.7273(4) 0.0248(12) Uani 1 1 d . . . N1 N -0.0183(6) 0.0617(7) 0.8811(4) 0.0106(11) Uani 1 1 d . . . N2 N 0.0884(7) 0.3891(7) 0.9812(4) 0.0124(12) Uani 1 1 d . . . C1 C 0.3904(9) 0.3777(10) 0.8816(5) 0.0158(15) Uani 1 1 d . . . C2 C 0.2791(8) 0.0486(10) 0.7822(6) 0.0157(15) Uani 1 1 d . . . C10 C -0.0642(8) -0.1044(9) 0.8282(5) 0.0152(14) Uani 1 1 d . . . H10 H 0.0051 -0.1575 0.7848 0.018 Uiso 1 1 calc R . . C11 C -0.2086(8) -0.2016(10) 0.8342(6) 0.0195(15) Uani 1 1 d . . . H11 H -0.2392 -0.3175 0.7944 0.023 Uiso 1 1 calc R . . C12 C -0.3077(9) -0.1262(9) 0.8996(5) 0.0164(16) Uani 1 1 d . . . H12 H -0.4070 -0.1901 0.9060 0.020 Uiso 1 1 calc R . . C13 C -0.2590(8) 0.0439(9) 0.9554(6) 0.0168(14) Uani 1 1 d . . . H13 H -0.3243 0.0968 1.0015 0.020 Uiso 1 1 calc R . . C14 C -0.1150(8) 0.1369(9) 0.9441(5) 0.0125(13) Uani 1 1 d . . . C15 C -0.0564(8) 0.3199(9) 0.9986(5) 0.0124(13) Uani 1 1 d . . . C16 C -0.1443(9) 0.4191(9) 1.0639(5) 0.0160(14) Uani 1 1 d . . . H16 H -0.2463 0.3700 1.0758 0.019 Uiso 1 1 calc R . . C17 C -0.0799(8) 0.5889(9) 1.1102(5) 0.0163(14) Uani 1 1 d . . . H17 H -0.1381 0.6596 1.1545 0.020 Uiso 1 1 calc R . . C18 C 0.0701(8) 0.6590(10) 1.0931(6) 0.0198(15) Uani 1 1 d . . . H18 H 0.1159 0.7764 1.1257 0.024 Uiso 1 1 calc R . . C19 C 0.1496(8) 0.5550(9) 1.0284(5) 0.0147(14) Uani 1 1 d . . . H19 H 0.2522 0.6019 1.0163 0.018 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 Os1 0.01010(10) 0.01105(10) 0.01011(11) -0.00071(16) 0.00338(7) -0.00168(16) Br1 0.0191(4) 0.0204(4) 0.0169(4) 0.0018(3) 0.0027(3) 0.0026(3) Br2 0.0158(4) 0.0225(4) 0.0170(4) 0.0043(3) 0.0036(3) -0.0016(3) O1 0.018(3) 0.021(3) 0.032(3) -0.001(2) 0.004(2) -0.007(2) O2 0.026(3) 0.020(3) 0.030(3) -0.001(2) 0.009(2) 0.004(2) N1 0.009(3) 0.015(3) 0.008(3) 0.001(2) 0.003(2) 0.003(2) N2 0.014(3) 0.011(3) 0.011(3) 0.003(2) 0.001(2) 0.001(2) C1 0.016(4) 0.019(4) 0.012(4) 0.001(3) 0.003(3) 0.012(3) C2 0.007(3) 0.020(4) 0.019(4) 0.005(3) 0.001(3) -0.004(3) C10 0.013(3) 0.016(4) 0.018(4) 0.002(3) 0.007(3) 0.006(3) C11 0.015(4) 0.016(4) 0.026(4) -0.002(3) 0.001(3) -0.005(3) C12 0.017(4) 0.013(3) 0.018(5) 0.002(3) 0.000(3) -0.001(3) C13 0.010(3) 0.021(4) 0.020(4) -0.003(3) 0.004(3) 0.000(3) C14 0.016(3) 0.010(3) 0.011(3) -0.002(3) 0.002(3) -0.001(2) C15 0.012(3) 0.015(4) 0.011(3) 0.006(3) 0.005(3) 0.005(2) C16 0.024(4) 0.014(3) 0.014(4) 0.003(3) 0.011(3) 0.001(3) C17 0.022(4) 0.015(3) 0.014(3) -0.003(3) 0.007(3) 0.005(3) C18 0.022(4) 0.012(3) 0.026(4) -0.008(3) 0.006(3) -0.006(3) C19 0.012(4) 0.019(4) 0.012(4) 0.000(3) 0.002(3) -0.005(3) _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 Os1 C2 1.887(7) . yes Os1 C1 1.897(7) . yes Os1 N1 2.125(5) . yes Os1 N2 2.133(5) . yes Os1 Br2 2.5208(8) . yes Os1 Br1 2.5254(8) . yes O1 C1 1.094(8) . ? O2 C2 1.118(8) . ? N1 C10 1.341(8) . ? N1 C14 1.350(7) . ? N2 C19 1.339(8) . ? N2 C15 1.350(8) . ? C10 C11 1.384(9) . ? C10 H10 0.9500 . ? C11 C12 1.387(8) . ? C11 H11 0.9500 . ? C12 C13 1.385(9) . ? C12 H12 0.9500 . ? C13 C14 1.386(9) . ? C13 H13 0.9500 . ? C14 C15 1.470(9) . ? C15 C16 1.393(8) . ? C16 C17 1.366(9) . ? C16 H16 0.9500 . ? C17 C18 1.390(9) . ? C17 H17 0.9500 . ? C18 C19 1.361(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Os1 C1 89.5(3) . . yes C2 Os1 N1 96.3(2) . . ? C1 Os1 N1 174.3(2) . . ? C2 Os1 N2 173.1(2) . . ? C1 Os1 N2 97.4(2) . . ? N1 Os1 N2 76.85(19) . . yes C2 Os1 Br2 92.5(2) . . ? C1 Os1 Br2 91.7(2) . . ? N1 Os1 Br2 87.73(14) . . ? N2 Os1 Br2 86.99(14) . . ? C2 Os1 Br1 93.3(2) . . ? C1 Os1 Br1 92.0(2) . . ? N1 Os1 Br1 87.97(14) . . ? N2 Os1 Br1 86.77(14) . . ? Br2 Os1 Br1 173.09(2) . . yes C10 N1 C14 119.1(5) . . ? C10 N1 Os1 124.9(4) . . ? C14 N1 Os1 116.0(4) . . ? C19 N2 C15 119.4(5) . . ? C19 N2 Os1 125.1(4) . . ? C15 N2 Os1 115.5(4) . . ? O1 C1 Os1 178.9(6) . . ? O2 C2 Os1 179.1(6) . . ? N1 C10 C11 122.7(6) . . ? N1 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 118.6(6) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 118.7(6) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 120.0(6) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? N1 C14 C13 120.9(6) . . ? N1 C14 C15 115.6(5) . . ? C13 C14 C15 123.4(5) . . ? N2 C15 C16 121.2(6) . . ? N2 C15 C14 116.1(5) . . ? C16 C15 C14 122.8(6) . . ? C17 C16 C15 118.2(6) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 120.5(6) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 118.3(6) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? N2 C19 C18 122.4(6) . . ? N2 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.801 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.184 #===END======================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 642577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H8 I2 N2 O2 Os' _chemical_formula_sum 'C12 H8 I2 N2 O2 Os' _chemical_formula_weight 656.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 'P n' _symmetry_space_group_name_Hall 'P -2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.4170(4) _cell_length_b 7.0934(4) _cell_length_c 13.1254(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.737(4) _cell_angle_gamma 90.00 _cell_volume 767.27(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2570 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 12.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2632 _exptl_absorpt_correction_T_max 0.5382 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _publ_section_exptl_refinement ; Hydrogens were positioned geometrically and constrained to ride on their parent atoms, with C---H =0.95 \%A, and U~iso~ = 1.2(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7768 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3208 _reflns_number_gt 2839 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1d (Brandenburg, 2006)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(6) _chemical_absolute_configuration unk _refine_ls_number_reflns 3208 _refine_ls_number_parameters 172 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_gt 0.0386 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.835 _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 Os1 Os 0.24500(4) 0.23169(4) 0.82913(3) 0.01173(7) Uani 1 1 d . . . I1 I 0.42082(6) 0.42712(8) 0.98996(4) 0.01797(11) Uani 1 1 d . . . I2 I 0.09319(5) 0.04447(6) 0.65813(3) 0.01811(13) Uani 1 1 d . . . O1 O -0.0436(7) 0.4790(7) 0.8213(4) 0.0248(12) Uani 1 1 d . . . O2 O 0.1148(6) -0.0326(7) 0.9691(4) 0.0236(12) Uani 1 1 d . . . N1 N 0.4547(7) 0.0721(8) 0.8221(4) 0.0119(13) Uani 1 1 d . . . N2 N 0.3600(7) 0.3946(8) 0.7285(4) 0.0134(13) Uani 1 1 d . . . C1 C 0.0633(10) 0.3870(11) 0.8245(5) 0.0174(17) Uani 1 1 d . . . C2 C 0.1617(10) 0.0663(11) 0.9186(6) 0.0205(18) Uani 1 1 d . . . C10 C 0.4985(8) -0.0881(10) 0.8704(5) 0.0160(16) Uani 1 1 d . . . H10 H 0.4298 -0.1393 0.9125 0.019 Uiso 1 1 calc R . . C11 C 0.6382(8) -0.1872(10) 0.8639(5) 0.0212(16) Uani 1 1 d . . . H11 H 0.6655 -0.3016 0.9010 0.025 Uiso 1 1 calc R . . C12 C 0.7364(9) -0.1119(10) 0.8010(5) 0.0225(17) Uani 1 1 d . . . H12 H 0.8343 -0.1735 0.7949 0.027 Uiso 1 1 calc R . . C13 C 0.6907(9) 0.0530(11) 0.7477(6) 0.0231(17) Uani 1 1 d . . . H13 H 0.7548 0.1029 0.7023 0.028 Uiso 1 1 calc R . . C14 C 0.5529(8) 0.1450(10) 0.7601(5) 0.0166(15) Uani 1 1 d . . . C15 C 0.5001(8) 0.3224(9) 0.7084(5) 0.0134(15) Uani 1 1 d . . . C16 C 0.5837(10) 0.4164(9) 0.6449(6) 0.0179(15) Uani 1 1 d . . . H16 H 0.6825 0.3658 0.6325 0.021 Uiso 1 1 calc R . . C17 C 0.5256(9) 0.5826(11) 0.5991(5) 0.0233(17) Uani 1 1 d . . . H17 H 0.5828 0.6466 0.5541 0.028 Uiso 1 1 calc R . . C18 C 0.3834(8) 0.6566(10) 0.6189(5) 0.0180(16) Uani 1 1 d . . . H18 H 0.3403 0.7713 0.5875 0.022 Uiso 1 1 calc R . . C19 C 0.3054(9) 0.5590(10) 0.6856(5) 0.0154(16) Uani 1 1 d . . . H19 H 0.2093 0.6109 0.7016 0.019 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 Os1 0.01080(11) 0.01325(17) 0.01176(10) 0.00029(13) 0.00375(7) 0.00113(14) I1 0.0187(3) 0.0197(3) 0.0151(2) -0.00126(17) 0.00241(18) -0.00257(19) I2 0.0137(3) 0.0235(3) 0.0165(2) -0.0046(2) 0.00188(19) 0.0017(2) O1 0.023(3) 0.027(3) 0.027(3) 0.002(2) 0.012(2) 0.007(3) O2 0.020(3) 0.018(3) 0.035(3) 0.002(2) 0.011(2) -0.007(2) N1 0.013(3) 0.015(3) 0.007(3) -0.005(2) 0.001(2) -0.001(3) N2 0.008(3) 0.018(3) 0.013(3) 0.001(2) -0.001(2) -0.002(3) C1 0.026(5) 0.017(4) 0.010(4) 0.000(3) 0.007(3) -0.008(4) C2 0.018(4) 0.021(5) 0.019(4) -0.010(3) -0.003(3) 0.004(3) C10 0.012(4) 0.017(4) 0.020(4) 0.003(3) 0.005(3) 0.003(3) C11 0.019(4) 0.012(4) 0.031(4) 0.003(3) 0.004(3) 0.002(3) C12 0.024(4) 0.015(4) 0.030(4) 0.005(3) 0.009(4) 0.008(3) C13 0.010(4) 0.035(5) 0.027(4) 0.006(3) 0.009(3) -0.001(3) C14 0.019(4) 0.021(4) 0.013(3) 0.002(3) 0.009(3) 0.001(3) C15 0.011(4) 0.020(4) 0.010(3) -0.002(3) 0.001(3) 0.007(3) C16 0.018(4) 0.017(4) 0.022(4) 0.003(3) 0.012(3) 0.004(3) C17 0.024(4) 0.031(5) 0.018(4) 0.007(3) 0.011(3) -0.001(3) C18 0.021(4) 0.016(4) 0.018(4) 0.008(3) 0.005(3) 0.002(3) C19 0.015(4) 0.013(4) 0.017(4) -0.004(3) 0.002(3) 0.006(3) _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 Os1 C1 1.876(9) . yes Os1 C2 1.893(9) . yes Os1 N1 2.114(6) . yes Os1 N2 2.130(5) . yes Os1 I2 2.6958(6) . yes Os1 I1 2.7012(7) . yes O1 C1 1.105(9) . ? O2 C2 1.092(9) . ? N1 C10 1.317(9) . ? N1 C14 1.373(8) . ? N2 C19 1.335(9) . ? N2 C15 1.360(8) . ? C10 C11 1.387(9) . ? C10 H10 0.9500 . ? C11 C12 1.389(9) . ? C11 H11 0.9500 . ? C12 C13 1.377(10) . ? C12 H12 0.9500 . ? C13 C14 1.369(10) . ? C13 H13 0.9500 . ? C14 C15 1.456(10) . ? C15 C16 1.368(9) . ? C16 C17 1.368(10) . ? C16 H16 0.9500 . ? C17 C18 1.379(9) . ? C17 H17 0.9500 . ? C18 C19 1.383(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Os1 C2 89.0(3) . . yes C1 Os1 N1 174.4(3) . . ? C2 Os1 N1 96.5(3) . . ? C1 Os1 N2 97.6(3) . . ? C2 Os1 N2 173.5(3) . . ? N1 Os1 N2 77.0(2) . . yes C1 Os1 I2 91.0(2) . . ? C2 Os1 I2 92.2(2) . . ? N1 Os1 I2 87.60(15) . . ? N2 Os1 I2 87.09(15) . . ? C1 Os1 I1 92.1(2) . . ? C2 Os1 I1 92.7(2) . . ? N1 Os1 I1 88.83(15) . . ? N2 Os1 I1 87.72(15) . . ? I2 Os1 I1 174.26(2) . . yes C10 N1 C14 117.8(6) . . ? C10 N1 Os1 126.5(5) . . ? C14 N1 Os1 115.6(4) . . ? C19 N2 C15 119.0(6) . . ? C19 N2 Os1 125.1(5) . . ? C15 N2 Os1 115.9(5) . . ? O1 C1 Os1 179.6(7) . . ? O2 C2 Os1 178.4(7) . . ? N1 C10 C11 124.4(6) . . ? N1 C10 H10 117.8 . . ? C11 C10 H10 117.8 . . ? C10 C11 C12 117.1(7) . . ? C10 C11 H11 121.4 . . ? C12 C11 H11 121.4 . . ? C13 C12 C11 119.4(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 120.0(6) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 N1 121.2(6) . . ? C13 C14 C15 122.8(6) . . ? N1 C14 C15 116.0(6) . . ? N2 C15 C16 120.5(6) . . ? N2 C15 C14 115.4(6) . . ? C16 C15 C14 124.0(6) . . ? C17 C16 C15 120.4(7) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.4(6) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C17 C18 C19 118.1(7) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? N2 C19 C18 122.5(6) . . ? N2 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.946 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.183