Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Paul V. Bernhardt' 'Brendan P. Macpherson' 'Manuel Martinez' _publ_contact_author_name 'Dr Paul Bernhardt' _publ_contact_author_address ; Dr Paul Bernhardt Chemistry University of Queensland Department of Chemistry University of Queensland Brisbane Queensland 4072 AUSTRALIA ; _publ_contact_author_email 'BERNHARDT@CHEMISTRY.UQ.EDU.AU' _publ_section_title ; The influence of cis/trans isomerism on the physical properties of a cyano-bridged dinuclear mixed valence complex. ; data_bm36209 _database_code_CSD 174290 # cis-Na[L14CoNCFe(CN)5].9H2O _audit_creation_date 2001-11-15T11:13:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'cis-Na[L14CoNCFe(CN)5].9H2O' _chemical_formula_structural 'NA CO FE C17 H27 N11' _chemical_formula_sum 'C17 H45 Co Fe N11 Na O9' _chemical_formula_weight 685.41 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.758(3) _cell_length_b 10.4960(10) _cell_length_c 19.359(3) _cell_angle_alpha 90 _cell_angle_beta 92.00(2) _cell_angle_gamma 90 _cell_volume 2996.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_factor_muR 0.322 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 7 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.6498 _exptl_absorpt_correction_T_max 0.7234 _exptl_absorpt_correction_T_ave 0.6887 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.66008E-1 _diffrn_orient_matrix_ub_12 -0.1239E-2 _diffrn_orient_matrix_ub_13 0.00986 _diffrn_orient_matrix_ub_21 0.00818 _diffrn_orient_matrix_ub_22 0.77116E-1 _diffrn_orient_matrix_ub_23 0.29879E-1 _diffrn_orient_matrix_ub_31 -0.12802E-1 _diffrn_orient_matrix_ub_32 0.55947E-1 _diffrn_orient_matrix_ub_33 -0.04101 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4 _diffrn_standards_decay_corr_max 1.035 _diffrn_standards_decay_corr_min 0.91 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 3 6 3 5 6 -3 5 -8 _diffrn_reflns_number 5498 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_unetI/netI 0.0382 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5279 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0742P)^2^+19.7974P] 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_number_reflns 5279 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.2016 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 1.142 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.1978(5) 0.8585(7) 0.2208(4) 0.0446(18) Uani 1 1 d . . . H1A H 0.1487 0.8646 0.2526 0.054 Uiso 1 1 calc R . . H1B H 0.2237 0.7737 0.2245 0.054 Uiso 1 1 calc R . . C1C C 0.2652(5) 1.3000(7) 0.2351(4) 0.0342(15) Uani 1 1 d . . . C2 C 0.3551(5) 0.9089(8) 0.2709(4) 0.0457(19) Uani 1 1 d . . . H2A H 0.3762 0.8339 0.247 0.055 Uiso 1 1 calc R . . H2B H 0.3468 0.8873 0.319 0.055 Uiso 1 1 calc R . . C2C C 0.1444(6) 1.4913(8) 0.2470(4) 0.0459(19) Uani 1 1 d . . . C3 C 0.4213(5) 1.0159(8) 0.2651(4) 0.049(2) Uani 1 1 d . . . H3A H 0.4813 0.9886 0.2811 0.058 Uiso 1 1 calc R . . H3B H 0.4032 1.0874 0.2932 0.058 Uiso 1 1 calc R . . C3C C 0.3161(5) 1.5423(7) 0.2187(4) 0.0390(17) Uani 1 1 d . . . C4 C 0.4775(5) 1.1703(9) 0.1799(4) 0.053(2) Uani 1 1 d . . . H4A H 0.5388 1.1567 0.1981 0.063 Uiso 1 1 calc R . . H4B H 0.4517 1.2413 0.2045 0.063 Uiso 1 1 calc R . . C4C C 0.3737(5) 1.4016(7) 0.3312(4) 0.0362(16) Uani 1 1 d . . . C5 C 0.4795(6) 1.2010(10) 0.1042(5) 0.066(3) Uani 1 1 d . . . H5A H 0.4994 1.1261 0.0796 0.079 Uiso 1 1 calc R . . H5B H 0.5237 1.2678 0.0974 0.079 Uiso 1 1 calc R . . C5C C 0.1989(5) 1.3563(7) 0.3592(4) 0.0399(17) Uani 1 1 d . . . C6 C 0.3891(6) 1.2434(10) 0.0732(5) 0.068(3) Uani 1 1 d . . . H6A H 0.368 1.3153 0.0997 0.082 Uiso 1 1 calc R . . H6B H 0.3982 1.2731 0.0265 0.082 Uiso 1 1 calc R . . C6C C 0.2546(6) 1.5988(7) 0.3478(4) 0.0453(19) Uani 1 1 d . . . C7 C 0.3227(6) 1.0489(10) 0.0132(4) 0.059(2) Uani 1 1 d . . . H7A H 0.2626 1.0329 -0.0067 0.071 Uiso 1 1 calc R . . H7B H 0.3602 1.0822 -0.0228 0.071 Uiso 1 1 calc R . . C8 C 0.3624(6) 0.9279(10) 0.0408(4) 0.058(2) Uani 1 1 d . . . H8A H 0.427 0.9381 0.0501 0.07 Uiso 1 1 calc R . . H8B H 0.3534 0.86 0.0073 0.07 Uiso 1 1 calc R . . C9 C 0.2264(5) 0.8297(8) 0.0947(4) 0.0487(19) Uani 1 1 d . . . H9A H 0.2335 0.7386 0.1015 0.058 Uiso 1 1 calc R . . H9B H 0.2032 0.8444 0.0479 0.058 Uiso 1 1 calc R . . C10 C 0.1617(5) 0.8829(7) 0.1459(4) 0.0417(17) Uani 1 1 d . . . C11 C 0.0667(5) 0.8284(9) 0.1351(5) 0.059(2) Uani 1 1 d . . . H11A H 0.0275 0.8644 0.1685 0.088 Uiso 1 1 calc R . . H11B H 0.0687 0.7375 0.1406 0.088 Uiso 1 1 calc R . . H11C H 0.0439 0.8489 0.0894 0.088 Uiso 1 1 calc R . . Co1 Co 0.29584(6) 1.05352(9) 0.15675(4) 0.0323(3) Uani 1 1 d . . . Fe1 Fe 0.25864(7) 1.44923(10) 0.28938(5) 0.0360(3) Uani 1 1 d . . . N1 N 0.2687(4) 0.9565(5) 0.2381(3) 0.0350(13) Uani 1 1 d . . . H1 H 0.2441 1.0116 0.2686 0.042 Uiso 1 1 calc R . . N1C N 0.2729(4) 1.2069(6) 0.2038(3) 0.0375(14) Uani 1 1 d . . . N2 N 0.4223(4) 1.0538(6) 0.1905(3) 0.0398(14) Uani 1 1 d . . . H2 H 0.4504 0.9895 0.1681 0.048 Uiso 1 1 calc R . . N2C N 0.0734(5) 1.5120(8) 0.2205(5) 0.071(2) Uani 1 1 d . . . N3 N 0.3171(4) 1.1450(7) 0.0707(3) 0.0470(16) Uani 1 1 d . . . H3 H 0.2649 1.1886 0.0613 0.056 Uiso 1 1 calc R . . N3C N 0.3488(5) 1.6016(7) 0.1756(4) 0.0574(19) Uani 1 1 d . . . N4 N 0.3161(4) 0.8958(6) 0.1061(3) 0.0402(14) Uani 1 1 d . . . H4 H 0.3533 0.8446 0.1323 0.048 Uiso 1 1 calc R . . N4C N 0.4423(5) 1.3705(7) 0.3560(3) 0.0491(16) Uani 1 1 d . . . N5 N 0.1674(4) 1.0227(6) 0.1355(3) 0.0406(15) Uani 1 1 d . . . H5C H 0.132 1.0651 0.1646 0.049 Uiso 1 1 calc R . . H5D H 0.1521 1.0446 0.0917 0.049 Uiso 1 1 calc R . . N5C N 0.1609(5) 1.3010(8) 0.3997(4) 0.061(2) Uani 1 1 d . . . N6C N 0.2481(7) 1.6870(7) 0.3824(4) 0.073(2) Uani 1 1 d . . . Na1 Na 0.5245(6) 1.1556(8) 0.4207(4) 0.173(3) Uani 1 1 d . . . O1 O 0.9213(6) 0.0362(10) 0.0315(5) 0.115(3) Uani 1 1 d . . . O2 O 0.2786(13) 0.6013(12) -0.0345(6) 0.203(7) Uani 1 1 d . . . O3 O 0.1896(11) 0.4834(15) 0.0716(6) 0.197(6) Uani 1 1 d . . . O4 O 0.1227(8) 0.2431(11) 0.0372(4) 0.140(4) Uani 1 1 d . . . O5 O 0.5751(13) 1.0383(15) 0.5385(7) 0.211(7) Uani 1 1 d . . . O6 O 1.0331(9) 0.1933(13) 0.2021(8) 0.083(5) Uiso 0.59(2) 1 d P A 1 O6' O 1.0683(12) 0.1552(18) 0.2459(10) 0.077(7) Uiso 0.41(2) 1 d P A 2 O7 O 1.2218(13) 0.0601(17) 0.3741(9) 0.103(8) Uiso 0.54(3) 1 d P B 1 O7' O 1.1470(17) 0.044(2) 0.3526(11) 0.117(10) Uiso 0.46(3) 1 d P B 2 O8 O 0.9446(8) 0.2265(12) 0.1005(6) 0.118(5) Uiso 0.801(16) 1 d P C 1 O8' O 0.854(2) 0.368(3) 0.0896(17) 0.067(12) Uiso 0.199(16) 1 d P C 2 O9 O 0.964(2) 0.439(3) -0.001(2) 0.178(16) Uiso 0.388(18) 1 d P . 1 O9' O 0.9768(11) 0.4545(15) 0.1153(8) 0.115(6) Uiso 0.612(18) 1 d P . 2 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 C1 0.050(4) 0.040(4) 0.043(4) 0.010(3) -0.002(3) -0.004(4) C1C 0.034(4) 0.032(4) 0.036(4) 0.001(3) 0.005(3) 0.006(3) C2 0.050(4) 0.046(5) 0.040(4) 0.002(3) -0.006(3) 0.008(4) C2C 0.049(5) 0.047(5) 0.042(4) 0.003(4) 0.009(4) 0.007(4) C3 0.052(5) 0.054(5) 0.039(4) -0.003(4) -0.009(4) 0.006(4) C3C 0.040(4) 0.039(4) 0.038(4) -0.004(3) -0.001(3) 0.012(3) C4 0.039(4) 0.058(5) 0.060(5) -0.005(4) 0.002(4) -0.013(4) C4C 0.042(4) 0.034(4) 0.034(4) -0.002(3) 0.008(3) -0.005(3) C5 0.049(5) 0.074(7) 0.075(6) 0.002(5) 0.016(5) -0.019(5) C5C 0.043(4) 0.038(4) 0.039(4) -0.006(3) 0.005(3) 0.002(3) C6 0.068(6) 0.075(7) 0.062(6) 0.024(5) 0.017(5) -0.011(5) C6C 0.066(5) 0.035(4) 0.036(4) 0.005(3) 0.004(4) 0.000(4) C7 0.050(5) 0.097(7) 0.031(4) -0.001(5) 0.006(3) 0.000(5) C8 0.045(4) 0.091(7) 0.039(4) -0.020(5) 0.011(4) 0.007(5) C9 0.058(5) 0.043(5) 0.045(4) -0.009(4) -0.004(4) -0.002(4) C10 0.036(4) 0.038(4) 0.052(5) 0.007(4) 0.002(3) -0.003(3) C11 0.049(5) 0.060(6) 0.066(6) 0.015(5) -0.008(4) -0.016(4) Co1 0.0330(5) 0.0341(5) 0.0302(5) -0.0004(4) 0.0067(4) 0.0041(4) Fe1 0.0369(6) 0.0344(6) 0.0372(6) -0.0028(5) 0.0061(4) 0.0034(5) N1 0.044(3) 0.031(3) 0.031(3) -0.002(3) 0.005(2) 0.002(3) N1C 0.043(3) 0.027(3) 0.043(3) 0.002(3) 0.009(3) 0.004(3) N2 0.032(3) 0.044(3) 0.043(3) -0.006(3) 0.002(3) 0.003(3) N2C 0.048(4) 0.080(6) 0.085(6) 0.009(5) 0.000(4) 0.014(4) N3 0.048(4) 0.057(4) 0.037(3) 0.009(3) 0.008(3) 0.000(3) N3C 0.059(4) 0.059(4) 0.054(4) 0.015(4) 0.008(4) -0.002(4) N4 0.042(3) 0.045(4) 0.034(3) -0.007(3) -0.001(3) 0.010(3) N4C 0.047(4) 0.051(4) 0.049(4) 0.008(3) -0.003(3) -0.001(3) N5 0.035(3) 0.046(4) 0.041(3) 0.010(3) 0.004(3) 0.006(3) N5C 0.057(4) 0.073(5) 0.054(4) 0.006(4) 0.014(4) -0.009(4) N6C 0.131(8) 0.040(4) 0.049(4) -0.009(4) 0.008(5) -0.009(5) Na1 0.215(8) 0.178(7) 0.130(5) 0.038(5) 0.056(5) 0.067(6) O1 0.087(6) 0.152(9) 0.108(7) 0.062(6) 0.018(5) 0.011(6) O2 0.38(2) 0.096(8) 0.139(10) 0.028(7) 0.082(12) 0.050(11) O3 0.246(16) 0.223(15) 0.119(9) -0.051(10) -0.040(10) -0.050(13) O4 0.205(11) 0.145(9) 0.071(5) 0.029(6) 0.027(6) 0.086(8) O5 0.30(2) 0.184(15) 0.155(12) 0.004(11) 0.026(12) 0.021(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 N1 1.497(9) . ? C1 C10 1.549(10) . ? C1C N1C 1.158(9) . ? C1C Fe1 1.890(7) . ? C2 N1 1.491(9) . ? C2 C3 1.496(11) . ? C2C N2C 1.171(10) . ? C2C Fe1 1.901(8) . ? C3 N2 1.498(9) . ? C3C N3C 1.159(10) . ? C3C Fe1 1.905(8) . ? C4 N2 1.487(10) . ? C4 C5 1.502(12) . ? C4C N4C 1.153(9) . ? C4C Fe1 1.921(8) . ? C5 C6 1.510(13) . ? C5C N5C 1.139(10) . ? C5C Fe1 1.907(8) . ? C6 N3 1.482(11) . ? C6C N6C 1.148(10) . ? C6C Fe1 1.937(8) . ? C7 C8 1.490(13) . ? C7 N3 1.505(11) . ? C8 N4 1.496(10) . ? C9 N4 1.505(10) . ? C9 C10 1.507(11) . ? C10 N5 1.484(9) . ? C10 C11 1.522(10) . ? Co1 N1C 1.886(6) . ? Co1 N1 1.930(6) . ? Co1 N5 1.952(6) . ? Co1 N4 1.953(6) . ? Co1 N2 1.956(6) . ? Co1 N3 1.957(6) . ? N3C Na1 2.745(10) 2_655 ? N4C Na1 2.831(10) . ? Na1 O5 2.65(2) 3_676 ? Na1 O5 2.676(16) . ? Na1 N3C 2.745(10) 2_645 ? O5 Na1 2.648(19) 3_676 ? O9 O9 1.66(7) 3_765 ? 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 N1 C1 C10 108.2(6) . . ? N1C C1C Fe1 176.7(6) . . ? N1 C2 C3 105.6(6) . . ? N2C C2C Fe1 177.3(8) . . ? C2 C3 N2 107.5(6) . . ? N3C C3C Fe1 177.8(7) . . ? N2 C4 C5 109.9(7) . . ? N4C C4C Fe1 178.6(7) . . ? C4 C5 C6 113.8(7) . . ? N5C C5C Fe1 178.0(7) . . ? N3 C6 C5 115.4(8) . . ? N6C C6C Fe1 177.0(9) . . ? C8 C7 N3 109.7(6) . . ? C7 C8 N4 108.0(6) . . ? N4 C9 C10 107.9(6) . . ? N5 C10 C9 103.7(6) . . ? N5 C10 C11 114.2(6) . . ? C9 C10 C11 111.9(7) . . ? N5 C10 C1 105.8(6) . . ? C9 C10 C1 110.4(6) . . ? C11 C10 C1 110.6(6) . . ? N1C Co1 N1 90.6(2) . . ? N1C Co1 N5 93.1(3) . . ? N1 Co1 N5 81.8(2) . . ? N1C Co1 N4 178.1(3) . . ? N1 Co1 N4 90.1(3) . . ? N5 Co1 N4 85.3(3) . . ? N1C Co1 N2 91.3(3) . . ? N1 Co1 N2 87.2(2) . . ? N5 Co1 N2 168.1(3) . . ? N4 Co1 N2 90.5(3) . . ? N1C Co1 N3 91.7(3) . . ? N1 Co1 N3 176.1(3) . . ? N5 Co1 N3 94.9(3) . . ? N4 Co1 N3 87.5(3) . . ? N2 Co1 N3 96.0(3) . . ? C1C Fe1 C2C 90.8(3) . . ? C1C Fe1 C3C 89.6(3) . . ? C2C Fe1 C3C 88.9(3) . . ? C1C Fe1 C5C 90.2(3) . . ? C2C Fe1 C5C 90.0(3) . . ? C3C Fe1 C5C 178.9(3) . . ? C1C Fe1 C4C 87.5(3) . . ? C2C Fe1 C4C 178.3(3) . . ? C3C Fe1 C4C 91.6(3) . . ? C5C Fe1 C4C 89.5(3) . . ? C1C Fe1 C6C 177.8(3) . . ? C2C Fe1 C6C 91.1(3) . . ? C3C Fe1 C6C 91.6(3) . . ? C5C Fe1 C6C 88.6(3) . . ? C4C Fe1 C6C 90.5(3) . . ? C2 N1 C1 116.5(6) . . ? C2 N1 Co1 109.0(4) . . ? C1 N1 Co1 110.1(4) . . ? C1C N1C Co1 174.8(6) . . ? C4 N2 C3 112.1(6) . . ? C4 N2 Co1 118.4(5) . . ? C3 N2 Co1 106.3(4) . . ? C6 N3 C7 115.7(7) . . ? C6 N3 Co1 116.8(5) . . ? C7 N3 Co1 108.4(5) . . ? C3C N3C Na1 155.5(7) . 2_655 ? C8 N4 C9 113.9(6) . . ? C8 N4 Co1 108.4(5) . . ? C9 N4 Co1 108.4(4) . . ? C4C N4C Na1 140.0(6) . . ? C10 N5 Co1 101.2(4) . . ? O5 Na1 O5 62.1(7) 3_676 . ? O5 Na1 N3C 116.2(5) 3_676 2_645 ? O5 Na1 N3C 107.9(5) . 2_645 ? O5 Na1 N4C 120.7(5) 3_676 . ? O5 Na1 N4C 147.8(5) . . ? N3C Na1 N4C 99.0(3) 2_645 . ? Na1 O5 Na1 117.9(7) 3_676 . ? #===END data_1464bm3 _database_code_CSD 174291 # cis-[L14CoNCFe(CN)5].4H2O _audit_creation_date 2001-11-15T11:41:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'cis-[L14CoNCFe(CN)5].4H2O' _chemical_formula_structural 'C17 H37 Co1 Fe1 N11 O4' _chemical_formula_sum 'C17 H37 Co Fe N11 O4' _chemical_formula_weight 574.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4920(10) _cell_length_b 14.709(2) _cell_length_c 18.760(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2619.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_factor_muR 0.062 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 0.9401 _exptl_absorpt_correction_T_ave 0.923 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.19514E-1 _diffrn_orient_matrix_ub_12 -0.25562E-1 _diffrn_orient_matrix_ub_13 0.48358E-1 _diffrn_orient_matrix_ub_21 0.97972E-1 _diffrn_orient_matrix_ub_22 -0.24938E-1 _diffrn_orient_matrix_ub_23 0.2006E-2 _diffrn_orient_matrix_ub_31 0.33639E-1 _diffrn_orient_matrix_ub_32 0.57882E-1 _diffrn_orient_matrix_ub_33 0.22239E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -1 _diffrn_standards_decay_corr_max 1.074 _diffrn_standards_decay_corr_min 0.959 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 1 -5 3 -1 5 2 3 2 _diffrn_reflns_number 2615 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.7592 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2615 _reflns_number_gt 482 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1134P)^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_number_reflns 2615 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.4689 _refine_ls_R_factor_gt 0.1079 _refine_ls_wR_factor_ref 0.3623 _refine_ls_wR_factor_gt 0.214 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(18) _refine_diff_density_max 0.82 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.135 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Co1 Co 0.8480(5) -0.0005(4) 0.9042(3) 0.0405(14) Uani 1 1 d . . . Fe1 Fe 1.2312(6) 0.0287(4) 1.0810(3) 0.0466(18) Uani 1 1 d . . . N4 N 0.691(3) -0.021(2) 0.8330(15) 0.047(10) Uiso 1 1 d . . . H1 H 0.6081 0.0001 0.8509 0.056 Uiso 1 1 d R . . N3 N 0.908(3) -0.126(2) 0.8853(16) 0.049(10) Uiso 1 1 d . . . H2 H 0.9971 -0.1209 0.8674 0.059 Uiso 1 1 d R . . N2 N 0.724(4) -0.031(3) 0.9823(18) 0.079(12) Uiso 1 1 d . . . H3 H 0.6405 -0.0504 0.9645 0.095 Uiso 1 1 d R . . N1 N 0.781(3) 0.128(2) 0.9174(19) 0.064(10) Uiso 1 1 d . . . H4 H 0.8508 0.1599 0.9394 0.076 Uiso 1 1 d R . . N5 N 0.944(4) 0.053(2) 0.8236(16) 0.064(12) Uiso 1 1 d . . . H5A H 1.0149 0.0894 0.8375 0.076 Uiso 1 1 d R . . H5B H 0.9772 0.0103 0.7937 0.076 Uiso 1 1 d R . . N1C N 1.002(2) 0.0193(18) 0.9675(12) 0.020(7) Uiso 1 1 d . . . N3C N 1.110(5) -0.142(3) 1.145(2) 0.086(15) Uiso 1 1 d . . . N2C N 1.426(4) -0.082(3) 0.990(2) 0.089(15) Uiso 1 1 d . . . N5C N 1.357(4) 0.203(2) 1.0133(16) 0.048(9) Uiso 1 1 d . . . N4C N 1.033(5) 0.141(3) 1.177(2) 0.105(16) Uiso 1 1 d . . . N6C N 1.451(5) 0.052(3) 1.198(2) 0.122(18) Uiso 1 1 d . . . C9 C 0.729(4) 0.028(3) 0.772(2) 0.061(13) Uiso 1 1 d . . . H1A H 0.6444 0.0524 0.7501 0.073 Uiso 1 1 d R . . H1B H 0.7733 -0.0127 0.7382 0.073 Uiso 1 1 d R . . C8 C 0.685(5) -0.119(3) 0.826(2) 0.059(14) Uiso 1 1 d . . . H2A H 0.6395 -0.1336 0.7811 0.071 Uiso 1 1 d R . . H2B H 0.6261 -0.1428 0.864 0.071 Uiso 1 1 d R . . C7 C 0.827(5) -0.164(3) 0.829(3) 0.088(18) Uiso 1 1 d . . . H3A H 0.8145 -0.2285 0.837 0.105 Uiso 1 1 d R . . H3B H 0.8753 -0.1557 0.7839 0.105 Uiso 1 1 d R . . C6 C 0.918(5) -0.192(3) 0.941(2) 0.085(16) Uiso 1 1 d . . . H4A H 1.0091 -0.1875 0.9641 0.102 Uiso 1 1 d R . . H4B H 0.9088 -0.2529 0.9216 0.102 Uiso 1 1 d R . . C5 C 0.799(6) -0.176(4) 0.998(3) 0.13(2) Uiso 1 1 d . . . H5C H 0.712 -0.1887 0.9731 0.153 Uiso 1 1 d R . . H5D H 0.8101 -0.2247 1.0327 0.153 Uiso 1 1 d R . . C4 C 0.770(6) -0.095(3) 1.039(3) 0.098(18) Uiso 1 1 d . . . H6A H 0.8551 -0.0735 1.0623 0.118 Uiso 1 1 d R . . H6B H 0.6971 -0.1048 1.0739 0.118 Uiso 1 1 d R . . C3 C 0.702(5) 0.056(3) 1.022(2) 0.076(16) Uiso 1 1 d . . . H7A H 0.7865 0.0737 1.0473 0.091 Uiso 1 1 d R . . H7B H 0.6252 0.0499 1.0553 0.091 Uiso 1 1 d R . . C2 C 0.666(5) 0.127(3) 0.963(2) 0.060(13) Uiso 1 1 d . . . H8A H 0.5822 0.1091 0.937 0.072 Uiso 1 1 d R . . H8B H 0.6508 0.1869 0.9833 0.072 Uiso 1 1 d R . . C1 C 0.761(6) 0.167(3) 0.846(2) 0.088(17) Uiso 1 1 d . . . H9A H 0.8036 0.2268 0.8442 0.105 Uiso 1 1 d R . . H9B H 0.6612 0.1732 0.8365 0.105 Uiso 1 1 d R . . C10 C 0.829(6) 0.105(4) 0.791(3) 0.100(19) Uiso 1 1 d . . . C11 C 0.880(7) 0.153(4) 0.718(3) 0.17(3) Uiso 1 1 d . . . H11A H 0.9473 0.1995 0.7281 0.258 Uiso 1 1 d R . . H11B H 0.7996 0.1796 0.6942 0.258 Uiso 1 1 d R . . H11C H 0.9215 0.1082 0.687 0.258 Uiso 1 1 d R . . C1C C 1.090(4) 0.022(3) 1.0073(18) 0.039(11) Uiso 1 1 d . . . C3C C 1.152(5) -0.080(3) 1.122(2) 0.054(13) Uiso 1 1 d . . . C2C C 1.354(5) -0.042(3) 1.022(2) 0.065(14) Uiso 1 1 d . . . C5C C 1.314(4) 0.137(3) 1.0361(19) 0.038(11) Uiso 1 1 d . . . C4C C 1.101(5) 0.103(3) 1.135(2) 0.056(14) Uiso 1 1 d . . . C6C C 1.362(6) 0.041(3) 1.154(2) 0.075(16) Uiso 1 1 d . . . O1 O 0.406(5) 0.038(3) 0.838(2) 0.167(19) Uiso 1 1 d . . . O2 O 1.100(5) 0.215(3) 0.870(2) 0.171(18) Uiso 1 1 d . . . O3 O 0.365(6) 0.210(4) 0.800(3) 0.24(3) Uiso 1 1 d . . . O4 O 1.288(4) 0.116(3) 1.348(2) 0.144(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.029(3) 0.044(3) 0.049(3) 0.007(4) -0.008(3) -0.002(3) Fe1 0.045(4) 0.051(4) 0.044(3) 0.005(4) -0.011(3) -0.005(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Co1 N1C 1.91(2) . ? Co1 N2 1.93(3) . ? Co1 N5 1.93(3) . ? Co1 N3 1.96(3) . ? Co1 N1 2.01(3) . ? Co1 N4 2.02(3) . ? Fe1 C6C 1.86(5) . ? Fe1 C2C 1.91(5) . ? Fe1 C3C 1.92(5) . ? Fe1 C1C 1.93(4) . ? Fe1 C4C 1.94(5) . ? Fe1 C5C 1.97(4) . ? N4 C9 1.40(4) . ? N4 C8 1.44(4) . ? N3 C7 1.42(5) . ? N3 C6 1.44(4) . ? N2 C4 1.48(5) . ? N2 C3 1.49(4) . ? N1 C2 1.38(5) . ? N1 C1 1.46(5) . ? N5 C10 1.47(6) . ? N1C C1C 1.12(3) . ? N3C C3C 1.08(5) . ? N2C C2C 1.08(5) . ? N5C C5C 1.13(4) . ? N4C C4C 1.16(5) . ? N6C C6C 1.19(6) . ? C9 C10 1.52(6) . ? C8 C7 1.51(6) . ? C6 C5 1.56(6) . ? C5 C4 1.45(6) . ? C3 C2 1.56(5) . ? C1 C10 1.53(6) . ? C10 C11 1.62(7) . ? 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 N1C Co1 N2 91.6(13) . . ? N1C Co1 N5 93.7(12) . . ? N2 Co1 N5 167.1(15) . . ? N1C Co1 N3 91.9(12) . . ? N2 Co1 N3 95.6(15) . . ? N5 Co1 N3 95.9(15) . . ? N1C Co1 N1 91.3(13) . . ? N2 Co1 N1 86.1(15) . . ? N5 Co1 N1 82.0(14) . . ? N3 Co1 N1 176.3(14) . . ? N1C Co1 N4 177.3(11) . . ? N2 Co1 N4 91.0(13) . . ? N5 Co1 N4 83.8(13) . . ? N3 Co1 N4 87.3(13) . . ? N1 Co1 N4 89.4(14) . . ? C6C Fe1 C2C 94.1(19) . . ? C6C Fe1 C3C 92.7(19) . . ? C2C Fe1 C3C 90.9(17) . . ? C6C Fe1 C1C 176.6(19) . . ? C2C Fe1 C1C 89.1(18) . . ? C3C Fe1 C1C 88.5(17) . . ? C6C Fe1 C4C 89(2) . . ? C2C Fe1 C4C 176(2) . . ? C3C Fe1 C4C 90.8(18) . . ? C1C Fe1 C4C 87.7(17) . . ? C6C Fe1 C5C 88.3(19) . . ? C2C Fe1 C5C 87.2(17) . . ? C3C Fe1 C5C 177.9(15) . . ? C1C Fe1 C5C 90.6(15) . . ? C4C Fe1 C5C 91.1(17) . . ? C9 N4 C8 117(3) . . ? C9 N4 Co1 106(2) . . ? C8 N4 Co1 104(3) . . ? C7 N3 C6 108(3) . . ? C7 N3 Co1 110(3) . . ? C6 N3 Co1 122(3) . . ? C4 N2 C3 103(3) . . ? C4 N2 Co1 121(3) . . ? C3 N2 Co1 105(3) . . ? C2 N1 C1 118(4) . . ? C2 N1 Co1 108(3) . . ? C1 N1 Co1 107(3) . . ? C10 N5 Co1 101(3) . . ? C1C N1C Co1 173(3) . . ? N4 C9 C10 111(3) . . ? N4 C8 C7 113(4) . . ? N3 C7 C8 110(4) . . ? N3 C6 C5 111(4) . . ? C4 C5 C6 128(5) . . ? C5 C4 N2 102(4) . . ? N2 C3 C2 105(3) . . ? N1 C2 C3 106(4) . . ? N1 C1 C10 110(4) . . ? N5 C10 C9 100(4) . . ? N5 C10 C1 110(4) . . ? C9 C10 C1 110(5) . . ? N5 C10 C11 111(4) . . ? C9 C10 C11 108(4) . . ? C1 C10 C11 116(5) . . ? N1C C1C Fe1 176(3) . . ? N3C C3C Fe1 179(5) . . ? N2C C2C Fe1 178(5) . . ? N5C C5C Fe1 176(3) . . ? N4C C4C Fe1 169(4) . . ? N6C C6C Fe1 175(5) . . ? #===END data_bm8130 _database_code_CSD 174292 # trans-[L14CoNCFe(CN)5].5H2O _audit_creation_date 2001-11-15T11:32:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'trans-[L14CoNCFe(CN)5].5H2O' _chemical_formula_structural 'C17 H37 Co1 Fe1 N11 O5' _chemical_formula_sum 'C17 H37 Co Fe N11 O5' _chemical_formula_weight 590.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.965(2) _cell_length_b 13.3110(10) _cell_length_c 20.226(4) _cell_angle_alpha 90 _cell_angle_beta 90.720(10) _cell_angle_gamma 90 _cell_volume 2682.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_factor_muR 0.121 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7759 _exptl_absorpt_correction_T_max 0.8861 _exptl_absorpt_correction_T_ave 0.861 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.65666E-1 _diffrn_orient_matrix_ub_12 -0.55771E-1 _diffrn_orient_matrix_ub_13 0.6624E-2 _diffrn_orient_matrix_ub_21 -0.69478E-1 _diffrn_orient_matrix_ub_22 0.49915E-1 _diffrn_orient_matrix_ub_23 0.13493E-1 _diffrn_orient_matrix_ub_31 -0.30485E-1 _diffrn_orient_matrix_ub_32 0.6424E-2 _diffrn_orient_matrix_ub_33 -0.47121E-1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -5 _diffrn_standards_decay_corr_max 1.04 _diffrn_standards_decay_corr_min 0.92 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -5 -3 2 0 9 1 -2 1 -10 _diffrn_reflns_number 4995 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_unetI/netI 0.1231 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4706 _reflns_number_gt 2082 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0459P)^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_number_reflns 4706 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1658 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.366 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.0571(7) 0.0419(5) 0.2451(3) 0.070(2) Uani 1 1 d . . . H1A H -0.0329 0.0551 0.2299 0.106 Uiso 1 1 calc R . . H1B H 0.0708 0.0721 0.2877 0.106 Uiso 1 1 calc R . . H1C H 0.0708 -0.0293 0.2483 0.106 Uiso 1 1 calc R . . C1C C 0.5008(5) 0.2334(4) 0.0193(2) 0.0330(13) Uani 1 1 d . . . C2 C 0.1565(6) 0.0864(4) 0.1962(3) 0.0443(15) Uani 1 1 d . . . C2C C 0.7415(6) 0.1390(5) -0.0018(3) 0.0432(16) Uani 1 1 d . . . C3 C 0.2995(6) 0.0674(4) 0.2181(3) 0.0492(17) Uani 1 1 d . . . H3A H 0.3112 0.0866 0.2641 0.059 Uiso 1 1 calc R . . H3B H 0.3202 -0.0035 0.2141 0.059 Uiso 1 1 calc R . . C3C C 0.7260(6) 0.3448(5) -0.0071(3) 0.0424(16) Uani 1 1 d . . . C4 C 0.4970(6) 0.1854(4) 0.2122(3) 0.0482(16) Uani 1 1 d . . . H4A H 0.5719 0.1992 0.1834 0.058 Uiso 1 1 calc R . . H4B H 0.5298 0.147 0.2498 0.058 Uiso 1 1 calc R . . C4C C 0.5238(6) 0.3291(5) -0.0992(3) 0.0433(16) Uani 1 1 d . . . C5 C 0.4362(6) 0.2817(5) 0.2351(3) 0.0466(15) Uani 1 1 d . . . H5A H 0.505 0.3254 0.2536 0.056 Uiso 1 1 calc R . . H5B H 0.3702 0.2687 0.2689 0.056 Uiso 1 1 calc R . . C5C C 0.5472(6) 0.1211(5) -0.0916(3) 0.0471(17) Uani 1 1 d . . . C6 C 0.2906(6) 0.4190(4) 0.1935(3) 0.0542(18) Uani 1 1 d . . . H6A H 0.3481 0.4687 0.2145 0.065 Uiso 1 1 calc R . . H6B H 0.2221 0.3999 0.2247 0.065 Uiso 1 1 calc R . . C6C C 0.7603(6) 0.2359(4) -0.1214(3) 0.0464(16) Uani 1 1 d . . . C7 C 0.2244(7) 0.4644(4) 0.1326(3) 0.0540(18) Uani 1 1 d . . . H7A H 0.1886 0.5298 0.1442 0.065 Uiso 1 1 calc R . . H7B H 0.2922 0.4747 0.0993 0.065 Uiso 1 1 calc R . . C8 C 0.1129(6) 0.4016(4) 0.1033(3) 0.0516(17) Uani 1 1 d . . . H8A H 0.0513 0.3824 0.1379 0.062 Uiso 1 1 calc R . . H8B H 0.0634 0.4409 0.0708 0.062 Uiso 1 1 calc R . . C9 C 0.0603(6) 0.2445(4) 0.0421(3) 0.0504(17) Uani 1 1 d . . . H9A H 0.0179 0.2778 0.0046 0.061 Uiso 1 1 calc R . . H9B H -0.0078 0.2302 0.0746 0.061 Uiso 1 1 calc R . . C10 C 0.1264(6) 0.1494(4) 0.0205(3) 0.0482(16) Uani 1 1 d . . . H10A H 0.0593 0.101 0.0063 0.058 Uiso 1 1 calc R . . H10B H 0.1855 0.1626 -0.0163 0.058 Uiso 1 1 calc R . . C11 C 0.1257(6) 0.0491(4) 0.1258(3) 0.0501(17) Uani 1 1 d . . . H11A H 0.1492 -0.0214 0.1221 0.06 Uiso 1 1 calc R . . H11B H 0.0306 0.0561 0.1162 0.06 Uiso 1 1 calc R . . Co1 Co 0.28480(7) 0.22256(5) 0.12452(3) 0.0315(2) Uani 1 1 d . . . Fe1 Fe 0.63241(8) 0.23482(6) -0.05020(4) 0.0365(2) Uani 1 1 d . . . N1 N 0.3923(5) 0.1276(3) 0.1759(2) 0.0393(12) Uani 1 1 d . . . H1 H 0.4336 0.085 0.1474 0.047 Uiso 1 1 calc R . . N1C N 0.4216(4) 0.2318(3) 0.0593(2) 0.0341(11) Uani 1 1 d . . . N2 N 0.3712(4) 0.3297(3) 0.1764(2) 0.0375(12) Uani 1 1 d . . . H2 H 0.4396 0.3528 0.1511 0.045 Uiso 1 1 calc R . . N2C N 0.8039(5) 0.0805(4) 0.0257(3) 0.0648(17) Uani 1 1 d . . . N3 N 0.1671(4) 0.3099(3) 0.0714(2) 0.0393(12) Uani 1 1 d . . . H3 H 0.2172 0.3316 0.037 0.047 Uiso 1 1 calc R . . N3C N 0.7818(6) 0.4084(4) 0.0194(3) 0.0630(16) Uani 1 1 d . . . N4 N 0.2046(5) 0.1093(3) 0.0776(2) 0.0387(12) Uani 1 1 d . . . H4 H 0.2718 0.07 0.0619 0.046 Uiso 1 1 calc R . . N4C N 0.4602(6) 0.3864(4) -0.1276(3) 0.0662(17) Uani 1 1 d . . . N5 N 0.1471(4) 0.1971(3) 0.1900(2) 0.0377(12) Uani 1 1 d . . . H5C H 0.1659 0.228 0.2285 0.045 Uiso 1 1 calc R . . H5D H 0.0654 0.2164 0.1753 0.045 Uiso 1 1 calc R . . N5C N 0.5023(6) 0.0508(4) -0.1158(3) 0.0736(19) Uani 1 1 d . . . N6C N 0.8338(6) 0.2357(4) -0.1645(3) 0.0780(19) Uani 1 1 d . . . O1 O 0.1791(6) 0.1110(4) 0.4363(2) 0.1032(19) Uani 1 1 d . . . O2 O 0.2254(6) 0.4703(5) 0.3553(3) 0.128(2) Uani 1 1 d . . . O3 O 0.8655(5) 0.2328(5) -0.3058(2) 0.112(2) Uani 1 1 d . . . O4 O 0.3633(4) 0.9098(3) 0.3543(2) 0.0699(13) Uani 1 1 d . . . O5 O 0.1320(4) 0.2752(4) 0.3247(2) 0.0860(16) Uani 1 1 d . . . H4OA H 0.2941 0.8982 0.393 0.129 Uiso 1 1 d R . . H2OB H 0.2052 0.471 0.3997 0.129 Uiso 1 1 d R . . H5OA H 0.1304 0.2629 0.3606 0.129 Uiso 1 1 d R . . H2OA H 0.2096 0.5488 0.3339 0.129 Uiso 1 1 d R . . H3OB H 0.7915 0.2212 -0.3237 0.129 Uiso 1 1 d R . . H5OB H 0.0872 0.2834 0.289 0.129 Uiso 1 1 d R . . H3OA H 0.868 0.3002 -0.2904 0.129 Uiso 1 1 d R . . H4OB H 0.4316 0.983 0.3609 0.129 Uiso 1 1 d R . . H1OA H 0.2352 0.0759 0.4645 0.129 Uiso 1 1 d R . . H1OB H 0.2429 0.1568 0.4302 0.129 Uiso 1 1 d 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 C1 0.084(5) 0.070(5) 0.058(4) 0.004(4) 0.032(4) -0.033(4) C1C 0.034(3) 0.040(3) 0.025(3) -0.002(3) 0.000(3) -0.003(3) C2 0.055(4) 0.042(4) 0.036(4) 0.003(3) 0.017(3) -0.011(3) C2C 0.038(4) 0.045(4) 0.047(4) -0.004(3) 0.005(3) 0.003(3) C3 0.066(5) 0.042(4) 0.039(4) 0.006(3) 0.009(3) -0.008(3) C3C 0.042(4) 0.049(4) 0.036(4) 0.004(3) 0.009(3) -0.003(3) C4 0.046(4) 0.054(4) 0.044(4) 0.009(3) -0.001(3) -0.001(3) C4C 0.048(4) 0.048(4) 0.034(4) -0.008(3) 0.007(3) 0.000(3) C5 0.049(4) 0.064(4) 0.027(3) 0.000(3) -0.002(3) -0.016(4) C5C 0.052(4) 0.044(4) 0.046(4) -0.007(3) 0.019(3) 0.002(3) C6 0.068(5) 0.041(4) 0.055(4) -0.025(3) 0.022(4) -0.011(3) C6C 0.048(4) 0.043(4) 0.049(4) -0.006(3) 0.018(3) -0.003(3) C7 0.071(5) 0.033(4) 0.058(5) -0.011(3) 0.017(4) 0.004(3) C8 0.057(4) 0.046(4) 0.051(4) 0.001(3) 0.008(3) 0.012(3) C9 0.036(3) 0.069(5) 0.046(4) 0.002(3) -0.007(3) -0.006(3) C10 0.053(4) 0.054(4) 0.038(4) -0.012(3) -0.001(3) -0.008(3) C11 0.055(4) 0.047(4) 0.049(4) -0.004(3) 0.016(3) -0.014(3) Co1 0.0321(4) 0.0359(4) 0.0268(4) -0.0027(4) 0.0085(3) -0.0024(4) Fe1 0.0372(5) 0.0400(5) 0.0326(5) 0.0002(4) 0.0127(4) -0.0008(4) N1 0.047(3) 0.038(3) 0.033(3) 0.002(2) 0.012(3) -0.001(2) N1C 0.036(3) 0.039(3) 0.027(2) 0.002(2) 0.009(2) 0.001(2) N2 0.038(3) 0.048(3) 0.026(3) -0.010(2) 0.009(2) -0.011(2) N2C 0.051(4) 0.065(4) 0.079(5) 0.020(3) 0.004(3) 0.007(3) N3 0.035(3) 0.043(3) 0.040(3) -0.002(2) 0.009(2) -0.003(2) N3C 0.062(4) 0.063(4) 0.064(4) -0.010(3) 0.006(3) -0.010(3) N4 0.043(3) 0.039(3) 0.034(3) -0.008(2) 0.012(2) -0.003(2) N4C 0.070(4) 0.073(4) 0.056(4) -0.002(3) -0.005(3) 0.019(3) N5 0.035(3) 0.044(3) 0.034(3) -0.006(2) 0.008(2) -0.007(2) N5C 0.085(5) 0.053(4) 0.083(5) -0.023(3) 0.022(4) -0.009(4) N6C 0.081(4) 0.081(4) 0.074(4) 0.004(4) 0.053(4) -0.001(4) O1 0.152(5) 0.074(4) 0.084(4) 0.006(3) 0.028(4) 0.013(4) O2 0.098(4) 0.201(7) 0.084(4) -0.044(4) -0.009(4) 0.006(5) O3 0.056(3) 0.208(6) 0.074(3) -0.024(4) 0.014(3) -0.017(4) O4 0.075(3) 0.071(3) 0.063(3) 0.002(2) 0.015(3) 0.015(3) O5 0.081(3) 0.133(5) 0.044(3) -0.023(3) 0.010(3) -0.004(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.528(7) . ? C1C N1C 1.138(5) . ? C1C Fe1 1.934(6) . ? C2 N5 1.481(6) . ? C2 C3 1.508(8) . ? C2 C11 1.536(7) . ? C2C N2C 1.138(7) . ? C2C Fe1 1.934(7) . ? C3 N1 1.498(6) . ? C3C N3C 1.142(7) . ? C3C Fe1 1.937(7) . ? C4 N1 1.484(7) . ? C4 C5 1.494(8) . ? C4C N4C 1.142(7) . ? C4C Fe1 1.924(7) . ? C5 N2 1.490(6) . ? C5C N5C 1.145(7) . ? C5C Fe1 1.922(7) . ? C6 N2 1.478(7) . ? C6 C7 1.515(8) . ? C6C N6C 1.146(6) . ? C6C Fe1 1.934(6) . ? C7 C8 1.507(8) . ? C8 N3 1.486(6) . ? C9 N3 1.491(6) . ? C9 C10 1.496(7) . ? C10 N4 1.485(7) . ? C11 N4 1.492(6) . ? Co1 N1C 1.913(4) . ? Co1 N4 1.948(4) . ? Co1 N5 1.948(4) . ? Co1 N1 1.948(4) . ? Co1 N2 1.963(4) . ? Co1 N3 1.962(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 N1C C1C Fe1 178.7(5) . . ? N5 C2 C3 104.5(5) . . ? N5 C2 C1 113.6(5) . . ? C3 C2 C1 111.3(5) . . ? N5 C2 C11 103.3(5) . . ? C3 C2 C11 113.3(5) . . ? C1 C2 C11 110.5(5) . . ? N2C C2C Fe1 178.1(6) . . ? N1 C3 C2 109.3(5) . . ? N3C C3C Fe1 178.6(6) . . ? N1 C4 C5 108.3(5) . . ? N4C C4C Fe1 178.8(6) . . ? C4 C5 N2 107.1(4) . . ? N5C C5C Fe1 176.6(6) . . ? N2 C6 C7 111.4(5) . . ? N6C C6C Fe1 178.4(6) . . ? C8 C7 C6 114.1(5) . . ? N3 C8 C7 110.9(5) . . ? N3 C9 C10 107.2(4) . . ? N4 C10 C9 107.8(4) . . ? N4 C11 C2 109.3(4) . . ? N1C Co1 N4 90.35(18) . . ? N1C Co1 N5 173.67(19) . . ? N4 Co1 N5 84.70(18) . . ? N1C Co1 N1 91.01(18) . . ? N4 Co1 N1 88.7(2) . . ? N5 Co1 N1 84.95(19) . . ? N1C Co1 N2 90.56(18) . . ? N4 Co1 N2 175.8(2) . . ? N5 Co1 N2 94.09(18) . . ? N1 Co1 N2 87.25(18) . . ? N1C Co1 N3 90.63(18) . . ? N4 Co1 N3 87.31(19) . . ? N5 Co1 N3 93.07(19) . . ? N1 Co1 N3 175.66(19) . . ? N2 Co1 N3 96.76(19) . . ? C5C Fe1 C4C 92.7(3) . . ? C5C Fe1 C6C 88.5(2) . . ? C4C Fe1 C6C 89.1(3) . . ? C5C Fe1 C2C 86.7(3) . . ? C4C Fe1 C2C 179.3(3) . . ? C6C Fe1 C2C 90.6(2) . . ? C5C Fe1 C1C 90.5(2) . . ? C4C Fe1 C1C 89.9(2) . . ? C6C Fe1 C1C 178.5(2) . . ? C2C Fe1 C1C 90.4(2) . . ? C5C Fe1 C3C 177.0(3) . . ? C4C Fe1 C3C 90.2(3) . . ? C6C Fe1 C3C 90.7(2) . . ? C2C Fe1 C3C 90.4(2) . . ? C1C Fe1 C3C 90.4(2) . . ? C4 N1 C3 115.5(4) . . ? C4 N1 Co1 107.8(3) . . ? C3 N1 Co1 108.2(4) . . ? C1C N1C Co1 176.9(5) . . ? C6 N2 C5 113.0(4) . . ? C6 N2 Co1 118.2(4) . . ? C5 N2 Co1 107.3(3) . . ? C8 N3 C9 113.0(4) . . ? C8 N3 Co1 117.8(4) . . ? C9 N3 Co1 106.9(3) . . ? C10 N4 C11 115.2(5) . . ? C10 N4 Co1 108.0(3) . . ? C11 N4 Co1 108.3(3) . . ? C2 N5 Co1 100.8(3) . . ? #===END