Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal ociety of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _audit_creation_date 2007-04-20 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? _publ_contact_author_name 'Wing-Tak Wong' _publ_contact_author_email wtwong@hkucc.hku.hk _publ_contact_author_fax '(852) 2547 2933' _publ_contact_author_phone '(852) 2859 2157' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_section_title ; An Open-Channel Architecture Assembly from the [Os3(CO)8{?-?3-ON=CPh(NC5H4)}2] Cluster ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Shuk-Yee Janet Wong' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; 'Yan-Juan Gu' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; 'Wing-Tak Wong' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., de Gelder, R., Israel, R. and Smits, J.M.M.(1999). The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). PATTY-The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Johnson, C. K. (1976) ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Larson, A. C. (1970), Crystallographic Computing, 291-294. Crystallographic Computing eq. 22 ed F. R. Ahmed, Munksgaard, Copenhagen. Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.8 Rigaku/MSC, TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Carruthers, J.R., Rollett, J.S., Betteridge, P.W., Kinna, D., Pearce, L., Larsen, A. and Gabe, E. (1999). CRYSTALS Issue 11, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_exptl_refinement ; All non-H atoms were refined anisotropically. The C-bound H atoms were placed at their geometrically calculated positions with C-H = 0.95 \%A and in the riding model with U~iso~(H) = 1.2 U~eq~(C). There are 3 channels running parallel to the c-axis, each with volume about 2668 \%A^3^, totalling to void volume of about 8000\%A^3^ per unit cell. >From the difference Fourier map, there are peaks with residual electron densities of range 0.81-3.62 e^-^/\%A^3^ inside the channel. Unfortunately, attempts to better model these peaks have failed, suggesting that the solvates in the channels are quite disordered. ; #============================================================================== data__JW005-CCDC645290 _database_code_depnum_ccdc_archive 'CCDC 645290' # JW005-R-3c_167-low_temp-Apex #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C32 H18 N4 O10 Os3 ' _chemical_formula_moiety 'C32 H18 N4 O10 Os3 ' _chemical_formula_weight 1189.11 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X+Y,+Y,1/2+Z 5 +X,+X-Y,1/2+Z 6 -Y,-X,1/2+Z 7 -X,-Y,-Z 8 +Y,-X+Y,-Z 9 +X-Y,+X,-Z 10 +X-Y,-Y,1/2-Z 11 -X,-X+Y,1/2-Z 12 +Y,+X,1/2-Z 13 2/3+X,1/3+Y,1/3+Z 14 2/3-Y,1/3+X-Y,1/3+Z 15 2/3-X+Y,1/3-X,1/3+Z 16 2/3-X+Y,1/3+Y,5/6+Z 17 2/3+X,1/3+X-Y,5/6+Z 18 2/3-Y,1/3-X,5/6+Z 19 2/3-X,1/3-Y,1/3-Z 20 2/3+Y,1/3-X+Y,1/3-Z 21 2/3+X-Y,1/3+X,1/3-Z 22 2/3+X-Y,1/3-Y,5/6-Z 23 2/3-X,1/3-X+Y,5/6-Z 24 2/3+Y,1/3+X,5/6-Z 25 1/3+X,2/3+Y,2/3+Z 26 1/3-Y,2/3+X-Y,2/3+Z 27 1/3-X+Y,2/3-X,2/3+Z 28 1/3-X+Y,2/3+Y,1/6+Z 29 1/3+X,2/3+X-Y,1/6+Z 30 1/3-Y,2/3-X,1/6+Z 31 1/3-X,2/3-Y,2/3-Z 32 1/3+Y,2/3-X+Y,2/3-Z 33 1/3+X-Y,2/3+X,2/3-Z 34 1/3+X-Y,2/3-Y,1/6-Z 35 1/3-X,2/3-X+Y,1/6-Z 36 1/3+Y,2/3+X,1/6-Z #------------------------------------------------------------------------------ _cell_length_a 37.703(8) _cell_length_b 37.703(8) _cell_length_c 17.320(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 21321(9) _cell_formula_units_Z 18 _cell_measurement_reflns_used 43178 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 28.0 _cell_measurement_temperature 253(1) #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour darkred _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9828.00 _exptl_absorpt_coefficient_mu 8.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.198 _exptl_absorpt_correction_T_max 0.298 _exptl_absorpt_process_details SADABS #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42081 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_max 27.99 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5653 _reflns_number_gt 3928 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.0648 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3963 _refine_ls_number_parameters 231 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + \s(Fo^2^) + 0.435]' _refine_ls_shift/su_max 0.0013 _refine_diff_density_max 3.08 _refine_diff_density_min -0.97 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Os Os -1.216 7.603 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os(1) Os 0.21215(2) 0.30615(2) 0.49338(3) 0.03020(14) Uani 1.00 1 d . . . Os(2) Os 0.28356(2) 0.3333 0.5833 0.0423(2) Uani 1.00 2 d S . . O(1) O 0.2050(3) 0.2233(3) 0.4863(6) 0.059(3) Uani 1.00 1 d . . . O(2) O 0.2683(3) 0.3316(3) 0.3541(5) 0.053(3) Uani 1.00 1 d . . . O(3) O 0.3150(4) 0.2875(5) 0.4849(8) 0.110(6) Uani 1.00 1 d . . . O(4) O 0.2304(3) 0.2557(3) 0.6788(6) 0.056(3) Uani 1.00 1 d . . . O(5) O 0.1863(2) 0.3022(2) 0.6647(4) 0.032(2) Uani 1.00 1 d . . . N(1) N 0.1527(3) 0.2873(3) 0.4463(5) 0.029(2) Uani 1.00 1 d . . . N(2) N 0.1733(3) 0.2926(3) 0.5912(5) 0.033(3) Uani 1.00 1 d . . . C(1) C 0.2066(4) 0.2557(5) 0.4879(7) 0.043(4) Uani 1.00 1 d . . . C(2) C 0.2460(4) 0.3221(4) 0.4068(7) 0.039(4) Uani 1.00 1 d . . . C(3) C 0.3030(5) 0.3052(6) 0.5205(9) 0.066(6) Uani 1.00 1 d . . . C(4) C 0.2517(4) 0.2856(5) 0.6452(8) 0.046(4) Uani 1.00 1 d . . . C(5) C 0.1428(4) 0.2855(3) 0.3717(7) 0.034(3) Uani 1.00 1 d . . . C(6) C 0.1035(3) 0.2711(4) 0.3455(7) 0.039(3) Uani 1.00 1 d . . . C(7) C 0.0723(4) 0.2548(4) 0.3987(8) 0.042(4) Uani 1.00 1 d . . . C(8) C 0.0809(3) 0.2550(4) 0.4754(8) 0.041(3) Uani 1.00 1 d . . . C(9) C 0.1216(3) 0.2714(3) 0.4975(7) 0.033(3) Uani 1.00 1 d . . . C(10) C 0.1340(3) 0.2751(3) 0.5788(6) 0.031(3) Uani 1.00 1 d . . . C(11) C 0.1040(3) 0.2622(4) 0.6435(7) 0.033(3) Uani 1.00 1 d . . . C(12) C 0.0980(4) 0.2290(4) 0.6888(8) 0.046(4) Uani 1.00 1 d . . . C(13) C 0.0708(4) 0.2177(5) 0.7510(8) 0.058(4) Uani 1.00 1 d . . . C(14) C 0.0503(4) 0.2376(5) 0.7665(8) 0.058(4) Uani 1.00 1 d . . . C(15) C 0.0558(4) 0.2693(5) 0.7225(8) 0.053(5) Uani 1.00 1 d . . . C(16) C 0.0828(4) 0.2821(4) 0.6601(8) 0.043(3) Uani 1.00 1 d . . . H(1) H 0.1641 0.2948 0.3346 0.041 Uiso 1.00 1 c R . . H(2) H 0.0981 0.2723 0.2923 0.047 Uiso 1.00 1 c R . . H(3) H 0.0447 0.2434 0.3822 0.050 Uiso 1.00 1 c R . . H(4) H 0.0596 0.2442 0.5127 0.049 Uiso 1.00 1 c R . . H(5) H 0.1121 0.2145 0.6777 0.056 Uiso 1.00 1 c R . . H(6) H 0.0666 0.1955 0.7830 0.070 Uiso 1.00 1 c R . . H(7) H 0.0319 0.2293 0.8089 0.069 Uiso 1.00 1 c R . . H(8) H 0.0411 0.2831 0.7338 0.063 Uiso 1.00 1 c R . . H(9) H 0.0866 0.3046 0.6293 0.051 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0278(2) 0.0485(3) 0.0247(2) 0.0268(2) 0.0044(2) 0.0076(2) Os(2) 0.0327(2) 0.0820(6) 0.0288(4) 0.0410(3) 0.0032(2) 0.0064(3) O(1) 0.080(8) 0.066(7) 0.062(7) 0.059(7) 0.002(6) -0.002(5) O(2) 0.040(5) 0.086(8) 0.039(5) 0.035(5) 0.012(4) 0.012(5) O(3) 0.115(12) 0.200(18) 0.081(10) 0.128(13) 0.038(9) 0.025(10) O(4) 0.072(7) 0.077(8) 0.045(6) 0.057(7) 0.002(5) 0.010(5) O(5) 0.039(5) 0.041(5) 0.024(4) 0.025(4) -0.004(3) 0.007(3) N(1) 0.029(5) 0.042(6) 0.025(5) 0.024(5) 0.004(4) 0.007(4) N(2) 0.044(6) 0.042(6) 0.026(5) 0.032(5) 0.002(4) 0.005(4) C(1) 0.034(7) 0.074(11) 0.024(6) 0.028(7) 0.007(5) -0.001(6) C(2) 0.037(7) 0.067(9) 0.029(6) 0.038(7) 0.000(5) 0.004(6) C(3) 0.066(11) 0.122(16) 0.049(9) 0.077(12) 0.014(8) 0.014(10) C(4) 0.047(8) 0.079(11) 0.034(7) 0.047(9) 0.002(6) 0.007(7) C(5) 0.034(7) 0.038(7) 0.041(7) 0.026(6) 0.002(5) 0.009(6) C(6) 0.029(6) 0.058(9) 0.028(6) 0.019(6) -0.005(5) 0.006(6) C(7) 0.027(7) 0.057(9) 0.044(8) 0.024(6) -0.003(6) -0.005(6) C(8) 0.021(6) 0.058(9) 0.037(7) 0.014(6) 0.006(5) 0.010(6) C(9) 0.033(7) 0.035(7) 0.035(6) 0.020(6) 0.005(5) 0.004(5) C(10) 0.030(6) 0.041(7) 0.029(6) 0.023(6) 0.000(5) 0.005(5) C(11) 0.024(6) 0.040(7) 0.031(6) 0.011(5) 0.005(5) 0.002(5) C(12) 0.040(8) 0.051(9) 0.047(8) 0.023(7) 0.014(6) 0.015(7) C(13) 0.045(9) 0.068(11) 0.036(8) 0.009(8) 0.001(7) 0.021(7) C(14) 0.033(8) 0.084(12) 0.035(8) 0.013(8) 0.001(6) -0.006(8) C(15) 0.053(9) 0.083(12) 0.039(8) 0.046(9) 0.006(7) 0.006(8) C(16) 0.031(7) 0.047(8) 0.038(7) 0.010(6) 0.011(5) 0.006(6) #============================================================================== _computing_data_collection 'Apex (Bruker, 2002)' _computing_cell_refinement 'Saint (Bruker, 2002)' _computing_data_reduction 'CrystalStructure (Rigaku, 2007)' _computing_structure_solution 'DIRDIF99-PATTY (Beurskens et al., 1999)' _computing_structure_refinement 'CRYSTALS (Carruthers et al., 1999)' _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Os(1) Os(2) 2.8226(8) yes . . Os(1) O(5) 2.111(10) yes . 34_556 Os(1) N(1) 2.145(10) yes . . Os(1) N(2) 2.128(10) yes . . Os(1) C(1) 1.81(2) yes . . Os(1) C(2) 1.862(13) yes . . Os(2) C(3) 1.90(2) yes . . Os(2) C(3) 1.904(16) yes . 34_556 Os(2) C(4) 1.916(15) yes . . Os(2) C(4) 1.916(18) yes . 34_556 O(1) C(1) 1.19(2) yes . . O(2) C(2) 1.171(16) yes . . O(3) C(3) 1.15(3) yes . . O(4) C(4) 1.161(18) yes . . O(5) N(2) 1.347(12) yes . . N(1) C(5) 1.337(16) yes . . N(1) C(9) 1.349(15) yes . . N(2) C(10) 1.303(17) yes . . C(5) C(6) 1.374(19) yes . . C(5) H(1) 0.950 yes . . C(6) C(7) 1.374(18) yes . . C(6) H(2) 0.950 yes . . C(7) C(8) 1.366(19) yes . . C(7) H(3) 0.950 yes . . C(8) C(9) 1.391(19) yes . . C(8) H(4) 0.950 yes . . C(9) C(10) 1.470(17) yes . . C(10) C(11) 1.492(17) yes . . C(11) C(12) 1.40(2) yes . . C(11) C(16) 1.37(2) yes . . C(12) C(13) 1.40(2) yes . . C(12) H(5) 0.950 yes . . C(13) C(14) 1.35(3) yes . . C(13) H(6) 0.950 yes . . C(14) C(15) 1.34(2) yes . . C(14) H(7) 0.950 yes . . C(15) C(16) 1.40(2) yes . . C(15) H(8) 0.950 yes . . C(16) H(9) 0.950 yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Os(2) Os(1) O(5) 90.4(2) yes . . 34_556 Os(2) Os(1) N(1) 168.3(2) yes . . . Os(2) Os(1) N(2) 93.7(3) yes . . . Os(2) Os(1) C(1) 89.9(4) yes . . . Os(2) Os(1) C(2) 87.3(4) yes . . . O(5) Os(1) N(1) 84.9(4) yes 34_556 . . O(5) Os(1) N(2) 83.6(4) yes 34_556 . . O(5) Os(1) C(1) 178.5(4) yes 34_556 . . O(5) Os(1) C(2) 91.5(6) yes 34_556 . . N(1) Os(1) N(2) 75.2(4) yes . . . N(1) Os(1) C(1) 94.5(5) yes . . . N(1) Os(1) C(2) 103.5(5) yes . . . N(2) Os(1) C(1) 94.9(5) yes . . . N(2) Os(1) C(2) 175.1(7) yes . . . C(1) Os(1) C(2) 89.9(7) yes . . . Os(1) Os(2) Os(1) 78.88(2) yes . . 34_556 Os(1) Os(2) C(3) 92.7(5) yes . . . Os(1) Os(2) C(3) 168.5(8) yes . . 34_556 Os(1) Os(2) C(4) 86.1(4) yes . . . Os(1) Os(2) C(4) 80.0(4) yes . . 34_556 Os(1) Os(2) C(3) 168.5(4) yes 34_556 . . Os(1) Os(2) C(3) 92.6(7) yes 34_556 . 34_556 Os(1) Os(2) C(4) 80.0(6) yes 34_556 . . Os(1) Os(2) C(4) 86.1(6) yes 34_556 . 34_556 C(3) Os(2) C(3) 96.7(9) yes . . 34_556 C(3) Os(2) C(4) 91.8(8) yes . . . C(3) Os(2) C(4) 100.2(8) yes . . 34_556 C(3) Os(2) C(4) 100.2(7) yes 34_556 . . C(3) Os(2) C(4) 91.8(7) yes 34_556 . 34_556 C(4) Os(2) C(4) 162.0(8) yes . . 34_556 Os(1) O(5) N(2) 112.0(5) yes 34_556 . . Os(1) N(1) C(5) 127.2(8) yes . . . Os(1) N(1) C(9) 115.5(8) yes . . . C(5) N(1) C(9) 116.9(10) yes . . . Os(1) N(2) O(5) 125.0(7) yes . . . Os(1) N(2) C(10) 117.5(8) yes . . . O(5) N(2) C(10) 117.4(10) yes . . . Os(1) C(1) O(1) 176.4(11) yes . . . Os(1) C(2) O(2) 176.9(16) yes . . . Os(2) C(3) O(3) 177.6(18) yes . . . Os(2) C(4) O(4) 175.3(13) yes . . . N(1) C(5) C(6) 124.0(12) yes . . . N(1) C(5) H(1) 118.0 yes . . . C(6) C(5) H(1) 118.0 yes . . . C(5) C(6) C(7) 117.9(12) yes . . . C(5) C(6) H(2) 121.1 yes . . . C(7) C(6) H(2) 121.1 yes . . . C(6) C(7) C(8) 120.2(12) yes . . . C(6) C(7) H(3) 119.9 yes . . . C(8) C(7) H(3) 119.9 yes . . . C(7) C(8) C(9) 118.4(12) yes . . . C(7) C(8) H(4) 120.8 yes . . . C(9) C(8) H(4) 120.8 yes . . . N(1) C(9) C(8) 122.5(11) yes . . . N(1) C(9) C(10) 115.0(11) yes . . . C(8) C(9) C(10) 122.4(11) yes . . . N(2) C(10) C(9) 115.7(10) yes . . . N(2) C(10) C(11) 121.9(10) yes . . . C(9) C(10) C(11) 122.3(11) yes . . . C(10) C(11) C(12) 117.9(15) yes . . . C(10) C(11) C(16) 122.3(13) yes . . . C(12) C(11) C(16) 119.8(12) yes . . . C(11) C(12) C(13) 117.9(18) yes . . . C(11) C(12) H(5) 121.1 yes . . . C(13) C(12) H(5) 121.1 yes . . . C(12) C(13) C(14) 121.5(17) yes . . . C(12) C(13) H(6) 119.2 yes . . . C(14) C(13) H(6) 119.2 yes . . . C(13) C(14) C(15) 120.4(15) yes . . . C(13) C(14) H(7) 119.8 yes . . . C(15) C(14) H(7) 119.8 yes . . . C(14) C(15) C(16) 121(2) yes . . . C(14) C(15) H(8) 119.7 yes . . . C(16) C(15) H(8) 119.7 yes . . . C(11) C(16) C(15) 119.7(16) yes . . . C(11) C(16) H(9) 120.1 yes . . . C(15) C(16) H(9) 120.1 yes . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Os(1) Os(1) 3.5861(7) . . 34_556 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C(6) H(2) O(5) 4_554 0.95 2.42 3.294(14) 153 . C(8) H(4) O(1) 9_556 0.95 2.54 3.306(15) 138 . #============================================================================== # start Validation Reply Form _vrf_PLAT602__JW005-CCDC645290 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: There are 3 channels running parallel to the c-axis, each with volume about 2668 \%A^3^, totalling to void volume of about 8000\%A^3^ per unit cell. >From the difference Fourier map, there are peaks with residual electron densities of range 0.81-3.62 e^-^/\%A^3^ inside the channel. Unfortunately, attempts to better model these peaks have failed, suggesting that the solvates in the channels are quite disordered. ; # end Validation Reply Form # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC645291 JW007-Apex.cif' #CCDC645291 #============================================================================== data__JW007-Apex-CCDC645291 _database_code_depnum_ccdc_archive 'CCDC 645291' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C32 H18 N4 O10 Os3 ' _chemical_formula_moiety 'C32 H18 N4 O10 Os3 ' _chemical_formula_weight 1189.11 _chemical_melting_point ? _chemical_absolute_configuration ad #'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' _symmetry_space_group_name_Hall 'P 4nw 2abw' _symmetry_Int_Tables_number 96 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-Y,1/2+X,3/4+Z 3 -X,-Y,1/2+Z 4 1/2+Y,1/2-X,1/4+Z 5 1/2-X,1/2+Y,3/4-Z 6 +Y,+X,-Z 7 1/2+X,1/2-Y,1/4-Z 8 -Y,-X,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 12.955(5) _cell_length_b 12.955(5) _cell_length_c 19.352(6) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3248.0(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20155 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 28.0 _cell_measurement_temperature 253(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 2.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184.00 _exptl_absorpt_coefficient_mu 11.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_T_max 0.152 _exptl_absorpt_process_details SADABS #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker Apex CCD' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20116 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_max 28.00 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.960 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3658 _reflns_number_gt 3205 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0267 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3219 _refine_ls_number_parameters 232 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 0.2\s(Fo^2^) + 0.005]' _refine_ls_shift/su_max 0.0031 _refine_diff_density_max 2.47 _refine_diff_density_min -0.85 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983). 1453 Friedel Pairs' _refine_ls_abs_structure_Flack -0.005(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Os Os -1.216 7.603 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os(1) Os 0.46423(2) 0.48651(2) 0.159820(10) 0.01250(5) Uani 1.00 1 d . . . Os(2) Os 0.36880(2) 0.63119(2) 0.2500 0.01262(6) Uani 1.00 2 d S . . O(1) O 0.5001(4) 0.6515(4) 0.0524(2) 0.0292(14) Uani 1.00 1 d . . . O(2) O 0.2585(4) 0.4315(4) 0.0967(2) 0.0321(15) Uani 1.00 1 d . . . O(3) O 0.2240(4) 0.7061(5) 0.1354(2) 0.0403(18) Uani 1.00 1 d . . . O(4) O 0.5547(4) 0.7664(4) 0.2094(2) 0.0264(14) Uani 1.00 1 d . . . O(5) O 0.6294(3) 0.5607(3) 0.2657(2) 0.0167(11) Uani 1.00 1 d . . . N(1) N 0.5663(4) 0.3802(4) 0.1081(2) 0.0172(14) Uani 1.00 1 d . . . N(2) N 0.6113(4) 0.5077(4) 0.2071(2) 0.0159(13) Uani 1.00 1 d . . . C(1) C 0.4857(5) 0.5890(4) 0.0938(3) 0.0173(15) Uani 1.00 1 d . . . C(2) C 0.3370(5) 0.4538(5) 0.1204(3) 0.0201(17) Uani 1.00 1 d . . . C(3) C 0.2789(5) 0.6777(5) 0.1780(3) 0.0187(17) Uani 1.00 1 d . . . C(4) C 0.4844(5) 0.7161(5) 0.2245(3) 0.0152(15) Uani 1.00 1 d . . . C(5) C 0.5405(5) 0.3066(5) 0.0617(3) 0.0189(17) Uani 1.00 1 d . . . C(6) C 0.6121(5) 0.2505(5) 0.0262(3) 0.0217(18) Uani 1.00 1 d . . . C(7) C 0.7164(6) 0.2691(5) 0.0369(3) 0.0237(18) Uani 1.00 1 d . . . C(8) C 0.7464(5) 0.3445(5) 0.0845(3) 0.0218(17) Uani 1.00 1 d . . . C(9) C 0.6695(5) 0.3970(5) 0.1200(3) 0.0152(16) Uani 1.00 1 d . . . C(10) C 0.6916(5) 0.4692(5) 0.1759(3) 0.0153(15) Uani 1.00 1 d . . . C(11) C 0.7992(5) 0.4922(5) 0.1995(3) 0.0174(16) Uani 1.00 1 d . . . C(12) C 0.8566(5) 0.5634(5) 0.1625(3) 0.0201(16) Uani 1.00 1 d . . . C(13) C 0.9557(6) 0.5903(6) 0.1848(3) 0.029(2) Uani 1.00 1 d . . . C(14) C 0.9968(5) 0.5444(5) 0.2437(3) 0.0263(19) Uani 1.00 1 d . . . C(15) C 0.9401(5) 0.4717(6) 0.2798(4) 0.029(2) Uani 1.00 1 d . . . C(16) C 0.8409(5) 0.4457(5) 0.2585(3) 0.0241(19) Uani 1.00 1 d . . . H(1) H 0.4694 0.2933 0.0535 0.023 Uiso 1.00 1 c R . . H(2) H 0.5907 0.1990 -0.0057 0.026 Uiso 1.00 1 c R . . H(3) H 0.7669 0.2309 0.0121 0.028 Uiso 1.00 1 c R . . H(4) H 0.8173 0.3593 0.0923 0.026 Uiso 1.00 1 c R . . H(5) H 0.8287 0.5939 0.1220 0.024 Uiso 1.00 1 c R . . H(6) H 0.9948 0.6397 0.1598 0.035 Uiso 1.00 1 c R . . H(7) H 1.0639 0.5630 0.2591 0.032 Uiso 1.00 1 c R . . H(8) H 0.9690 0.4394 0.3194 0.035 Uiso 1.00 1 c R . . H(9) H 0.8018 0.3967 0.2839 0.029 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.01192(12) 0.01365(13) 0.01193(10) 0.00155(9) -0.00155(9) -0.00154(9) Os(2) 0.01202(11) 0.01202(11) 0.01382(15) 0.00166(13) -0.00057(10) -0.00057(10) O(1) 0.037(3) 0.026(2) 0.025(2) -0.003(2) 0.001(2) 0.006(2) O(2) 0.025(2) 0.040(3) 0.031(2) -0.008(2) -0.011(2) 0.007(2) O(3) 0.033(3) 0.048(4) 0.040(3) 0.005(3) -0.015(2) 0.008(2) O(4) 0.023(2) 0.027(3) 0.029(2) -0.003(2) 0.000(2) 0.002(2) O(5) 0.018(2) 0.020(2) 0.013(2) 0.0001(19) 0.0015(18) -0.0054(17) N(1) 0.019(2) 0.019(3) 0.013(2) 0.001(2) -0.000(2) 0.004(2) N(2) 0.021(2) 0.015(2) 0.012(2) 0.003(2) -0.002(2) -0.001(2) C(1) 0.022(3) 0.017(3) 0.013(2) -0.000(2) -0.001(2) -0.007(2) C(2) 0.021(3) 0.021(3) 0.018(3) 0.001(2) -0.004(2) 0.005(2) C(3) 0.015(3) 0.019(3) 0.021(3) -0.000(2) 0.001(2) -0.002(2) C(4) 0.012(3) 0.018(3) 0.016(2) 0.007(2) -0.001(2) -0.001(2) C(5) 0.019(3) 0.013(3) 0.025(3) -0.002(2) -0.004(2) -0.004(2) C(6) 0.022(3) 0.024(3) 0.020(3) 0.007(3) -0.004(2) -0.009(2) C(7) 0.030(4) 0.022(3) 0.019(3) 0.008(3) 0.007(3) -0.005(2) C(8) 0.020(3) 0.022(3) 0.023(3) -0.000(2) 0.001(2) -0.005(3) C(9) 0.019(3) 0.015(3) 0.011(2) -0.003(2) -0.001(2) 0.002(2) C(10) 0.014(3) 0.019(3) 0.013(2) 0.004(2) -0.004(2) 0.002(2) C(11) 0.015(3) 0.013(3) 0.024(3) 0.002(2) -0.002(2) -0.003(2) C(12) 0.021(3) 0.019(3) 0.020(3) 0.001(2) -0.001(2) 0.003(2) C(13) 0.026(4) 0.028(4) 0.032(4) -0.006(3) 0.008(3) -0.001(3) C(14) 0.013(3) 0.027(3) 0.038(4) -0.002(3) -0.006(3) -0.004(3) C(15) 0.020(3) 0.026(4) 0.041(4) 0.007(3) -0.011(3) 0.004(3) C(16) 0.023(3) 0.025(3) 0.024(3) -0.003(3) -0.002(2) 0.002(3) #============================================================================== _computing_data_collection 'Apex (Bruker, 2002)' _computing_cell_refinement 'Saint (Bruker, 2002)' _computing_data_reduction 'CrystalStructure (Rigaku, 2007)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'CRYSTALS (Carruthers et al., 1999)' _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Os(1) Os(2) 2.8438(3) yes . . Os(1) O(5) 2.106(4) yes . 8_665 Os(1) N(1) 2.155(5) yes . . Os(1) N(2) 2.132(5) yes . . Os(1) C(1) 1.863(6) yes . . Os(1) C(2) 1.865(7) yes . . Os(2) C(3) 1.913(6) yes . . Os(2) C(3) 1.913(6) yes . 8_665 Os(2) C(4) 1.922(6) yes . . Os(2) C(4) 1.922(6) yes . 8_665 O(1) C(1) 1.154(8) yes . . O(2) C(2) 1.152(9) yes . . O(3) C(3) 1.150(8) yes . . O(4) C(4) 1.158(8) yes . . O(5) N(2) 1.346(6) yes . . N(1) C(5) 1.351(8) yes . . N(1) C(9) 1.375(8) yes . . N(2) C(10) 1.302(8) yes . . C(5) C(6) 1.365(10) yes . . C(5) H(1) 0.95 yes . . C(6) C(7) 1.388(10) yes . . C(6) H(2) 0.95 yes . . C(7) C(8) 1.398(10) yes . . C(7) H(3) 0.950 yes . . C(8) C(9) 1.388(9) yes . . C(8) H(4) 0.95 yes . . C(9) C(10) 1.459(8) yes . . C(10) C(11) 1.496(9) yes . . C(11) C(12) 1.384(9) yes . . C(11) C(16) 1.399(9) yes . . C(12) C(13) 1.398(10) yes . . C(12) H(5) 0.95 yes . . C(13) C(14) 1.391(10) yes . . C(13) H(6) 0.95 yes . . C(14) C(15) 1.384(10) yes . . C(14) H(7) 0.95 yes . . C(15) C(16) 1.390(10) yes . . C(15) H(8) 0.95 yes . . C(16) H(9) 0.95 yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Os(2) Os(1) O(5) 89.05(12) yes . . 8_665 Os(2) Os(1) N(1) 166.58(14) yes . . . Os(2) Os(1) N(2) 92.30(14) yes . . . Os(2) Os(1) C(1) 90.90(19) yes . . . Os(2) Os(1) C(2) 91.0(2) yes . . . O(5) Os(1) N(1) 87.49(19) yes 8_665 . . O(5) Os(1) N(2) 86.27(19) yes 8_665 . . O(5) Os(1) C(1) 179.8(2) yes 8_665 . . O(5) Os(1) C(2) 89.0(2) yes 8_665 . . N(1) Os(1) N(2) 74.5(2) yes . . . N(1) Os(1) C(1) 92.6(2) yes . . . N(1) Os(1) C(2) 101.9(2) yes . . . N(2) Os(1) C(1) 94.0(2) yes . . . N(2) Os(1) C(2) 174.2(2) yes . . . C(1) Os(1) C(2) 90.8(3) yes . . . Os(1) Os(2) Os(1) 78.669(9) yes . . 8_665 Os(1) Os(2) C(3) 91.5(2) yes . . . Os(1) Os(2) C(3) 170.1(2) yes . . 8_665 Os(1) Os(2) C(4) 83.18(19) yes . . . Os(1) Os(2) C(4) 83.84(19) yes . . 8_665 Os(1) Os(2) C(3) 170.1(2) yes 8_665 . . Os(1) Os(2) C(3) 91.5(2) yes 8_665 . 8_665 Os(1) Os(2) C(4) 83.84(19) yes 8_665 . . Os(1) Os(2) C(4) 83.18(19) yes 8_665 . 8_665 C(3) Os(2) C(3) 98.4(2) yes . . 8_665 C(3) Os(2) C(4) 96.2(2) yes . . . C(3) Os(2) C(4) 94.8(2) yes . . 8_665 C(3) Os(2) C(4) 94.8(2) yes 8_665 . . C(3) Os(2) C(4) 96.2(2) yes 8_665 . 8_665 C(4) Os(2) C(4) 163.2(2) yes . . 8_665 Os(1) O(5) N(2) 112.0(3) yes 8_665 . . Os(1) N(1) C(5) 127.4(4) yes . . . Os(1) N(1) C(9) 114.7(4) yes . . . C(5) N(1) C(9) 117.6(5) yes . . . Os(1) N(2) O(5) 125.6(3) yes . . . Os(1) N(2) C(10) 117.8(4) yes . . . O(5) N(2) C(10) 116.5(5) yes . . . Os(1) C(1) O(1) 178.9(5) yes . . . Os(1) C(2) O(2) 178.6(6) yes . . . Os(2) C(3) O(3) 179.2(5) yes . . . Os(2) C(4) O(4) 179.3(5) yes . . . N(1) C(5) C(6) 122.9(6) yes . . . N(1) C(5) H(1) 118.6 yes . . . C(6) C(5) H(1) 118.6 yes . . . C(5) C(6) C(7) 119.6(6) yes . . . C(5) C(6) H(2) 120.2 yes . . . C(7) C(6) H(2) 120.2 yes . . . C(6) C(7) C(8) 119.4(6) yes . . . C(6) C(7) H(3) 120.3 yes . . . C(8) C(7) H(3) 120.3 yes . . . C(7) C(8) C(9) 117.9(6) yes . . . C(7) C(8) H(4) 121.0 yes . . . C(9) C(8) H(4) 121.0 yes . . . N(1) C(9) C(8) 122.6(5) yes . . . N(1) C(9) C(10) 114.6(5) yes . . . C(8) C(9) C(10) 122.7(6) yes . . . N(2) C(10) C(9) 115.6(5) yes . . . N(2) C(10) C(11) 121.7(5) yes . . . C(9) C(10) C(11) 122.5(5) yes . . . C(10) C(11) C(12) 118.4(5) yes . . . C(10) C(11) C(16) 121.5(6) yes . . . C(12) C(11) C(16) 120.0(6) yes . . . C(11) C(12) C(13) 120.0(6) yes . . . C(11) C(12) H(5) 120.0 yes . . . C(13) C(12) H(5) 120.0 yes . . . C(12) C(13) C(14) 119.9(7) yes . . . C(12) C(13) H(6) 120.1 yes . . . C(14) C(13) H(6) 120.1 yes . . . C(13) C(14) C(15) 120.0(6) yes . . . C(13) C(14) H(7) 120.0 yes . . . C(15) C(14) H(7) 120.0 yes . . . C(14) C(15) C(16) 120.4(7) yes . . . C(14) C(15) H(8) 119.8 yes . . . C(16) C(15) H(8) 119.8 yes . . . C(11) C(16) C(15) 119.6(6) yes . . . C(11) C(16) H(9) 120.2 yes . . . C(15) C(16) H(9) 120.2 yes . . . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C7 H3 O4 2_644 0.95 2.54 3.165(8) 124 . C7 H3 O5 2_644 0.95 2.59 3.433(8) 148 . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================