# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_compound_CoHBpe _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- archive.cif' _publ_contact_author ; Dra. Miren Karmele Urtiaga Greaves Facultad de Ciencia y Tecnolog\'ia Dpto. de Mineralog\'ia y Petrolog\'ia Universidad del Pa\'is Vasco Apartado 644 48080 Bilbao Spain ; _publ_contact_author_phone '34 4 601000 ext 5372' _publ_contact_author_fax '34 4 4648500' _publ_contact_author_email karmele.urtiaga@ehu.es loop_ _publ_author_name _publ_author_address 'Roberto F. de Luis' ; Dpto. de Mineralog\'ia y Petrolog\'ia Facultad de Ciencia y Tecnolog\'ia Uiversidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; "Jos\'e L. Mesa " ; Dpto. Qu\'imica Inorg\'anica Facultad de Ciencia y Tecnolog\'ia Uiversidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; 'M. Karmele Urtiaga' ; Dpto. de Mineralog\'ia y Petrolog\'ia Facultad de Ciencia y Tecnolog\'ia Uiversidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; "Mar\'ia I. Arriortua" ; Dpto. de Mineralog\'ia y Petrolog\'ia Facultad de Ciencia y Tecnolog\'ia Uiversidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; "Te\'ofilo Rojo" ; Dpto. Qu\'imica Inorg\'anica Facultad de Ciencia y Tecnolog\'ia Uiversidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; _publ_requested_category FM _publ_contact_author_name 'Dra. Miren Karmele Urtiaga Greaves' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-03-12 at 10:03:20 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : ni567_i ni567_i_exp struct data_CoHBpe100K _database_code_depnum_ccdc_archive 'CCDC 818190' #TrackingRef '- archive.cif' _audit_creation_date 2010-02-24T16:26:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H22 Co N4 O12 V4' _chemical_formula_sum 'C24 H22 Co N4 O12 V4' _chemical_formula_weight 821.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.4705(3) _cell_length_b 11.8919(3) _cell_length_c 7.8490(2) _cell_angle_alpha 88.252(2) _cell_angle_beta 95.429(2) _cell_angle_gamma 92.534(2) _cell_volume 1435.62(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15320 _cell_measurement_theta_min 2.6019 _cell_measurement_theta_max 32.4401 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.3153 _exptl_crystal_size_mid 0.1371 _exptl_crystal_size_min 0.0755 _exptl_crystal_density_diffrn 1.9 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.89 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.676 _exptl_absorpt_correction_T_max 0.877 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 8.3504 _diffrn_orient_matrix_ub_11 0.0185059924 _diffrn_orient_matrix_ub_12 0.0114414579 _diffrn_orient_matrix_ub_13 -0.0452791369 _diffrn_orient_matrix_ub_21 0.0030040807 _diffrn_orient_matrix_ub_22 -0.058589162 _diffrn_orient_matrix_ub_23 -0.0070559076 _diffrn_orient_matrix_ub_31 -0.0888357767 _diffrn_orient_matrix_ub_32 0.0020538392 _diffrn_orient_matrix_ub_33 -0.0052763378 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0379 _diffrn_reflns_number 38209 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 32.51 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 9571 _reflns_number_gt 6993 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0421P)^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 9571 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.707 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.12 #----------------------------------------------------------------------------# # 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' 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' V V 0.3005 0.5294 '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' 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 -0.17735(10) -0.05421(14) 0.6174(2) 0.0144(3) Uani 1 1 d . . . H1 H -0.1535 -0.1266 0.6292 0.017 Uiso 1 1 calc R . . C2 C -0.26249(11) -0.04416(14) 0.6508(2) 0.0156(3) Uani 1 1 d . . . H2 H -0.2961 -0.1088 0.6832 0.019 Uiso 1 1 calc R . . C3 C -0.29929(10) 0.06142(13) 0.6370(2) 0.0110(3) Uani 1 1 d . . . C4 C -0.24511(10) 0.15251(14) 0.5916(2) 0.0144(3) Uani 1 1 d . . . H4 H -0.2662 0.2265 0.5837 0.017 Uiso 1 1 calc R . . C5 C -0.16049(10) 0.13461(13) 0.5580(2) 0.0134(3) Uani 1 1 d . . . H5 H -0.1251 0.1975 0.5257 0.016 Uiso 1 1 calc R . . C6 C -0.38937(10) 0.07946(14) 0.6697(2) 0.0120(3) Uani 1 1 d . . . H6 H -0.4102 0.1533 0.6527 0.014 Uiso 1 1 calc R . . C7 C -0.44415(10) -0.00248(14) 0.7222(2) 0.0137(3) Uani 1 1 d . . . H7 H -0.4233 -0.0766 0.7326 0.016 Uiso 1 1 calc R . . C8 C -0.66247(11) -0.07381(15) 0.8706(2) 0.0170(3) Uani 1 1 d . . . H8 H -0.694 -0.1386 0.9092 0.02 Uiso 1 1 calc R . . C9 C -0.57982(10) -0.08321(14) 0.8226(2) 0.0161(3) Uani 1 1 d . . . H9 H -0.5543 -0.1546 0.8287 0.019 Uiso 1 1 calc R . . C10 C -0.53303(10) 0.01207(14) 0.7646(2) 0.0118(3) Uani 1 1 d . . . C11 C -0.57376(10) 0.11498(14) 0.7566(2) 0.0129(3) Uani 1 1 d . . . H11 H -0.5447 0.181 0.7156 0.015 Uiso 1 1 calc R . . C12 C -0.65605(10) 0.12068(14) 0.8080(2) 0.0129(3) Uani 1 1 d . . . H12 H -0.6831 0.1909 0.805 0.015 Uiso 1 1 calc R . . C13 C -0.33427(10) 0.42609(14) 0.3631(2) 0.0140(3) Uani 1 1 d . . . H13 H -0.3684 0.3582 0.3473 0.017 Uiso 1 1 calc R . . C14 C -0.24841(11) 0.42722(14) 0.3270(2) 0.0145(3) Uani 1 1 d . . . H14 H -0.2246 0.3616 0.2877 0.017 Uiso 1 1 calc R . . C15 C -0.19713(10) 0.52693(14) 0.3493(2) 0.0120(3) Uani 1 1 d . . . C16 C -0.23722(10) 0.62070(14) 0.4035(2) 0.0134(3) Uani 1 1 d . . . H16 H -0.2054 0.6905 0.4175 0.016 Uiso 1 1 calc R . . C17 C -0.32336(10) 0.61142(14) 0.4365(2) 0.0137(3) Uani 1 1 d . . . H17 H -0.3494 0.6762 0.4734 0.016 Uiso 1 1 calc R . . C18 C -0.10550(10) 0.53797(14) 0.3161(2) 0.0133(3) Uani 1 1 d . . . H18 H -0.0783 0.6111 0.3222 0.016 Uiso 1 1 calc R . . C19 C -0.05700(10) 0.45319(15) 0.2779(2) 0.0142(3) Uani 1 1 d . . . H19 H -0.0826 0.3791 0.2793 0.017 Uiso 1 1 calc R . . C20 C 0.16519(10) 0.38224(14) 0.1797(2) 0.0145(3) Uani 1 1 d . . . H20 H 0.1987 0.3174 0.1764 0.017 Uiso 1 1 calc R . . C21 C 0.08223(10) 0.37201(14) 0.2296(2) 0.0140(3) Uani 1 1 d . . . H21 H 0.0586 0.3001 0.261 0.017 Uiso 1 1 calc R . . C22 C 0.03281(10) 0.46706(14) 0.2342(2) 0.0117(3) Uani 1 1 d . . . C23 C 0.07084(11) 0.57213(14) 0.1883(2) 0.0153(3) Uani 1 1 d . . . H23 H 0.0392 0.6386 0.1913 0.018 Uiso 1 1 calc R . . C24 C 0.15398(11) 0.57811(15) 0.1392(2) 0.0170(3) Uani 1 1 d . . . H24 H 0.1799 0.6487 0.1076 0.02 Uiso 1 1 calc R . . N1 N -0.12637(8) 0.03303(12) 0.56904(17) 0.0113(3) Uani 1 1 d . . . N2 N -0.69825(9) 0.02676(12) 0.86261(17) 0.0135(3) Uani 1 1 d . . . H2A H -0.751 0.0318 0.894 0.016 Uiso 1 1 calc R . . N3 N -0.37208(9) 0.51578(12) 0.41921(17) 0.0123(3) Uani 1 1 d . . . N4 N 0.19863(9) 0.48328(12) 0.13601(17) 0.0141(3) Uani 1 1 d . . . H4A H 0.2517 0.4883 0.104 0.017 Uiso 1 1 calc R . . O1 O 0.05949(7) 0.13550(9) 0.63675(13) 0.0117(2) Uani 1 1 d . . . O2 O -0.01494(7) 0.17130(9) 0.94276(14) 0.0131(2) Uani 1 1 d . . . O3 O 0.15663(7) 0.24212(10) 0.88480(14) 0.0144(2) Uani 1 1 d . . . O4 O 0.13181(7) 0.01285(9) 0.93016(14) 0.0109(2) Uani 1 1 d . . . O5 O 0.15436(7) -0.21464(9) 0.86729(14) 0.0130(2) Uani 1 1 d . . . O6 O -0.01731(7) 0.11138(9) 0.29380(14) 0.0121(2) Uani 1 1 d . . . O7 O -0.66720(7) 0.71207(9) 0.09960(15) 0.0146(2) Uani 1 1 d . . . O8 O -0.63073(7) 0.48736(9) 0.07031(14) 0.0108(2) Uani 1 1 d . . . O9 O -0.65425(7) 0.25545(9) 0.13777(15) 0.0142(2) Uani 1 1 d . . . O10 O -0.49815(8) 0.32387(10) 0.00179(15) 0.0167(3) Uani 1 1 d . . . O11 O -0.53350(7) 0.37274(10) 0.33434(14) 0.0133(2) Uani 1 1 d . . . O12 O -0.45153(8) 0.37413(9) 0.66978(14) 0.0133(2) Uani 1 1 d . . . V1 V 0.082792(16) 0.14270(2) 0.84740(3) 0.00740(6) Uani 1 1 d . . . V2 V 0.079723(16) -0.12522(2) 0.88901(3) 0.00728(6) Uani 1 1 d . . . V3 V -0.579621(16) 0.35622(2) 0.13713(3) 0.00747(6) Uani 1 1 d . . . V4 V -0.586983(16) 0.62791(2) 0.12551(3) 0.00750(6) Uani 1 1 d . . . Co1 Co 0 0 0.5 0.00741(6) Uani 1 2 d S . . Co2 Co -0.5 0.5 0.5 0.00825(6) Uani 1 2 d S . . 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 0.0121(8) 0.0122(8) 0.0195(8) 0.0020(6) 0.0053(6) 0.0017(6) C2 0.0121(8) 0.0134(8) 0.0221(8) 0.0023(6) 0.0074(7) -0.0005(6) C3 0.0085(7) 0.0125(7) 0.0121(7) -0.0012(6) 0.0021(6) 0.0004(6) C4 0.0118(8) 0.0114(8) 0.0207(8) 0.0003(6) 0.0058(6) 0.0017(6) C5 0.0100(7) 0.0121(8) 0.0186(8) -0.0001(6) 0.0058(6) -0.0020(6) C6 0.0086(7) 0.0140(8) 0.0141(7) -0.0014(6) 0.0033(6) 0.0017(6) C7 0.0073(7) 0.0167(8) 0.0178(8) 0.0000(6) 0.0042(6) 0.0025(6) C8 0.0094(7) 0.0192(9) 0.0221(8) 0.0093(7) 0.0029(6) 0.0011(6) C9 0.0095(8) 0.0148(8) 0.0244(9) 0.0051(7) 0.0036(6) 0.0035(6) C10 0.0072(7) 0.0153(8) 0.0130(7) -0.0004(6) 0.0021(6) 0.0004(6) C11 0.0092(7) 0.0144(8) 0.0151(7) -0.0021(6) 0.0016(6) -0.0014(6) C12 0.0107(7) 0.0139(8) 0.0146(7) -0.0035(6) 0.0020(6) 0.0007(6) C13 0.0109(7) 0.0143(8) 0.0173(8) -0.0008(6) 0.0036(6) 0.0009(6) C14 0.0126(8) 0.0145(8) 0.0174(8) -0.0017(6) 0.0044(6) 0.0031(6) C15 0.0097(7) 0.0152(8) 0.0115(7) 0.0017(6) 0.0031(6) 0.0020(6) C16 0.0133(8) 0.0116(8) 0.0160(8) 0.0006(6) 0.0056(6) -0.0002(6) C17 0.0126(8) 0.0143(8) 0.0152(8) 0.0013(6) 0.0049(6) 0.0039(6) C18 0.0110(7) 0.0148(8) 0.0144(7) 0.0010(6) 0.0040(6) -0.0008(6) C19 0.0090(7) 0.0165(8) 0.0173(8) -0.0008(6) 0.0032(6) -0.0009(6) C20 0.0099(7) 0.0181(8) 0.0159(8) -0.0066(6) -0.0002(6) 0.0015(6) C21 0.0100(7) 0.0133(8) 0.0187(8) -0.0043(6) 0.0010(6) -0.0014(6) C22 0.0079(7) 0.0157(8) 0.0115(7) -0.0009(6) 0.0005(6) 0.0012(6) C23 0.0104(7) 0.0156(8) 0.0204(8) 0.0028(6) 0.0032(6) 0.0037(6) C24 0.0116(8) 0.0185(9) 0.0205(8) 0.0074(7) 0.0023(6) 0.0000(6) N1 0.0080(6) 0.0153(7) 0.0109(6) -0.0007(5) 0.0028(5) 0.0004(5) N2 0.0065(6) 0.0197(7) 0.0144(6) 0.0018(5) 0.0023(5) 0.0015(5) N3 0.0100(6) 0.0159(7) 0.0116(6) 0.0012(5) 0.0034(5) 0.0021(5) N4 0.0076(6) 0.0220(7) 0.0128(6) -0.0015(5) 0.0019(5) 0.0003(5) O1 0.0133(6) 0.0126(5) 0.0093(5) -0.0008(4) 0.0020(4) 0.0004(4) O2 0.0133(6) 0.0142(6) 0.0130(5) 0.0031(4) 0.0069(4) 0.0039(4) O3 0.0137(6) 0.0147(6) 0.0144(6) -0.0016(4) 0.0008(5) -0.0044(4) O4 0.0084(5) 0.0117(5) 0.0125(5) -0.0004(4) 0.0003(4) 0.0010(4) O5 0.0096(5) 0.0124(6) 0.0178(6) -0.0004(4) 0.0043(4) 0.0028(4) O6 0.0109(5) 0.0139(6) 0.0107(5) 0.0026(4) -0.0007(4) -0.0030(4) O7 0.0105(5) 0.0122(6) 0.0211(6) 0.0027(5) 0.0017(5) 0.0034(4) O8 0.0093(5) 0.0101(5) 0.0125(5) 0.0002(4) -0.0008(4) -0.0004(4) O9 0.0104(5) 0.0125(6) 0.0197(6) 0.0004(5) 0.0032(5) -0.0030(4) O10 0.0187(6) 0.0127(6) 0.0208(6) -0.0018(5) 0.0136(5) -0.0005(5) O11 0.0130(6) 0.0148(6) 0.0120(5) -0.0015(4) -0.0004(4) 0.0040(4) O12 0.0166(6) 0.0127(6) 0.0100(5) 0.0001(4) -0.0008(4) 0.0000(4) V1 0.00659(12) 0.00802(12) 0.00781(12) -0.00024(9) 0.00202(9) -0.00017(9) V2 0.00556(12) 0.00850(12) 0.00804(12) 0.00065(9) 0.00187(9) 0.00097(9) V3 0.00615(12) 0.00807(12) 0.00847(12) -0.00034(9) 0.00244(9) -0.00024(9) V4 0.00635(12) 0.00831(12) 0.00807(12) 0.00065(9) 0.00190(9) 0.00083(9) Co1 0.00563(13) 0.00979(14) 0.00695(13) 0.00017(10) 0.00158(10) 0.00012(10) Co2 0.00715(14) 0.01058(15) 0.00725(13) 0.00019(11) 0.00132(11) 0.00169(11) #----------------------------------------------------------------------------# # 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 1.343(2) . ? C1 C2 1.378(2) . ? C1 H1 0.95 . ? C2 C3 1.398(2) . ? C2 H2 0.95 . ? C3 C4 1.399(2) . ? C3 C6 1.467(2) . ? C4 C5 1.386(2) . ? C4 H4 0.95 . ? C5 N1 1.337(2) . ? C5 H5 0.95 . ? C6 C7 1.344(2) . ? C6 H6 0.95 . ? C7 C10 1.464(2) . ? C7 H7 0.95 . ? C8 N2 1.337(2) . ? C8 C9 1.377(2) . ? C8 H8 0.95 . ? C9 C10 1.405(2) . ? C9 H9 0.95 . ? C10 C11 1.398(2) . ? C11 C12 1.376(2) . ? C11 H11 0.95 . ? C12 N2 1.348(2) . ? C12 H12 0.95 . ? C13 N3 1.344(2) . ? C13 C14 1.383(2) . ? C13 H13 0.95 . ? C14 C15 1.403(2) . ? C14 H14 0.95 . ? C15 C16 1.396(2) . ? C15 C18 1.465(2) . ? C16 C17 1.381(2) . ? C16 H16 0.95 . ? C17 N3 1.340(2) . ? C17 H17 0.95 . ? C18 C19 1.341(2) . ? C18 H18 0.95 . ? C19 C22 1.464(2) . ? C19 H19 0.95 . ? C20 N4 1.335(2) . ? C20 C21 1.376(2) . ? C20 H20 0.95 . ? C21 C22 1.395(2) . ? C21 H21 0.95 . ? C22 C23 1.409(2) . ? C23 C24 1.376(2) . ? C23 H23 0.95 . ? C24 N4 1.350(2) . ? C24 H24 0.95 . ? N1 Co1 2.1334(13) . ? N2 H2A 0.88 . ? N3 Co2 2.1333(13) . ? N4 H4A 0.88 . ? O1 V1 1.6626(11) . ? O1 Co1 2.0935(11) . ? O2 V2 1.7906(11) 2_557 ? O2 V1 1.7992(11) . ? O3 V1 1.6208(11) . ? O4 V2 1.8208(11) . ? O4 V1 1.8250(11) . ? O5 V2 1.6279(11) . ? O6 V2 1.6600(11) 2_556 ? O6 Co1 2.0650(10) . ? O7 V4 1.6226(11) . ? O8 V3 1.8201(11) . ? O8 V4 1.8243(11) . ? O9 V3 1.6272(11) . ? O10 V3 1.7850(11) . ? O10 V4 1.7914(11) 2_465 ? O11 V3 1.6555(12) . ? O11 Co2 2.0428(12) . ? O12 V4 1.6598(11) 2_466 ? O12 Co2 2.0897(11) . ? V2 O6 1.6600(11) 2_556 ? V2 O2 1.7906(11) 2_557 ? V4 O12 1.6598(11) 2_466 ? V4 O10 1.7914(11) 2_465 ? Co1 O6 2.0650(10) 2_556 ? Co1 O1 2.0935(11) 2_556 ? Co1 N1 2.1334(13) 2_556 ? Co2 O11 2.0428(12) 2_466 ? Co2 O12 2.0897(11) 2_466 ? Co2 N3 2.1333(13) 2_466 ? 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 C2 123.38(15) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.81(15) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 116.55(14) . . ? C2 C3 C6 123.31(14) . . ? C4 C3 C6 120.13(14) . . ? C5 C4 C3 119.83(15) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.10(14) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C7 C6 C3 123.77(15) . . ? C7 C6 H6 118.1 . . ? C3 C6 H6 118.1 . . ? C6 C7 C10 125.91(15) . . ? C6 C7 H7 117 . . ? C10 C7 H7 117 . . ? N2 C8 C9 119.77(15) . . ? N2 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 120.41(15) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 117.60(14) . . ? C11 C10 C7 124.53(14) . . ? C9 C10 C7 117.84(15) . . ? C12 C11 C10 119.99(15) . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? N2 C12 C11 120.13(15) . . ? N2 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? N3 C13 C14 123.63(16) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 118.93(15) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 117.27(14) . . ? C16 C15 C18 118.93(15) . . ? C14 C15 C18 123.79(15) . . ? C17 C16 C15 119.62(15) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N3 C17 C16 123.36(15) . . ? N3 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? C19 C18 C15 125.26(16) . . ? C19 C18 H18 117.4 . . ? C15 C18 H18 117.4 . . ? C18 C19 C22 124.40(16) . . ? C18 C19 H19 117.8 . . ? C22 C19 H19 117.8 . . ? N4 C20 C21 120.01(15) . . ? N4 C20 H20 120 . . ? C21 C20 H20 120 . . ? C20 C21 C22 120.13(15) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 118.01(14) . . ? C21 C22 C19 119.10(15) . . ? C23 C22 C19 122.82(15) . . ? C24 C23 C22 119.74(16) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? N4 C24 C23 119.74(15) . . ? N4 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C5 N1 C1 117.28(13) . . ? C5 N1 Co1 124.21(10) . . ? C1 N1 Co1 118.39(11) . . ? C8 N2 C12 122.09(14) . . ? C8 N2 H2A 119 . . ? C12 N2 H2A 119 . . ? C17 N3 C13 117.15(14) . . ? C17 N3 Co2 121.94(11) . . ? C13 N3 Co2 120.64(11) . . ? C20 N4 C24 122.37(14) . . ? C20 N4 H4A 118.8 . . ? C24 N4 H4A 118.8 . . ? V1 O1 Co1 127.50(6) . . ? V2 O2 V1 142.53(7) 2_557 . ? V2 O4 V1 122.18(6) . . ? V2 O6 Co1 139.51(6) 2_556 . ? V3 O8 V4 125.24(6) . . ? V3 O10 V4 148.83(7) . 2_465 ? V3 O11 Co2 138.76(7) . . ? V4 O12 Co2 133.81(7) 2_466 . ? O3 V1 O1 108.32(6) . . ? O3 V1 O2 111.15(6) . . ? O1 V1 O2 108.56(5) . . ? O3 V1 O4 105.94(6) . . ? O1 V1 O4 109.64(5) . . ? O2 V1 O4 113.12(5) . . ? O5 V2 O6 109.73(6) . 2_556 ? O5 V2 O2 110.46(5) . 2_557 ? O6 V2 O2 110.03(5) 2_556 2_557 ? O5 V2 O4 108.86(5) . . ? O6 V2 O4 106.11(5) 2_556 . ? O2 V2 O4 111.56(5) 2_557 . ? O9 V3 O11 109.32(6) . . ? O9 V3 O10 110.78(6) . . ? O11 V3 O10 108.89(6) . . ? O9 V3 O8 108.88(5) . . ? O11 V3 O8 107.19(5) . . ? O10 V3 O8 111.69(5) . . ? O7 V4 O12 108.82(6) . 2_466 ? O7 V4 O10 110.34(6) . 2_465 ? O12 V4 O10 108.91(6) 2_466 2_465 ? O7 V4 O8 107.16(6) . . ? O12 V4 O8 108.68(5) 2_466 . ? O10 V4 O8 112.85(5) 2_465 . ? O6 Co1 O6 180 2_556 . ? O6 Co1 O1 86.71(4) 2_556 2_556 ? O6 Co1 O1 93.29(4) . 2_556 ? O6 Co1 O1 93.29(4) 2_556 . ? O6 Co1 O1 86.71(4) . . ? O1 Co1 O1 180.00(4) 2_556 . ? O6 Co1 N1 90.04(5) 2_556 . ? O6 Co1 N1 89.96(5) . . ? O1 Co1 N1 86.53(5) 2_556 . ? O1 Co1 N1 93.47(5) . . ? O6 Co1 N1 89.96(5) 2_556 2_556 ? O6 Co1 N1 90.04(5) . 2_556 ? O1 Co1 N1 93.47(5) 2_556 2_556 ? O1 Co1 N1 86.53(5) . 2_556 ? N1 Co1 N1 180 . 2_556 ? O11 Co2 O11 180.00(4) . 2_466 ? O11 Co2 O12 85.76(4) . . ? O11 Co2 O12 94.24(4) 2_466 . ? O11 Co2 O12 94.24(4) . 2_466 ? O11 Co2 O12 85.76(4) 2_466 2_466 ? O12 Co2 O12 180.0000(10) . 2_466 ? O11 Co2 N3 88.50(5) . 2_466 ? O11 Co2 N3 91.50(5) 2_466 2_466 ? O12 Co2 N3 94.05(5) . 2_466 ? O12 Co2 N3 85.95(5) 2_466 2_466 ? O11 Co2 N3 91.50(5) . . ? O11 Co2 N3 88.50(5) 2_466 . ? O12 Co2 N3 85.95(5) . . ? O12 Co2 N3 94.05(5) 2_466 . ? N3 Co2 N3 180 2_466 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.9(3) . . . . ? C1 C2 C3 C4 -1.0(2) . . . . ? C1 C2 C3 C6 179.77(15) . . . . ? C2 C3 C4 C5 1.9(2) . . . . ? C6 C3 C4 C5 -178.90(15) . . . . ? C3 C4 C5 N1 -0.9(3) . . . . ? C2 C3 C6 C7 2.6(3) . . . . ? C4 C3 C6 C7 -176.53(16) . . . . ? C3 C6 C7 C10 176.76(15) . . . . ? N2 C8 C9 C10 -0.3(3) . . . . ? C8 C9 C10 C11 -0.5(3) . . . . ? C8 C9 C10 C7 177.56(16) . . . . ? C6 C7 C10 C11 -0.1(3) . . . . ? C6 C7 C10 C9 -178.05(17) . . . . ? C9 C10 C11 C12 1.4(2) . . . . ? C7 C10 C11 C12 -176.55(16) . . . . ? C10 C11 C12 N2 -1.5(2) . . . . ? N3 C13 C14 C15 -0.1(3) . . . . ? C13 C14 C15 C16 -1.5(2) . . . . ? C13 C14 C15 C18 179.69(15) . . . . ? C14 C15 C16 C17 1.6(2) . . . . ? C18 C15 C16 C17 -179.52(14) . . . . ? C15 C16 C17 N3 -0.1(2) . . . . ? C16 C15 C18 C19 174.01(16) . . . . ? C14 C15 C18 C19 -7.2(3) . . . . ? C15 C18 C19 C22 175.80(15) . . . . ? N4 C20 C21 C22 0.2(2) . . . . ? C20 C21 C22 C23 -0.6(2) . . . . ? C20 C21 C22 C19 176.44(15) . . . . ? C18 C19 C22 C21 167.57(16) . . . . ? C18 C19 C22 C23 -15.5(3) . . . . ? C21 C22 C23 C24 0.7(2) . . . . ? C19 C22 C23 C24 -176.27(16) . . . . ? C22 C23 C24 N4 -0.3(3) . . . . ? C4 C5 N1 C1 -1.0(2) . . . . ? C4 C5 N1 Co1 175.05(12) . . . . ? C2 C1 N1 C5 1.9(2) . . . . ? C2 C1 N1 Co1 -174.38(13) . . . . ? C9 C8 N2 C12 0.3(3) . . . . ? C11 C12 N2 C8 0.6(2) . . . . ? C16 C17 N3 C13 -1.5(2) . . . . ? C16 C17 N3 Co2 172.53(12) . . . . ? C14 C13 N3 C17 1.6(2) . . . . ? C14 C13 N3 Co2 -172.50(13) . . . . ? C21 C20 N4 C24 0.3(2) . . . . ? C23 C24 N4 C20 -0.2(3) . . . . ? Co1 O1 V1 O3 160.18(7) . . . . ? Co1 O1 V1 O2 -79.02(8) . . . . ? Co1 O1 V1 O4 45.01(9) . . . . ? V2 O2 V1 O3 -110.11(12) 2_557 . . . ? V2 O2 V1 O1 130.86(12) 2_557 . . . ? V2 O2 V1 O4 8.93(14) 2_557 . . . ? V2 O4 V1 O3 -170.49(6) . . . . ? V2 O4 V1 O1 -53.82(8) . . . . ? V2 O4 V1 O2 67.50(8) . . . . ? V1 O4 V2 O5 144.55(7) . . . . ? V1 O4 V2 O6 26.52(8) . . . 2_556 ? V1 O4 V2 O2 -93.30(7) . . . 2_557 ? Co2 O11 V3 O9 -131.84(9) . . . . ? Co2 O11 V3 O10 107.02(10) . . . . ? Co2 O11 V3 O8 -13.97(11) . . . . ? V4 O10 V3 O9 157.40(14) 2_465 . . . ? V4 O10 V3 O11 -82.35(16) 2_465 . . . ? V4 O10 V3 O8 35.83(17) 2_465 . . . ? V4 O8 V3 O9 154.78(7) . . . . ? V4 O8 V3 O11 36.63(8) . . . . ? V4 O8 V3 O10 -82.57(8) . . . . ? V3 O8 V4 O7 -159.87(7) . . . . ? V3 O8 V4 O12 -42.43(8) . . . 2_466 ? V3 O8 V4 O10 78.47(8) . . . 2_465 ? V2 O6 Co1 O1 21.56(10) 2_556 . . 2_556 ? V2 O6 Co1 O1 -158.44(10) 2_556 . . . ? V2 O6 Co1 N1 -64.95(10) 2_556 . . . ? V2 O6 Co1 N1 115.05(10) 2_556 . . 2_556 ? V1 O1 Co1 O6 166.06(8) . . . . ? V1 O1 Co1 N1 76.30(8) . . . . ? V1 O1 Co1 N1 -103.70(8) . . . 2_556 ? C5 N1 Co1 O6 141.21(13) . . . 2_556 ? C1 N1 Co1 O6 -42.82(12) . . . 2_556 ? C5 N1 Co1 O6 -38.79(13) . . . . ? C1 N1 Co1 O6 137.18(12) . . . . ? C5 N1 Co1 O1 -132.08(13) . . . 2_556 ? C1 N1 Co1 O1 43.88(12) . . . 2_556 ? C5 N1 Co1 O1 47.92(13) . . . . ? C1 N1 Co1 O1 -136.12(12) . . . . ? V3 O11 Co2 O12 -179.10(10) . . . . ? V3 O11 Co2 O12 0.90(10) . . . 2_466 ? V3 O11 Co2 N3 86.73(10) . . . 2_466 ? V3 O11 Co2 N3 -93.27(10) . . . . ? V4 O12 Co2 O11 -171.98(9) 2_466 . . . ? V4 O12 Co2 O11 8.02(9) 2_466 . . 2_466 ? V4 O12 Co2 N3 -83.79(9) 2_466 . . 2_466 ? V4 O12 Co2 N3 96.21(9) 2_466 . . . ? C17 N3 Co2 O11 156.34(12) . . . . ? C13 N3 Co2 O11 -29.85(12) . . . . ? C17 N3 Co2 O11 -23.66(12) . . . 2_466 ? C13 N3 Co2 O11 150.15(12) . . . 2_466 ? C17 N3 Co2 O12 -118.02(12) . . . . ? C13 N3 Co2 O12 55.80(12) . . . . ? C17 N3 Co2 O12 61.98(12) . . . 2_466 ? C13 N3 Co2 O12 -124.20(12) . . . 2_466 ? #-.....END data_CoHBpe293k _database_code_depnum_ccdc_archive 'CCDC 818191' #TrackingRef '- archive.cif' _audit_creation_date 2010-03-04T16:41:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H22 Co N4 O12 V4' _chemical_formula_sum 'C24 H22 Co N4 O12 V4' _chemical_formula_weight 821.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.4905(17) _cell_length_b 12.0219(9) _cell_length_c 7.8804(7) _cell_angle_alpha 88.690(8) _cell_angle_beta 95.030(9) _cell_angle_gamma 90.906(8) _cell_volume 1461.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7366 _cell_measurement_theta_min 3.0062 _cell_measurement_theta_max 32.3496 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.2828 _exptl_crystal_size_mid 0.1283 _exptl_crystal_size_min 0.0586 _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.857 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.907 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 8.3504 _diffrn_orient_matrix_ub_11 0.045296796 _diffrn_orient_matrix_ub_12 0.012568353 _diffrn_orient_matrix_ub_13 0.0039286482 _diffrn_orient_matrix_ub_21 0.009013878 _diffrn_orient_matrix_ub_22 -0.0573688407 _diffrn_orient_matrix_ub_23 -0.0110116774 _diffrn_orient_matrix_ub_31 -0.0031831776 _diffrn_orient_matrix_ub_32 0.0083673024 _diffrn_orient_matrix_ub_33 -0.0899759197 _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w and \p scans' _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_unetI/netI 0.072 _diffrn_reflns_number 32894 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.990 _reflns_number_total 5314 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.1501P)^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 5314 _refine_ls_number_parameters 410 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2157 _refine_ls_wR_factor_gt 0.1936 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.832 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.346 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.173 #----------------------------------------------------------------------------# # 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' 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' V V 0.3005 0.5294 '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' 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 N1 N -0.1277(6) 0.0269(10) 0.5743(11) 0.038(2) Uani 1 1 d . . . C1 C -0.1737(9) -0.0650(13) 0.6232(16) 0.054(4) Uani 1 1 d U . . H1 H -0.1476 -0.1342 0.6348 0.065 Uiso 1 1 calc R . . C2 C -0.2610(8) -0.0532(12) 0.6556(16) 0.050(3) Uani 1 1 d U . . H2 H -0.2934 -0.1158 0.6832 0.06 Uiso 1 1 calc R . . C3 C -0.2990(8) 0.0496(12) 0.6470(14) 0.044(3) Uani 1 1 d U . . C4 C -0.2496(9) 0.1402(13) 0.6012(16) 0.057(3) Uani 1 1 d U . . H4 H -0.2734 0.2109 0.5938 0.069 Uiso 1 1 calc R . . C5 C -0.1641(8) 0.1255(13) 0.5660(15) 0.049(3) Uani 1 1 d U . . H5 H -0.1316 0.1873 0.5357 0.059 Uiso 1 1 calc R . . C6 C -0.3909(7) 0.0672(12) 0.6823(14) 0.045(3) Uani 1 1 d U . . H6 H -0.4115 0.1396 0.6779 0.054 Uiso 1 1 calc R . . C7 C -0.4446(7) -0.0147(14) 0.7194(15) 0.051(3) Uani 1 1 d U . . H7 H -0.4245 -0.087 0.7156 0.062 Uiso 1 1 calc R . . N2 N -0.6979(7) 0.0141(11) 0.8605(11) 0.049(3) Uani 1 1 d . . . H2A H -0.7494 0.0191 0.8917 0.059 Uiso 1 1 calc R . . C8 C -0.6657(9) -0.0853(15) 0.8493(19) 0.065(4) Uani 1 1 d U . . H8 H -0.6987 -0.1485 0.8709 0.078 Uiso 1 1 calc R . . C9 C -0.5827(8) -0.0946(13) 0.8053(17) 0.057(3) Uani 1 1 d U . . H9 H -0.5584 -0.1646 0.8011 0.068 Uiso 1 1 calc R . . C10 C -0.5343(8) -0.0005(12) 0.7666(15) 0.044(3) Uani 1 1 d U . . C11 C -0.5727(8) 0.1018(12) 0.7745(16) 0.051(3) Uani 1 1 d U . . H11 H -0.5433 0.1665 0.7452 0.062 Uiso 1 1 calc R . . C12 C -0.6554(9) 0.1071(14) 0.8265(16) 0.054(3) Uani 1 1 d U . . H12 H -0.6811 0.1757 0.8375 0.065 Uiso 1 1 calc R . . N3 N -0.3721(6) 0.5155(11) 0.4223(11) 0.045(3) Uani 1 1 d . . . C13 C -0.3292(8) 0.4287(15) 0.3723(17) 0.061(4) Uani 1 1 d U . . H13 H -0.3594 0.3613 0.3638 0.073 Uiso 1 1 calc R . . C14 C -0.2449(8) 0.4289(14) 0.3321(17) 0.061(4) Uani 1 1 d U . . H14 H -0.2198 0.3649 0.2958 0.073 Uiso 1 1 calc R . . C15 C -0.1984(8) 0.5282(14) 0.3476(14) 0.054(3) Uani 1 1 d U . . C16 C -0.2425(8) 0.6204(14) 0.3946(15) 0.056(3) Uani 1 1 d U . . H16 H -0.2142 0.6891 0.403 0.067 Uiso 1 1 calc R . . C17 C -0.3285(9) 0.6107(13) 0.4291(15) 0.052(4) Uani 1 1 d U . . H17 H -0.3568 0.6743 0.4584 0.063 Uiso 1 1 calc R . . C18 C -0.1073(9) 0.5441(14) 0.3109(16) 0.063(4) Uani 1 1 d U . . H18 H -0.0843 0.6161 0.3128 0.076 Uiso 1 1 calc R . . C19 C -0.0566(8) 0.4625(16) 0.2756(16) 0.061(4) Uani 1 1 d U . . H19 H -0.0796 0.3906 0.2758 0.073 Uiso 1 1 calc R . . N4 N 0.1981(6) 0.4913(11) 0.1400(12) 0.050(3) Uani 1 1 d . . . H4A H 0.2504 0.4955 0.1115 0.059 Uiso 1 1 calc R . . C20 C 0.1642(8) 0.3898(15) 0.1692(17) 0.060(4) Uani 1 1 d U . . H20 H 0.196 0.326 0.1561 0.072 Uiso 1 1 calc R . . C21 C 0.0814(8) 0.3825(14) 0.2188(17) 0.063(4) Uani 1 1 d U . . H21 H 0.057 0.3131 0.2412 0.075 Uiso 1 1 calc R . . C22 C 0.0340(8) 0.4776(13) 0.2359(15) 0.051(3) Uani 1 1 d U . . C23 C 0.0716(9) 0.5795(15) 0.2009(16) 0.062(4) Uani 1 1 d U . . H23 H 0.0407 0.6446 0.2096 0.074 Uiso 1 1 calc R . . C24 C 0.1562(9) 0.5847(15) 0.1524(17) 0.063(4) Uani 1 1 d U . . H24 H 0.1823 0.6529 0.1292 0.076 Uiso 1 1 calc R . . O1 O 0.0541(5) 0.1316(8) 0.6457(8) 0.045(2) Uani 1 1 d . . . O2 O -0.0095(6) 0.1719(8) 0.9598(9) 0.049(2) Uani 1 1 d . . . O3 O 0.1597(5) 0.2305(8) 0.8854(10) 0.047(2) Uani 1 1 d . . . O4 O 0.1309(5) 0.0044(7) 0.9249(10) 0.043(2) Uani 1 1 d . . . O5 O 0.1537(5) -0.2204(8) 0.8661(10) 0.049(2) Uani 1 1 d . . . O6 O -0.0225(5) 0.1173(8) 0.3055(8) 0.045(2) Uani 1 1 d . . . O7 O -0.6637(5) 0.7151(8) 0.1048(11) 0.049(2) Uani 1 1 d . . . O8 O -0.6305(5) 0.4939(7) 0.0744(9) 0.036(2) Uani 1 1 d . . . O9 O -0.6525(5) 0.2657(8) 0.1390(10) 0.050(2) Uani 1 1 d . . . O10 O -0.5012(6) 0.3275(9) -0.0088(11) 0.061(3) Uani 1 1 d . . . O11 O -0.5279(5) 0.3762(9) 0.3278(9) 0.052(2) Uani 1 1 d . . . O12 O -0.4506(5) 0.3726(8) 0.6650(8) 0.043(2) Uani 1 1 d . . . V1 V 0.08313(11) 0.13717(18) 0.8536(2) 0.0305(5) Uani 1 1 d . . . V2 V 0.07891(11) -0.12954(18) 0.8800(2) 0.0300(5) Uani 1 1 d . . . V3 V -0.57856(11) 0.36177(18) 0.1343(2) 0.0318(5) Uani 1 1 d . . . V4 V -0.58517(11) 0.62941(19) 0.1319(2) 0.0326(5) Uani 1 1 d . . . Co1 Co 0 0 0.5 0.0337(6) Uani 1 2 d S . . Co2 Co -0.5 0.5 0.5 0.0338(6) Uani 1 2 d S . . 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 N1 0.032(5) 0.053(7) 0.031(5) 0.001(5) 0.010(4) -0.005(5) C1 0.037(6) 0.076(11) 0.052(7) 0.008(7) 0.019(6) 0.003(6) C2 0.037(6) 0.061(7) 0.054(7) -0.005(7) 0.015(6) -0.011(5) C3 0.027(5) 0.067(7) 0.040(6) -0.007(6) 0.013(5) -0.001(5) C4 0.043(6) 0.067(8) 0.066(8) -0.002(7) 0.027(6) -0.002(6) C5 0.039(6) 0.060(10) 0.052(7) -0.003(7) 0.023(6) -0.005(6) C6 0.025(5) 0.071(9) 0.039(6) 0.002(6) 0.008(5) 0.007(5) C7 0.019(5) 0.092(10) 0.043(6) 0.007(7) 0.006(5) 0.002(5) N2 0.031(6) 0.089(11) 0.028(5) -0.003(5) 0.005(5) 0.004(6) C8 0.035(6) 0.080(12) 0.079(9) 0.046(9) 0.012(7) -0.006(7) C9 0.027(5) 0.060(7) 0.082(9) 0.020(7) 0.000(6) 0.007(5) C10 0.025(5) 0.074(8) 0.034(6) 0.000(6) 0.007(5) -0.002(5) C11 0.024(5) 0.066(7) 0.065(7) -0.020(7) 0.007(5) -0.010(5) C12 0.031(6) 0.069(10) 0.062(7) -0.018(7) 0.001(5) 0.001(6) N3 0.020(5) 0.083(9) 0.031(5) 0.004(5) 0.003(4) 0.001(6) C13 0.023(6) 0.104(13) 0.058(8) -0.023(8) 0.011(6) 0.000(6) C14 0.030(6) 0.093(9) 0.064(8) -0.013(8) 0.025(6) 0.007(6) C15 0.024(5) 0.102(9) 0.035(6) -0.003(7) 0.004(5) 0.000(5) C16 0.029(5) 0.093(9) 0.047(6) 0.007(7) 0.007(5) -0.005(6) C17 0.042(6) 0.063(10) 0.054(7) 0.007(7) 0.021(6) 0.006(7) C18 0.033(6) 0.110(11) 0.049(7) 0.011(7) 0.019(6) 0.000(6) C19 0.023(5) 0.104(11) 0.057(8) -0.006(8) 0.006(6) -0.003(5) N4 0.014(5) 0.097(11) 0.039(6) -0.008(6) 0.006(4) 0.001(6) C20 0.024(5) 0.094(12) 0.063(8) -0.022(8) 0.001(5) -0.008(7) C21 0.028(6) 0.093(9) 0.069(8) -0.022(8) 0.008(6) -0.004(6) C22 0.025(5) 0.093(9) 0.034(6) -0.001(6) 0.005(5) -0.003(5) C23 0.036(6) 0.092(9) 0.057(7) 0.010(8) 0.009(6) 0.002(6) C24 0.035(6) 0.098(13) 0.055(7) 0.029(8) 0.005(6) -0.006(7) O1 0.041(5) 0.068(6) 0.026(4) 0.000(4) 0.008(3) 0.000(4) O2 0.039(5) 0.075(7) 0.036(4) 0.004(4) 0.019(3) 0.011(4) O3 0.035(5) 0.059(6) 0.046(4) -0.003(4) -0.003(4) -0.015(4) O4 0.016(4) 0.073(7) 0.038(4) -0.004(4) -0.001(3) 0.001(4) O5 0.016(4) 0.079(7) 0.052(5) 0.006(4) 0.011(3) 0.011(4) O6 0.037(4) 0.069(6) 0.025(4) 0.009(4) -0.008(3) -0.010(4) O7 0.026(4) 0.069(7) 0.051(5) 0.003(4) 0.002(4) 0.011(4) O8 0.028(4) 0.044(6) 0.034(4) 0.005(3) -0.003(3) 0.007(4) O9 0.027(4) 0.070(7) 0.052(5) 0.004(4) 0.005(4) -0.011(4) O10 0.051(5) 0.073(7) 0.067(5) -0.003(5) 0.048(5) 0.000(5) O11 0.042(5) 0.078(7) 0.036(4) -0.009(4) -0.005(4) 0.017(5) O12 0.044(5) 0.060(6) 0.024(4) -0.001(4) -0.002(3) -0.001(4) V1 0.0190(9) 0.0498(14) 0.0230(8) -0.0009(9) 0.0041(7) -0.0008(9) V2 0.0161(9) 0.0521(14) 0.0224(8) 0.0002(9) 0.0043(7) 0.0022(9) V3 0.0186(9) 0.0535(14) 0.0242(9) -0.0016(9) 0.0066(7) -0.0009(9) V4 0.0186(9) 0.0577(15) 0.0220(8) 0.0005(9) 0.0058(7) 0.0003(9) Co1 0.0169(11) 0.0658(19) 0.0186(10) 0.0013(10) 0.0039(9) -0.0020(10) Co2 0.0184(11) 0.0647(19) 0.0186(10) -0.0008(10) 0.0026(9) 0.0021(10) #----------------------------------------------------------------------------# # 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 N1 C5 1.319(17) . ? N1 C1 1.371(17) . ? N1 Co1 2.143(9) . ? C1 C2 1.408(18) . ? C2 C3 1.375(19) . ? C3 C4 1.381(18) . ? C3 C6 1.493(15) . ? C4 C5 1.391(18) . ? C6 C7 1.323(18) . ? C7 C10 1.483(16) . ? N2 C8 1.310(19) . ? N2 C12 1.322(18) . ? C8 C9 1.367(19) . ? C9 C10 1.390(18) . ? C10 C11 1.380(19) . ? C11 C12 1.382(18) . ? N3 C13 1.332(18) . ? N3 C17 1.319(18) . ? N3 Co2 2.129(9) . ? C13 C14 1.370(17) . ? C14 C15 1.39(2) . ? C15 C16 1.39(2) . ? C15 C18 1.474(17) . ? C16 C17 1.386(17) . ? C18 C19 1.32(2) . ? C19 C22 1.473(17) . ? N4 C24 1.32(2) . ? N4 C20 1.344(19) . ? C20 C21 1.375(18) . ? C21 C22 1.38(2) . ? C22 C23 1.38(2) . ? C23 C24 1.396(19) . ? O1 V1 1.663(7) . ? O1 Co1 2.096(9) . ? O2 V1 1.783(8) . ? O2 V2 1.789(7) 2_557 ? O3 V1 1.627(8) . ? O4 V2 1.817(9) . ? O4 V1 1.825(9) . ? O5 V2 1.617(8) . ? O6 V2 1.641(7) 2_556 ? O6 Co1 2.069(8) . ? O7 V4 1.602(9) . ? O8 V4 1.814(8) . ? O8 V3 1.826(8) . ? O9 V3 1.615(9) . ? O10 V3 1.775(8) . ? O10 V4 1.783(8) 2_465 ? O11 V3 1.664(8) . ? O11 Co2 2.053(9) . ? O12 V4 1.647(7) 2_466 ? O12 Co2 2.096(8) . ? V2 O6 1.641(7) 2_556 ? V2 O2 1.789(7) 2_557 ? V4 O12 1.647(7) 2_466 ? V4 O10 1.783(8) 2_465 ? Co1 O6 2.069(8) 2_556 ? Co1 O1 2.096(9) 2_556 ? Co1 N1 2.143(9) 2_556 ? Co2 O11 2.053(9) 2_466 ? Co2 O12 2.096(8) 2_466 ? Co2 N3 2.129(9) 2_466 ? 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 C5 N1 C1 119.9(11) . . ? C5 N1 Co1 122.9(8) . . ? C1 N1 Co1 117.1(9) . . ? N1 C1 C2 119.1(14) . . ? C3 C2 C1 120.9(13) . . ? C4 C3 C2 117.9(11) . . ? C4 C3 C6 118.9(13) . . ? C2 C3 C6 123.2(12) . . ? C3 C4 C5 119.8(14) . . ? N1 C5 C4 122.2(13) . . ? C7 C6 C3 123.5(13) . . ? C6 C7 C10 125.3(14) . . ? C8 N2 C12 123.7(12) . . ? N2 C8 C9 118.9(14) . . ? C8 C9 C10 120.7(14) . . ? C11 C10 C9 117.9(11) . . ? C11 C10 C7 123.4(12) . . ? C9 C10 C7 118.8(13) . . ? C10 C11 C12 119.3(13) . . ? N2 C12 C11 119.6(15) . . ? C13 N3 C17 115.6(11) . . ? C13 N3 Co2 122.2(10) . . ? C17 N3 Co2 122.1(9) . . ? N3 C13 C14 126.3(15) . . ? C13 C14 C15 117.6(14) . . ? C14 C15 C16 117.0(12) . . ? C14 C15 C18 125.2(14) . . ? C16 C15 C18 117.7(14) . . ? C17 C16 C15 120.3(15) . . ? N3 C17 C16 123.0(14) . . ? C19 C18 C15 123.8(16) . . ? C18 C19 C22 124.3(16) . . ? C24 N4 C20 124.0(12) . . ? N4 C20 C21 118.3(16) . . ? C20 C21 C22 120.6(15) . . ? C21 C22 C23 118.5(12) . . ? C21 C22 C19 117.2(14) . . ? C23 C22 C19 124.0(14) . . ? C22 C23 C24 119.8(15) . . ? N4 C24 C23 118.8(15) . . ? V1 O1 Co1 130.1(5) . . ? V1 O2 V2 145.3(6) . 2_557 ? V2 O4 V1 123.5(4) . . ? V2 O6 Co1 138.9(5) 2_556 . ? V4 O8 V3 124.4(4) . . ? V3 O10 V4 149.0(7) . 2_465 ? V3 O11 Co2 138.4(6) . . ? V4 O12 Co2 132.4(5) 2_466 . ? O3 V1 O1 108.8(4) . . ? O3 V1 O2 110.9(5) . . ? O1 V1 O2 108.6(4) . . ? O3 V1 O4 106.2(4) . . ? O1 V1 O4 108.6(4) . . ? O2 V1 O4 113.7(4) . . ? O5 V2 O6 108.8(4) . 2_556 ? O5 V2 O2 110.3(4) . 2_557 ? O6 V2 O2 110.0(4) 2_556 2_557 ? O5 V2 O4 108.3(4) . . ? O6 V2 O4 107.3(4) 2_556 . ? O2 V2 O4 112.0(4) 2_557 . ? O9 V3 O11 109.9(4) . . ? O9 V3 O10 110.7(5) . . ? O11 V3 O10 108.8(4) . . ? O9 V3 O8 108.8(4) . . ? O11 V3 O8 107.2(4) . . ? O10 V3 O8 111.5(4) . . ? O7 V4 O12 108.3(4) . 2_466 ? O7 V4 O10 110.5(5) . 2_465 ? O12 V4 O10 108.9(4) 2_466 2_465 ? O7 V4 O8 106.2(4) . . ? O12 V4 O8 109.5(4) 2_466 . ? O10 V4 O8 113.3(4) 2_465 . ? O6 Co1 O6 180.0(4) . 2_556 ? O6 Co1 O1 86.1(3) . . ? O6 Co1 O1 93.9(3) 2_556 . ? O6 Co1 O1 93.9(3) . 2_556 ? O6 Co1 O1 86.1(3) 2_556 2_556 ? O1 Co1 O1 180.0(3) . 2_556 ? O6 Co1 N1 90.7(4) . 2_556 ? O6 Co1 N1 89.3(4) 2_556 2_556 ? O1 Co1 N1 86.9(4) . 2_556 ? O1 Co1 N1 93.1(4) 2_556 2_556 ? O6 Co1 N1 89.3(4) . . ? O6 Co1 N1 90.7(4) 2_556 . ? O1 Co1 N1 93.1(4) . . ? O1 Co1 N1 86.9(4) 2_556 . ? N1 Co1 N1 180.00(16) 2_556 . ? O11 Co2 O11 180.0(4) 2_466 . ? O11 Co2 O12 94.4(3) 2_466 . ? O11 Co2 O12 85.6(3) . . ? O11 Co2 O12 85.6(3) 2_466 2_466 ? O11 Co2 O12 94.4(3) . 2_466 ? O12 Co2 O12 180.0000(10) . 2_466 ? O11 Co2 N3 89.6(4) 2_466 . ? O11 Co2 N3 90.4(4) . . ? O12 Co2 N3 85.9(4) . . ? O12 Co2 N3 94.1(4) 2_466 . ? O11 Co2 N3 90.4(4) 2_466 2_466 ? O11 Co2 N3 89.6(4) . 2_466 ? O12 Co2 N3 94.1(4) . 2_466 ? O12 Co2 N3 85.9(4) 2_466 2_466 ? N3 Co2 N3 180.00(15) . 2_466 ? #-.....END data_CoHbpe438K _database_code_depnum_ccdc_archive 'CCDC 818192' #TrackingRef '- archive.cif' _audit_creation_date 2010-03-08T11:47:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H22 Co N4 O12 V4' _chemical_formula_sum 'C24 H22 Co N4 O12 V4' _chemical_formula_weight 821.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'C -1' _symmetry_space_group_name_Hall '-C 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z' '-x, -y, -z' '-x+1/2, -y+1/2, -z' _cell_length_a 15.4955(7) _cell_length_b 12.1132(6) _cell_length_c 7.9099(7) _cell_angle_alpha 88.155(6) _cell_angle_beta 95.227(6) _cell_angle_gamma 90.875(4) _cell_volume 1477.63(16) _cell_formula_units_Z 2 _cell_measurement_temperature 438(2) _cell_measurement_reflns_used 2658 _cell_measurement_theta_min 2.9971 _cell_measurement_theta_max 28.4945 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.2828 _exptl_crystal_size_mid 0.1283 _exptl_crystal_size_min 0.0586 _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90054 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 438(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 8.3504 _diffrn_orient_matrix_ub_11 0.0356589397 _diffrn_orient_matrix_ub_12 0.0373016453 _diffrn_orient_matrix_ub_13 0.0003082825 _diffrn_orient_matrix_ub_21 -0.0288760403 _diffrn_orient_matrix_ub_22 0.0449715251 _diffrn_orient_matrix_ub_23 -0.0106869542 _diffrn_orient_matrix_ub_31 0.0005953389 _diffrn_orient_matrix_ub_32 0.003458697 _diffrn_orient_matrix_ub_33 0.0892980332 _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_number 6235 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.883 _reflns_number_total 3230 _reflns_number_gt 2143 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0940P)^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 3230 _refine_ls_number_parameters 319 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.789 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.147 #----------------------------------------------------------------------------# # 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' 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' V V 0.3005 0.5294 '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' 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 N1A N 0.3752(9) 0.0173(18) 0.591(3) 0.038(3) Uani 0.5 1 d PD A 1 C1A C 0.3232(15) -0.0689(17) 0.607(7) 0.065(7) Uani 0.5 1 d PDU A 1 H1A H 0.3446 -0.1386 0.5899 0.078 Uiso 0.5 1 calc PR A 1 C2A C 0.2384(11) -0.0613(13) 0.647(3) 0.060(5) Uani 0.5 1 d PDU A 1 H2A H 0.2063 -0.125 0.6687 0.072 Uiso 0.5 1 calc PR A 1 C3A C 0.2020(8) 0.0410(13) 0.655(2) 0.041(3) Uani 0.5 1 d PDU A 1 C4A C 0.2534(11) 0.1316(13) 0.622(3) 0.064(5) Uani 0.5 1 d PDU A 1 H4A H 0.2316 0.2025 0.625 0.076 Uiso 0.5 1 calc PR A 1 C5A C 0.3381(13) 0.1156(15) 0.585(4) 0.055(5) Uani 0.5 1 d PDU A 1 H5A H 0.3706 0.1771 0.5551 0.066 Uiso 0.5 1 calc PR A 1 N1B N 0.3680(9) -0.0036(18) 0.559(3) 0.038(3) Uani 0.5 1 d PD A 2 C1B C 0.3285(16) -0.0994(18) 0.585(7) 0.066(6) Uani 0.5 1 d PDU A 2 H1B H 0.3599 -0.1639 0.5813 0.08 Uiso 0.5 1 calc PR A 2 C2B C 0.2423(12) -0.1079(15) 0.619(3) 0.069(5) Uani 0.5 1 d PDU A 2 H2B H 0.2141 -0.1762 0.6159 0.082 Uiso 0.5 1 calc PR A 2 C3B C 0.1983(8) -0.0143(17) 0.656(2) 0.056(4) Uani 0.5 1 d PDU A 2 C4B C 0.2429(12) 0.0843(15) 0.651(3) 0.072(6) Uani 0.5 1 d PDU A 2 H4B H 0.2164 0.1499 0.674 0.086 Uiso 0.5 1 calc PR A 2 C5B C 0.3281(13) 0.0838(16) 0.612(5) 0.062(6) Uani 0.5 1 d PDU A 2 H5B H 0.3597 0.1495 0.6222 0.075 Uiso 0.5 1 calc PR A 2 C7A C 0.0544(6) -0.0232(10) 0.7216(15) 0.040(2) Uani 0.5 1 d PDU A 1 H7A H 0.073 -0.0953 0.7128 0.048 Uiso 0.5 1 calc PR A 1 C6A C 0.1122(6) 0.0558(9) 0.6939(13) 0.039(2) Uani 0.5 1 d PDU A 1 H6A H 0.0938 0.1282 0.6995 0.047 Uiso 0.5 1 calc PR A 1 C7B C 0.0558(9) 0.0451(14) 0.716(2) 0.066(4) Uani 0.5 1 d PDU A 2 H7B H 0.0748 0.1177 0.7008 0.079 Uiso 0.5 1 calc PR A 2 C6B C 0.1080(8) -0.0336(13) 0.6944(16) 0.065(3) Uani 0.5 1 d PDU A 2 H6B H 0.0878 -0.106 0.7037 0.078 Uiso 0.5 1 calc PR A 2 N2B N -0.198(3) 0.006(3) 0.858(12) 0.059(3) Uani 0.5 1 d PD A 2 H2B1 H -0.2524 0.0004 0.8676 0.071 Uiso 0.5 1 calc PR A 2 C8B C -0.1518(16) -0.085(2) 0.853(6) 0.056(6) Uani 0.5 1 d PDU A 2 H8B H -0.1747 -0.1536 0.883 0.067 Uiso 0.5 1 calc PR A 2 C9B C -0.0680(14) -0.0752(18) 0.803(5) 0.059(6) Uani 0.5 1 d PDU A 2 H9B H -0.0354 -0.1384 0.7952 0.071 Uiso 0.5 1 calc PR A 2 C10B C -0.0334(11) 0.025(2) 0.764(5) 0.038(5) Uani 0.5 1 d PDU A 2 C11B C -0.0796(16) 0.1156(19) 0.792(4) 0.053(6) Uani 0.5 1 d PDU A 2 H11B H -0.056 0.1854 0.772 0.063 Uiso 0.5 1 calc PR A 2 C12B C -0.1611(13) 0.106(2) 0.849(4) 0.059(7) Uani 0.5 1 d PDU A 2 H12B H -0.1896 0.1683 0.8812 0.071 Uiso 0.5 1 calc PR A 2 N2A N -0.198(3) 0.020(3) 0.862(13) 0.059(3) Uani 0.5 1 d PD A 1 H2A1 H -0.2433 0.0305 0.9133 0.071 Uiso 0.5 1 calc PR A 1 C8A C -0.1731(17) -0.083(3) 0.841(7) 0.069(8) Uani 0.5 1 d PDU A 1 H8A H -0.2102 -0.1425 0.8572 0.083 Uiso 0.5 1 calc PR A 1 C9A C -0.0894(16) -0.0981(19) 0.793(5) 0.059(6) Uani 0.5 1 d PDU A 1 H9A H -0.07 -0.1694 0.7807 0.071 Uiso 0.5 1 calc PR A 1 C10A C -0.0362(13) -0.011(2) 0.765(5) 0.046(6) Uani 0.5 1 d PDU A 1 C11A C -0.070(2) 0.0918(18) 0.765(4) 0.064(7) Uani 0.5 1 d PDU A 1 H11A H -0.0365 0.1526 0.7364 0.077 Uiso 0.5 1 calc PR A 1 C12A C -0.154(2) 0.108(2) 0.807(4) 0.069(9) Uani 0.5 1 d PDU A 1 H12A H -0.1786 0.1775 0.797 0.083 Uiso 0.5 1 calc PR A 1 O1 O 0.5338(3) -0.1220(3) 0.6830(4) 0.0588(10) Uani 1 1 d . A . O2 O 0.6552(2) 0.2299(3) 0.8717(5) 0.0617(10) Uani 1 1 d . . . O3 O 0.6580(2) -0.2177(3) 0.8837(5) 0.0592(10) Uani 1 1 d . . . O4 O 0.5052(3) -0.1701(3) 1.0206(5) 0.0698(12) Uani 1 1 d . . . O5 O 0.6294(2) 0.0054(3) 0.9231(4) 0.0445(8) Uani 1 1 d . . . O6 O 0.5417(2) 0.1286(3) 0.6568(4) 0.0545(9) Uani 1 1 d . A . V1 V 0.58134(4) -0.12888(6) 0.87600(9) 0.0328(2) Uani 1 1 d . . . V2 V 0.58032(5) 0.13610(6) 0.85741(9) 0.0332(2) Uani 1 1 d . . . Co1 Co 0.5 0 0.5 0.0351(2) Uani 1 2 d SD . . 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 N1A 0.028(3) 0.057(7) 0.030(9) -0.019(5) 0.002(4) -0.005(3) C1A 0.058(10) 0.051(11) 0.090(17) 0.019(12) 0.032(9) 0.022(9) C2A 0.043(8) 0.052(11) 0.088(12) -0.008(9) 0.023(8) -0.020(8) C3A 0.036(7) 0.035(8) 0.056(7) -0.007(7) 0.020(5) -0.011(6) C4A 0.045(7) 0.042(9) 0.108(13) -0.013(9) 0.030(7) -0.008(7) C5A 0.042(8) 0.048(10) 0.080(13) -0.015(10) 0.033(7) -0.016(7) N1B 0.028(3) 0.057(7) 0.030(9) -0.019(5) 0.002(4) -0.005(3) C1B 0.048(10) 0.062(12) 0.094(15) 0.014(15) 0.035(9) -0.004(8) C2B 0.052(8) 0.081(13) 0.075(10) -0.009(11) 0.019(7) -0.020(9) C3B 0.030(7) 0.071(12) 0.068(8) -0.001(10) 0.018(6) -0.008(8) C4B 0.053(11) 0.062(14) 0.108(13) -0.006(13) 0.040(10) 0.013(11) C5B 0.037(9) 0.057(12) 0.098(15) -0.010(11) 0.029(8) -0.012(8) C7A 0.017(5) 0.047(7) 0.057(6) 0.005(6) 0.008(4) 0.013(5) C6A 0.021(5) 0.047(7) 0.052(6) -0.011(5) 0.020(4) 0.002(4) C7B 0.046(8) 0.072(10) 0.080(9) -0.008(9) -0.001(7) 0.019(8) C6B 0.047(8) 0.093(11) 0.056(7) 0.006(7) 0.014(6) 0.010(7) N2B 0.025(2) 0.096(7) 0.058(5) 0.000(9) 0.006(2) 0.004(5) C8B 0.009(11) 0.070(10) 0.084(13) 0.037(8) -0.003(11) -0.003(7) C9B 0.018(11) 0.059(14) 0.098(12) -0.003(11) -0.003(10) -0.001(9) C10B 0.014(6) 0.052(14) 0.050(8) -0.007(11) 0.007(5) 0.001(6) C11B 0.032(9) 0.053(8) 0.076(14) -0.041(8) 0.012(8) -0.009(6) C12B 0.025(8) 0.098(15) 0.057(14) -0.042(10) 0.006(7) 0.003(8) N2A 0.025(2) 0.096(7) 0.058(5) 0.000(9) 0.006(2) 0.004(5) C8A 0.019(13) 0.098(14) 0.086(14) 0.037(10) -0.003(14) 0.008(9) C9A 0.022(11) 0.052(9) 0.099(13) 0.024(9) -0.001(10) -0.008(7) C10A 0.039(9) 0.051(14) 0.047(8) 0.000(12) 0.003(6) -0.001(8) C11A 0.047(11) 0.085(17) 0.065(11) -0.032(13) 0.025(8) -0.022(12) C12A 0.081(17) 0.065(12) 0.064(17) -0.013(9) 0.023(10) 0.001(10) O1 0.074(3) 0.053(2) 0.046(2) 0.0077(17) -0.0094(19) -0.0133(19) O2 0.046(2) 0.058(2) 0.080(3) -0.003(2) 0.003(2) -0.0178(18) O3 0.041(2) 0.058(2) 0.080(3) 0.000(2) 0.0119(19) 0.0162(17) O4 0.076(3) 0.059(2) 0.083(3) 0.005(2) 0.053(2) 0.008(2) O5 0.0416(18) 0.044(2) 0.0474(19) -0.0020(15) -0.0001(16) 0.0009(14) O6 0.067(2) 0.051(2) 0.0428(19) -0.0048(16) -0.0102(18) 0.0094(18) V1 0.0252(4) 0.0401(5) 0.0337(4) 0.0020(3) 0.0071(3) 0.0045(3) V2 0.0260(4) 0.0391(5) 0.0355(4) -0.0031(3) 0.0081(3) -0.0024(3) Co1 0.0257(4) 0.0518(6) 0.0280(4) -0.0007(4) 0.0045(3) 0.0011(4) #----------------------------------------------------------------------------# # 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 N1A C1A 1.319(13) . ? N1A C5A 1.329(16) . ? N1A Co1 2.139(10) . ? C1A C2A 1.385(15) . ? C2A C3A 1.376(17) . ? C3A C4A 1.378(16) . ? C3A C6A 1.465(13) . ? C4A C5A 1.388(15) . ? N1B C1B 1.323(14) . ? N1B C5B 1.329(15) . ? N1B Co1 2.140(10) . ? C1B C2B 1.386(15) . ? C2B C3B 1.385(18) . ? C3B C4B 1.370(18) . ? C3B C6B 1.475(14) . ? C4B C5B 1.385(14) . ? C7A C6A 1.328(12) . ? C7A C10A 1.486(14) . ? C7B C6B 1.284(13) . ? C7B C10B 1.481(14) . ? N2B C8B 1.325(16) . ? N2B C12B 1.335(18) . ? C8B C9B 1.396(15) . ? C9B C10B 1.355(16) . ? C10B C11B 1.356(16) . ? C11B C12B 1.383(16) . ? N2A C8A 1.328(17) . ? N2A C12A 1.337(19) . ? C8A C9A 1.400(16) . ? C9A C10A 1.354(16) . ? C10A C11A 1.360(16) . ? C11A C12A 1.384(16) . ? O1 V1 1.634(4) . ? O1 Co1 2.074(4) . ? O2 V2 1.610(3) . ? O3 V1 1.610(3) . ? O4 V2 1.770(4) 3_657 ? O4 V1 1.772(4) . ? O5 V2 1.808(3) . ? O5 V1 1.814(3) . ? O6 V2 1.649(3) . ? O6 Co1 2.081(3) . ? V2 O4 1.770(4) 3_657 ? Co1 O1 2.074(4) 3_656 ? Co1 O6 2.081(3) 3_656 ? Co1 N1A 2.139(10) 3_656 ? Co1 N1B 2.140(10) 3_656 ? 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 C1A N1A C5A 116.0(13) . . ? C1A N1A Co1 121.1(13) . . ? C5A N1A Co1 120.0(15) . . ? N1A C1A C2A 123.7(15) . . ? C3A C2A C1A 119.5(13) . . ? C2A C3A C4A 117.0(11) . . ? C2A C3A C6A 122.7(13) . . ? C4A C3A C6A 120.2(14) . . ? C3A C4A C5A 119.3(13) . . ? N1A C5A C4A 123.5(14) . . ? C1B N1B C5B 114.9(14) . . ? C1B N1B Co1 119.8(13) . . ? C5B N1B Co1 123.3(12) . . ? N1B C1B C2B 122.8(16) . . ? C3B C2B C1B 119.8(14) . . ? C4B C3B C2B 117.0(11) . . ? C4B C3B C6B 127.9(16) . . ? C2B C3B C6B 115.1(16) . . ? C3B C4B C5B 118.5(14) . . ? N1B C5B C4B 124.8(16) . . ? C6A C7A C10A 128.2(15) . . ? C7A C6A C3A 126.9(12) . . ? C6B C7B C10B 122.5(19) . . ? C7B C6B C3B 123.0(17) . . ? C8B N2B C12B 122(2) . . ? N2B C8B C9B 118.2(14) . . ? C10B C9B C8B 121.2(14) . . ? C9B C10B C11B 117.5(14) . . ? C9B C10B C7B 125.6(18) . . ? C11B C10B C7B 116.2(18) . . ? C10B C11B C12B 121.2(14) . . ? N2B C12B C11B 118.2(16) . . ? C8A N2A C12A 122(2) . . ? N2A C8A C9A 117.6(16) . . ? C10A C9A C8A 121.2(16) . . ? C9A C10A C11A 117.6(15) . . ? C9A C10A C7A 123(2) . . ? C11A C10A C7A 119(2) . . ? C10A C11A C12A 121.4(15) . . ? N2A C12A C11A 117.7(16) . . ? V1 O1 Co1 137.3(2) . . ? V2 O4 V1 149.4(3) 3_657 . ? V2 O5 V1 124.72(18) . . ? V2 O6 Co1 134.5(2) . . ? O3 V1 O1 108.8(2) . . ? O3 V1 O4 109.7(2) . . ? O1 V1 O4 109.9(2) . . ? O3 V1 O5 108.19(18) . . ? O1 V1 O5 107.97(17) . . ? O4 V1 O5 112.20(17) . . ? O2 V2 O6 108.7(2) . . ? O2 V2 O4 110.4(2) . 3_657 ? O6 V2 O4 108.7(2) . 3_657 ? O2 V2 O5 107.86(18) . . ? O6 V2 O5 108.21(17) . . ? O4 V2 O5 112.87(17) 3_657 . ? O1 Co1 O1 180.00(15) 3_656 . ? O1 Co1 O6 93.94(14) 3_656 3_656 ? O1 Co1 O6 86.06(14) . 3_656 ? O1 Co1 O6 86.06(14) 3_656 . ? O1 Co1 O6 93.94(14) . . ? O6 Co1 O6 180.0000(10) 3_656 . ? O1 Co1 N1A 91.7(8) 3_656 3_656 ? O1 Co1 N1A 88.3(8) . 3_656 ? O6 Co1 N1A 87.0(5) 3_656 3_656 ? O6 Co1 N1A 93.0(5) . 3_656 ? O1 Co1 N1A 88.3(8) 3_656 . ? O1 Co1 N1A 91.7(8) . . ? O6 Co1 N1A 93.0(5) 3_656 . ? O6 Co1 N1A 87.0(5) . . ? N1A Co1 N1A 180.0(2) 3_656 . ? O1 Co1 N1B 91.9(8) 3_656 3_656 ? O1 Co1 N1B 88.1(8) . 3_656 ? O6 Co1 N1B 96.9(5) 3_656 3_656 ? O6 Co1 N1B 83.1(5) . 3_656 ? N1A Co1 N1B 9.9(10) 3_656 3_656 ? N1A Co1 N1B 170.1(10) . 3_656 ? O1 Co1 N1B 88.1(8) 3_656 . ? O1 Co1 N1B 91.9(8) . . ? O6 Co1 N1B 83.1(5) 3_656 . ? O6 Co1 N1B 96.9(5) . . ? N1A Co1 N1B 170.1(10) 3_656 . ? N1A Co1 N1B 9.9(10) . . ? N1B Co1 N1B 180.00(16) 3_656 . ? #-.....END data_CoHBpe503K _database_code_depnum_ccdc_archive 'CCDC 818193' #TrackingRef '- archive.cif' _audit_creation_date 2010-04-21T11:55:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H22 Co N4 O12 V4' _chemical_formula_sum 'C24 H22 Co N4 O12 V4' _chemical_formula_weight 821.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'C -1' _symmetry_space_group_name_Hall '-C 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, z' '-x, -y, -z' '-x+1/2, -y+1/2, -z' _cell_length_a 15.456(3) _cell_length_b 12.141(3) _cell_length_c 7.915(5) _cell_angle_alpha 89.727(18) _cell_angle_beta 95.358(18) _cell_angle_gamma 90.177(17) _cell_volume 1478.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 503(2) _cell_measurement_reflns_used 2285 _cell_measurement_theta_min 3.0065 _cell_measurement_theta_max 32.5723 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.4753 _exptl_crystal_size_mid 0.1641 _exptl_crystal_size_min 0.1191 _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.835 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.628 _exptl_absorpt_correction_T_max 0.827 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 503(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 8.3504 _diffrn_orient_matrix_ub_11 0.0334596788 _diffrn_orient_matrix_ub_12 -0.0397383845 _diffrn_orient_matrix_ub_13 0.0176648526 _diffrn_orient_matrix_ub_21 0.0307515422 _diffrn_orient_matrix_ub_22 0.0431208049 _diffrn_orient_matrix_ub_23 0.0155025494 _diffrn_orient_matrix_ub_31 -0.0079015592 _diffrn_orient_matrix_ub_32 0.0005287249 _diffrn_orient_matrix_ub_33 0.0873041224 _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_unetI/netI 0.0753 _diffrn_reflns_number 9295 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 32.45 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.903 _reflns_number_total 4801 _reflns_number_gt 2488 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0628P)^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 4801 _refine_ls_number_parameters 319 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.609 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.090 #----------------------------------------------------------------------------# # 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' 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' V V 0.3005 0.5294 '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' 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 N1A N 0.3694(8) 0.0142(14) 0.562(3) 0.049(3) Uani 0.50 1 d PD A 1 C1A C 0.3235(11) -0.0749(14) 0.592(4) 0.086(6) Uani 0.50 1 d PDU A 1 H1A H 0.3468 -0.1436 0.5713 0.103 Uiso 0.50 1 calc PR A 1 C2A C 0.2417(9) -0.0701(12) 0.653(2) 0.072(4) Uani 0.50 1 d PDU A 1 H2A H 0.2153 -0.1332 0.6912 0.086 Uiso 0.50 1 calc PR A 1 C3A C 0.2014(7) 0.0303(13) 0.655(2) 0.057(3) Uani 0.50 1 d PDU A 1 C4A C 0.2494(10) 0.1219(11) 0.624(3) 0.077(4) Uani 0.50 1 d PDU A 1 H4A H 0.2245 0.1915 0.6227 0.092 Uiso 0.50 1 calc PR A 1 C5A C 0.3351(10) 0.1089(13) 0.594(4) 0.067(4) Uani 0.50 1 d PDU A 1 H5A H 0.3705 0.1710 0.5980 0.080 Uiso 0.50 1 calc PR A 1 N1B N 0.3738(8) -0.0107(14) 0.590(3) 0.049(3) Uani 0.50 1 d PD A 2 C1B C 0.3346(10) -0.1077(13) 0.601(3) 0.067(4) Uani 0.50 1 d PDU A 2 H1B H 0.3676 -0.1713 0.5957 0.081 Uiso 0.50 1 calc PR A 2 C2B C 0.2462(9) -0.1183(12) 0.619(2) 0.073(4) Uani 0.50 1 d PDU A 2 H2B H 0.2192 -0.1866 0.6061 0.087 Uiso 0.50 1 calc PR A 2 C3B C 0.1994(7) -0.0277(14) 0.656(2) 0.059(4) Uani 0.50 1 d PDU A 2 C4B C 0.2396(9) 0.0733(12) 0.646(3) 0.071(4) Uani 0.50 1 d PDU A 2 H4B H 0.2112 0.1379 0.6701 0.085 Uiso 0.50 1 calc PR A 2 C5B C 0.3232(11) 0.0753(13) 0.599(4) 0.082(6) Uani 0.50 1 d PDU A 2 H5B H 0.3458 0.1436 0.5725 0.098 Uiso 0.50 1 calc PR A 2 C7A C 0.0543(6) -0.0303(10) 0.7217(16) 0.061(3) Uani 0.50 1 d PDU A 1 H7A H 0.0688 -0.1040 0.7099 0.073 Uiso 0.50 1 calc PR A 1 C6A C 0.1102(5) 0.0458(9) 0.6929(13) 0.068(3) Uani 0.50 1 d PDU A 1 H6A H 0.0908 0.1182 0.6961 0.082 Uiso 0.50 1 calc PR A 1 C7B C 0.0552(7) 0.0364(11) 0.7204(17) 0.065(3) Uani 0.50 1 d PDU A 2 H7B H 0.0711 0.1101 0.7143 0.078 Uiso 0.50 1 calc PR A 2 C6B C 0.1088(5) -0.0425(10) 0.6942(12) 0.066(2) Uani 0.50 1 d PDU A 2 H6B H 0.0882 -0.1143 0.6999 0.079 Uiso 0.50 1 calc PR A 2 N2B N -0.2010(12) -0.0101(19) 0.842(2) 0.060(3) Uani 0.50 1 d PD A 2 H2B1 H -0.2567 -0.0129 0.8262 0.072 Uiso 0.50 1 calc PR A 2 C8B C -0.1521(14) -0.1025(19) 0.847(5) 0.096(8) Uani 0.50 1 d PDU A 2 H8B H -0.1703 -0.1675 0.8951 0.116 Uiso 0.50 1 calc PR A 2 C9B C -0.0751(15) -0.096(2) 0.776(5) 0.092(8) Uani 0.50 1 d PDU A 2 H9B H -0.0501 -0.1599 0.7382 0.111 Uiso 0.50 1 calc PR A 2 C10B C -0.0344(10) 0.002(2) 0.761(4) 0.066(7) Uani 0.50 1 d PDU A 2 C11B C -0.0766(14) 0.0957(19) 0.812(3) 0.076(6) Uani 0.50 1 d PDU A 2 H11B H -0.0495 0.1641 0.8109 0.091 Uiso 0.50 1 calc PR A 2 C12B C -0.1584(14) 0.0865(17) 0.865(2) 0.073(6) Uani 0.50 1 d PDU A 2 H12B H -0.1839 0.1458 0.9155 0.087 Uiso 0.50 1 calc PR A 2 N2A N -0.1952(11) 0.0110(18) 0.878(3) 0.060(3) Uani 0.50 1 d PD A 1 H2A1 H -0.2352 0.0155 0.9461 0.072 Uiso 0.50 1 calc PR A 1 C8A C -0.1660(13) -0.0881(15) 0.834(4) 0.069(5) Uani 0.50 1 d PDU A 1 H8A H -0.2020 -0.1497 0.8223 0.082 Uiso 0.50 1 calc PR A 1 C9A C -0.0803(16) -0.0924(17) 0.806(5) 0.080(7) Uani 0.50 1 d PDU A 1 H9A H -0.0527 -0.1604 0.8095 0.096 Uiso 0.50 1 calc PR A 1 C10A C -0.0342(12) -0.001(2) 0.774(5) 0.081(8) Uani 0.50 1 d PDU A 1 C11A C -0.0792(14) 0.099(2) 0.762(3) 0.083(7) Uani 0.50 1 d PDU A 1 H11A H -0.0539 0.1618 0.7204 0.099 Uiso 0.50 1 calc PR A 1 C12A C -0.1614(12) 0.1031(18) 0.814(2) 0.070(5) Uani 0.50 1 d PDU A 1 H12A H -0.1932 0.1681 0.8052 0.084 Uiso 0.50 1 calc PR A 1 O1 O 0.53699(19) -0.1247(3) 0.6712(3) 0.0672(8) Uani 1 1 d . A . O2 O 0.65634(17) 0.2240(3) 0.8777(4) 0.0732(9) Uani 1 1 d . . . O3 O 0.65646(17) -0.2230(3) 0.8787(4) 0.0713(8) Uani 1 1 d . . . O4 O 0.5001(2) -0.1700(3) 1.0011(4) 0.0840(10) Uani 1 1 d . . . O5 O 0.62960(15) 0.0005(2) 0.9216(3) 0.0556(7) Uani 1 1 d . . . O6 O 0.53738(19) 0.1252(3) 0.6691(3) 0.0664(8) Uani 1 1 d . A . V1 V 0.58073(3) -0.13196(5) 0.86699(7) 0.04279(18) Uani 1 1 d . . . V2 V 0.58062(3) 0.13300(5) 0.86577(7) 0.04266(18) Uani 1 1 d . . . Co1 Co 0.5000 0.0000 0.5000 0.0446(2) Uani 1 2 d SD . . 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 N1A 0.0355(19) 0.068(7) 0.043(7) 0.019(5) 0.009(3) 0.005(3) C1A 0.051(7) 0.066(11) 0.145(12) 0.051(10) 0.031(7) 0.025(7) C2A 0.048(6) 0.086(11) 0.086(9) -0.013(8) 0.032(6) -0.026(8) C3A 0.039(5) 0.079(10) 0.054(5) -0.005(8) 0.017(4) -0.011(6) C4A 0.055(6) 0.066(9) 0.114(11) -0.011(10) 0.034(6) -0.007(7) C5A 0.036(5) 0.062(9) 0.105(9) -0.018(9) 0.021(6) -0.011(6) N1B 0.0355(19) 0.068(7) 0.043(7) 0.019(5) 0.009(3) 0.005(3) C1B 0.047(7) 0.059(9) 0.100(9) 0.025(8) 0.030(7) 0.008(6) C2B 0.060(6) 0.078(10) 0.083(9) -0.008(8) 0.024(6) -0.014(7) C3B 0.037(5) 0.089(10) 0.054(5) 0.009(8) 0.015(4) -0.007(7) C4B 0.046(7) 0.070(11) 0.102(9) 0.002(10) 0.035(6) 0.008(8) C5B 0.053(7) 0.063(10) 0.137(12) -0.039(11) 0.042(7) -0.024(7) C7A 0.030(4) 0.082(8) 0.074(6) -0.001(7) 0.019(4) -0.004(5) C6A 0.035(4) 0.078(8) 0.094(7) -0.009(6) 0.020(4) -0.003(5) C7B 0.036(5) 0.086(8) 0.074(6) -0.002(8) 0.008(4) -0.005(6) C6B 0.038(5) 0.088(8) 0.073(5) 0.010(6) 0.012(4) -0.004(5) N2B 0.029(2) 0.118(9) 0.034(8) -0.029(5) 0.001(4) -0.011(4) C8B 0.052(11) 0.137(16) 0.101(12) 0.067(10) 0.015(10) 0.028(9) C9B 0.043(9) 0.145(18) 0.090(14) 0.005(11) 0.017(8) 0.028(10) C10B 0.021(8) 0.137(17) 0.042(7) 0.005(10) 0.008(6) -0.001(11) C11B 0.056(8) 0.107(13) 0.066(12) -0.036(8) 0.010(7) -0.028(8) C12B 0.061(8) 0.103(14) 0.053(10) -0.032(9) -0.007(7) 0.012(9) N2A 0.029(2) 0.118(9) 0.034(8) -0.029(5) 0.001(4) -0.011(4) C8A 0.033(6) 0.071(10) 0.099(12) 0.017(9) -0.010(7) 0.000(7) C9A 0.074(14) 0.076(11) 0.092(13) 0.035(9) 0.013(9) 0.020(9) C10A 0.045(13) 0.116(16) 0.081(15) -0.019(13) 0.000(10) 0.003(13) C11A 0.062(9) 0.119(13) 0.070(14) -0.015(9) 0.015(8) -0.036(9) C12A 0.042(7) 0.112(11) 0.055(10) 0.009(7) 0.004(6) -0.003(6) O1 0.0724(18) 0.076(2) 0.0500(14) 0.0105(14) -0.0125(14) -0.0105(16) O2 0.0483(15) 0.079(2) 0.091(2) -0.0071(17) 0.0028(15) -0.0192(15) O3 0.0476(15) 0.074(2) 0.093(2) 0.0049(17) 0.0070(15) 0.0147(14) O4 0.087(2) 0.079(2) 0.097(2) 0.0004(18) 0.0648(18) 0.0008(17) O5 0.0418(13) 0.0623(18) 0.0609(15) -0.0011(13) -0.0049(12) -0.0020(12) O6 0.0753(19) 0.070(2) 0.0508(14) -0.0078(13) -0.0106(14) 0.0087(15) V1 0.0300(3) 0.0590(4) 0.0404(3) 0.0032(3) 0.0085(2) 0.0030(2) V2 0.0306(3) 0.0580(4) 0.0404(3) -0.0044(3) 0.0090(2) -0.0042(2) Co1 0.0299(3) 0.0716(5) 0.0325(3) -0.0002(3) 0.0051(2) -0.0005(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 N1A C5A 1.305(13) . ? N1A C1A 1.324(12) . ? N1A Co1 2.128(9) . ? C1A C2A 1.398(13) . ? C2A C3A 1.371(15) . ? C3A C4A 1.369(15) . ? C3A C6A 1.480(11) . ? C4A C5A 1.376(12) . ? N1B C5B 1.314(13) . ? N1B C1B 1.330(12) . ? N1B Co1 2.140(9) . ? C1B C2B 1.392(13) . ? C2B C3B 1.367(15) . ? C3B C4B 1.378(15) . ? C3B C6B 1.469(11) . ? C4B C5B 1.377(12) . ? C7A C6A 1.298(11) . ? C7A C10A 1.510(14) . ? C7B C6B 1.298(11) . ? C7B C10B 1.508(13) . ? N2B C12B 1.349(13) . ? N2B C8B 1.352(14) . ? C8B C9B 1.362(15) . ? C9B C10B 1.357(13) . ? C10B C11B 1.392(15) . ? C11B C12B 1.371(13) . ? N2A C8A 1.345(13) . ? N2A C12A 1.349(14) . ? C8A C9A 1.363(14) . ? C9A C10A 1.358(13) . ? C10A C11A 1.396(15) . ? C11A C12A 1.371(13) . ? O1 V1 1.634(3) . ? O1 Co1 2.073(3) . ? O2 V2 1.604(3) . ? O3 V1 1.609(3) . ? O4 V2 1.768(3) 3_657 ? O4 V1 1.769(3) . ? O5 V1 1.812(3) . ? O5 V2 1.815(3) . ? O6 V2 1.639(3) . ? O6 Co1 2.075(3) . ? V2 O4 1.768(3) 3_657 ? Co1 O1 2.073(3) 3_656 ? Co1 O6 2.075(3) 3_656 ? Co1 N1A 2.128(9) 3_656 ? Co1 N1B 2.140(9) 3_656 ? 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 C5A N1A C1A 116.7(11) . . ? C5A N1A Co1 122.2(11) . . ? C1A N1A Co1 120.5(10) . . ? N1A C1A C2A 122.8(13) . . ? C3A C2A C1A 118.2(11) . . ? C4A C3A C2A 117.6(9) . . ? C4A C3A C6A 118.2(13) . . ? C2A C3A C6A 124.2(12) . . ? C3A C4A C5A 118.8(12) . . ? N1A C5A C4A 123.6(13) . . ? C5B N1B C1B 115.0(10) . . ? C5B N1B Co1 122.8(11) . . ? C1B N1B Co1 120.4(11) . . ? N1B C1B C2B 122.9(12) . . ? C3B C2B C1B 119.7(12) . . ? C2B C3B C4B 117.0(9) . . ? C2B C3B C6B 118.9(13) . . ? C4B C3B C6B 124.1(13) . . ? C5B C4B C3B 117.9(11) . . ? N1B C5B C4B 125.7(13) . . ? C6A C7A C10A 120.7(15) . . ? C7A C6A C3A 127.2(12) . . ? C6B C7B C10B 116.5(15) . . ? C7B C6B C3B 125.4(13) . . ? C12B N2B C8B 117.1(16) . . ? N2B C8B C9B 117.0(16) . . ? C10B C9B C8B 120.8(16) . . ? C9B C10B C11B 117.3(12) . . ? C9B C10B C7B 134.4(18) . . ? C11B C10B C7B 107.7(18) . . ? C12B C11B C10B 119.7(13) . . ? N2B C12B C11B 118.6(13) . . ? C8A N2A C12A 119.5(15) . . ? N2A C8A C9A 115.7(13) . . ? C10A C9A C8A 122.1(13) . . ? C9A C10A C11A 117.1(13) . . ? C9A C10A C7A 110.9(18) . . ? C11A C10A C7A 130.7(19) . . ? C12A C11A C10A 119.1(14) . . ? N2A C12A C11A 118.7(14) . . ? V1 O1 Co1 136.19(18) . . ? V2 O4 V1 150.1(2) 3_657 . ? V1 O5 V2 125.00(13) . . ? V2 O6 Co1 136.23(18) . . ? O3 V1 O1 108.91(16) . . ? O3 V1 O4 109.76(16) . . ? O1 V1 O4 109.25(16) . . ? O3 V1 O5 108.25(14) . . ? O1 V1 O5 107.90(14) . . ? O4 V1 O5 112.69(14) . . ? O2 V2 O6 109.19(16) . . ? O2 V2 O4 109.80(16) . 3_657 ? O6 V2 O4 109.52(16) . 3_657 ? O2 V2 O5 108.00(14) . . ? O6 V2 O5 107.51(14) . . ? O4 V2 O5 112.75(14) 3_657 . ? O1 Co1 O1 180.0 . 3_656 ? O1 Co1 O6 86.00(12) . 3_656 ? O1 Co1 O6 94.00(12) 3_656 3_656 ? O1 Co1 O6 94.00(12) . . ? O1 Co1 O6 86.00(12) 3_656 . ? O6 Co1 O6 180.0 3_656 . ? O1 Co1 N1A 83.0(5) . 3_656 ? O1 Co1 N1A 97.0(5) 3_656 3_656 ? O6 Co1 N1A 90.2(7) 3_656 3_656 ? O6 Co1 N1A 89.8(7) . 3_656 ? O1 Co1 N1A 97.0(5) . . ? O1 Co1 N1A 83.0(5) 3_656 . ? O6 Co1 N1A 89.8(7) 3_656 . ? O6 Co1 N1A 90.2(7) . . ? N1A Co1 N1A 180.000(1) 3_656 . ? O1 Co1 N1B 93.1(5) . 3_656 ? O1 Co1 N1B 86.9(5) 3_656 3_656 ? O6 Co1 N1B 92.0(7) 3_656 3_656 ? O6 Co1 N1B 88.0(7) . 3_656 ? N1A Co1 N1B 10.1(8) 3_656 3_656 ? N1A Co1 N1B 169.9(8) . 3_656 ? O1 Co1 N1B 86.9(5) . . ? O1 Co1 N1B 93.1(5) 3_656 . ? O6 Co1 N1B 88.0(7) 3_656 . ? O6 Co1 N1B 92.0(7) . . ? N1A Co1 N1B 169.9(8) 3_656 . ? N1A Co1 N1B 10.1(8) . . ? N1B Co1 N1B 180.0(2) 3_656 . ? #-.....END data_CoHBpe533K _database_code_depnum_ccdc_archive 'CCDC 818194' #TrackingRef '- archive.cif' _audit_creation_date 2010-04-22T10:10:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H5.50 Co0.25 N O3 V' _chemical_formula_sum 'C6 H5.50 Co0.25 N O3 V' _chemical_formula_weight 205.29 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_oxdiff_length_a 15.404(5) _cell_oxdiff_length_b 12.082(4) _cell_oxdiff_length_c 7.885(2) _cell_oxdiff_angle_alpha 90.11(2) _cell_oxdiff_angle_beta 85.05(2) _cell_oxdiff_angle_gamma 90.31(2) _cell_oxdiff_volume 1461.9(8) _cell_length_a 15.404(5) _cell_length_b 12.082(4) _cell_length_c 7.885(2) _cell_angle_alpha 90 _cell_angle_beta 94.95(2) _cell_angle_gamma 90 _cell_volume 1462.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 533(2) _cell_measurement_reflns_used 279 _cell_measurement_theta_min 3.2722 _cell_measurement_theta_max 28.39 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.2828 _exptl_crystal_size_mid 0.1283 _exptl_crystal_size_min 0.0586 _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.85477 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 533(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 8.3504 _diffrn_orient_matrix_ub_11 0.0362831258 _diffrn_orient_matrix_ub_12 -0.0359880599 _diffrn_orient_matrix_ub_13 -0.0010417424 _diffrn_orient_matrix_ub_21 -0.0285889773 _diffrn_orient_matrix_ub_22 -0.0461605312 _diffrn_orient_matrix_ub_23 0.0099284599 _diffrn_orient_matrix_ub_31 0.0005257056 _diffrn_orient_matrix_ub_32 -0.0046892681 _diffrn_orient_matrix_ub_33 -0.0898046041 _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.111 _diffrn_reflns_av_unetI/netI 0.1663 _diffrn_reflns_number 1087 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.651 _diffrn_measured_fraction_theta_max 0.628 _reflns_number_total 988 _reflns_number_gt 381 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET) (compiled May 29 2009,17:40:42) ; _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0581P)^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 988 _refine_ls_number_parameters 96 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.485 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # 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' 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' V V 0.3005 0.5294 '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 0 0 0.0492(11) Uani 1 4 d SD . . V2 V 0.08058(10) 0.13203(16) 0.3654(3) 0.0475(7) Uani 1 1 d . . . O3 O 0.0378(4) 0.1253(6) 0.1658(9) 0.065(2) Uani 1 1 d . . . O4 O 0.1284(5) 0 0.4239(14) 0.055(3) Uani 1 2 d S . . O6 O 0.1552(4) 0.2219(6) 0.3773(12) 0.075(3) Uani 1 1 d . . . O8 O 0 0.1718(10) 0.5 0.094(5) Uani 1 2 d S . . N1 N 0.1299(7) 0 -0.0815(19) 0.065(4) Uani 1 2 d SD . . C1A C 0.1614(11) -0.1011(15) -0.098(5) 0.066(3) Uani 0.5 1 d PD A 1 H1A H 0.1252 -0.1624 -0.0943 0.079 Uiso 0.5 1 calc PR A 1 C1B C 0.1833(11) 0.0855(16) -0.089(4) 0.066(3) Uani 0.5 1 d PD A 2 H1B H 0.166 0.1564 -0.0606 0.079 Uiso 0.5 1 calc PR A 2 C2A C 0.2480(11) -0.114(2) -0.122(4) 0.066(3) Uani 0.5 1 d PD . . H2A H 0.2697 -0.1861 -0.1171 0.079 Uiso 0.5 1 calc PR A 1 C2B C 0.2651(10) 0.066(2) -0.141(4) 0.066(3) Uani 0.5 1 d PD . . H2B H 0.2961 0.1283 -0.1715 0.079 Uiso 0.5 1 calc PR A 2 C3 C 0.3052(11) 0.0319(19) -0.153(3) 0.066(3) Uani 0.5 1 d P . . C4 C 0.3888(10) -0.0434(16) -0.189(3) 0.066(3) Uani 0.5 1 d P . . H4 H 0.4093 -0.1156 -0.1939 0.079 Uiso 0.5 1 calc PR . . C5 C 0.4442(10) 0.0345(18) -0.216(3) 0.066(3) Uani 0.5 1 d P . . H5 H 0.4301 0.1087 -0.2035 0.079 Uiso 0.5 1 calc PR . . C6 C 0.5340(9) 0 -0.271(3) 0.066(3) Uani 1 2 d S . . C7A C 0.5865(16) 0.111(3) -0.286(4) 0.066(3) Uani 0.5 1 d P . . H7A H 0.564 0.1803 -0.2645 0.079 Uiso 0.5 1 calc PR . . C7B C 0.5687(13) 0.073(3) -0.299(5) 0.066(3) Uani 0.5 1 d P . . H7B H 0.5374 0.1385 -0.2939 0.079 Uiso 0.5 1 calc PR . . C8A C 0.6498(17) 0.098(3) -0.324(6) 0.066(3) Uani 0.5 1 d P . . H8A H 0.6809 0.1629 -0.3365 0.079 Uiso 0.5 1 calc PR . . C8B C 0.6714(16) 0.087(3) -0.351(6) 0.066(3) Uani 0.5 1 d P . . H8B H 0.7011 0.1528 -0.3679 0.079 Uiso 0.5 1 calc PR . . N2 N 0.6968(8) 0 -0.360(2) 0.072(5) Uani 1 2 d S . . H2 H 0.7487 0.0081 -0.3904 0.087 Uiso 0.5 1 calc PR . . 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 0.0319(14) 0.094(3) 0.021(3) 0 0.0009(16) 0 V2 0.0303(9) 0.0801(15) 0.0321(18) -0.0055(11) 0.0025(9) -0.0048(10) O3 0.079(5) 0.104(6) 0.011(7) -0.005(4) -0.007(4) 0.003(5) O4 0.043(5) 0.080(8) 0.041(10) 0 -0.006(5) 0 O6 0.045(4) 0.080(6) 0.099(9) 0.000(5) 0.002(5) -0.025(4) O8 0.079(7) 0.119(11) 0.091(15) 0 0.039(8) 0 N1 0.038(7) 0.083(11) 0.069(14) 0 -0.016(7) 0 C1A 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C1B 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C2A 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C2B 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C3 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C4 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C5 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C6 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C7A 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C7B 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C8A 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) C8B 0.025(4) 0.103(7) 0.071(7) 0.010(5) 0.008(4) 0.005(4) N2 0.037(8) 0.129(15) 0.051(15) 0 0.009(8) 0 #----------------------------------------------------------------------------# # 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 O3 2.051(7) . ? Co1 O3 2.051(7) 5 ? Co1 O3 2.051(7) 6 ? Co1 O3 2.051(7) 2 ? Co1 N1 2.154(12) 5 ? Co1 N1 2.154(12) . ? Co1 N1 2.154(12) 6 ? V2 O6 1.578(6) . ? V2 O3 1.655(7) . ? V2 O8 1.768(4) . ? V2 O4 1.800(4) . ? O4 V2 1.800(4) 6 ? O8 V2 1.768(4) 2_556 ? N1 C1A 1.325(16) . ? N1 C1B 1.325(16) . ? C1A C2A 1.372(16) . ? C1B C2B 1.379(17) . ? C2A C3 1.36(3) 6 ? C2B C3 1.345(15) 6 ? C3 C3 0.77(5) 6 ? C3 C2B 1.345(15) 6 ? C3 C2A 1.36(3) 6 ? C3 C4 1.35(2) 6 ? C4 C5 1.30(2) . ? C4 C3 1.35(2) 6 ? C5 C6 1.54(2) . ? C6 C7B 1.06(2) 6 ? C6 C5 1.54(2) 6 ? C6 C7A 1.57(2) . ? C6 C7A 1.57(2) 6 ? C7A C8A 1.06(3) . ? C7B C6 1.06(2) 6 ? C7B C8B 1.68(4) . ? C8A N2 1.43(3) . ? C8B N2 1.13(4) 6 ? N2 C8B 1.13(4) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O3 180.0(4) . 5 ? O3 Co1 O3 95.1(4) . 6 ? O3 Co1 O3 84.9(4) 5 6 ? O3 Co1 O3 84.9(4) . 2 ? O3 Co1 O3 95.1(4) 5 2 ? O3 Co1 O3 180.0(5) 6 2 ? O3 Co1 N1 91.7(3) . 5 ? O3 Co1 N1 88.3(3) 5 5 ? O3 Co1 N1 91.7(3) 6 5 ? O3 Co1 N1 88.3(3) 2 5 ? O3 Co1 N1 88.3(3) . . ? O3 Co1 N1 91.7(3) 5 . ? O3 Co1 N1 88.3(3) 6 . ? O3 Co1 N1 91.7(3) 2 . ? N1 Co1 N1 180.0(8) 5 . ? O3 Co1 N1 88.3(3) . 6 ? O3 Co1 N1 91.7(3) 5 6 ? O3 Co1 N1 88.3(3) 6 6 ? O3 Co1 N1 91.7(3) 2 6 ? N1 Co1 N1 180.0(8) 5 6 ? N1 Co1 N1 0.0(8) . 6 ? O6 V2 O3 108.6(4) . . ? O6 V2 O8 108.9(4) . . ? O3 V2 O8 110.0(2) . . ? O6 V2 O4 108.3(3) . . ? O3 V2 O4 108.7(4) . . ? O8 V2 O4 112.3(5) . . ? V2 O3 Co1 135.3(4) . . ? V2 O4 V2 124.8(5) 6 . ? V2 O8 V2 148.5(7) . 2_556 ? C1A N1 C1B 118.7(14) . . ? C1A N1 Co1 112.8(11) . . ? C1B N1 Co1 127.6(10) . . ? N1 C1A C2A 119(2) . . ? N1 C1B C2B 118(2) . . ? C3 C2A C1A 126(2) 6 . ? C3 C2B C1B 127(2) 6 . ? C3 C2B C4 54.0(10) 6 6 ? C1B C2B C4 173(3) . 6 ? C3 C3 C2A 136.8(13) 6 6 ? C2B C3 C2A 108.9(16) 6 6 ? C3 C3 C4 95.9(13) 6 6 ? C2B C3 C4 123.9(18) 6 6 ? C2A C3 C4 127(2) 6 6 ? C5 C4 C3 127.7(19) . 6 ? C5 C4 C2B 141.6(15) . 6 ? C4 C5 C6 117.9(15) . . ? C7B C6 C5 108.2(19) 6 6 ? C7B C6 C5 140(2) 6 . ? C7B C6 C7A 114.7(18) 6 . ? C5 C6 C7A 137.0(15) 6 . ? C5 C6 C7A 105.7(15) . . ? C5 C6 C7A 105.7(15) 6 6 ? C5 C6 C7A 137.0(15) . 6 ? C7A C6 C7A 116(2) . 6 ? C8A C7A C6 113(3) . . ? C6 C7B C8B 130(3) 6 . ? C7A C8A N2 132(4) . . ? N2 C8B C7B 105(3) 6 . ? C8B N2 C8A 125.2(17) 6 . ? #-.....END