# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Lentz, Dieter' 'Mujkic, Monika' _publ_contact_author_name 'Lentz, Dieter' _publ_contact_author_email lentz@chemie.fu-berlin.de _publ_section_title ; Syntheses of Highly Unsaturated Isocyanides via Organometallic Pathways ; # Attachment '- ZZ-8.CIF' data_2crco _database_code_depnum_ccdc_archive 'CCDC 179717' #TrackingRef '- ZZ-8.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mue2-eta2-eta2[(mue-eta1-eta1-Z,Z-2,3,5,6-tetrafluoro1,6-diisocyano- hexa-1,5-dien-3-in)-bis(pentacarbonylchromium)]dicobalt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 Co2 Cr2 F4 N2 O16' _chemical_formula_weight 870.12 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0587(6) _cell_length_b 12.0685(7) _cell_length_c 13.6716(8) _cell_angle_alpha 107.4920(10) _cell_angle_beta 93.9400(10) _cell_angle_gamma 103.9440(10) _cell_volume 1518.29(15) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6367 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 33.1 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.472 _exptl_absorpt_correction_T_max 0.628 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER-AXS, CCD SMART 1000' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21046 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 33.29 _reflns_number_total 10576 _reflns_number_gt 8946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10576 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.179620(17) 0.272214(15) 0.027915(12) 0.02417(4) Uani 1 1 d . . . Co2 Co 0.155758(18) 0.447235(15) 0.169262(13) 0.02501(4) Uani 1 1 d . . . Cr3 Cr 0.471434(19) 0.003573(17) 0.257524(15) 0.02441(5) Uani 1 1 d . . . Cr4 Cr 0.161405(19) 0.282385(16) 0.551267(14) 0.02358(5) Uani 1 1 d . . . C1 C 0.08042(12) 0.10564(10) 0.22718(9) 0.0252(2) Uani 1 1 d . . . C2 C 0.04739(11) 0.19536(11) 0.20117(9) 0.0240(2) Uani 1 1 d . . . C3 C 0.13727(11) 0.28417(10) 0.16925(9) 0.02224(19) Uani 1 1 d . . . C4 C 0.27329(12) 0.33720(10) 0.16975(8) 0.02185(19) Uani 1 1 d . . . C5 C 0.40730(11) 0.36485(10) 0.22813(9) 0.0229(2) Uani 1 1 d . . . C6 C 0.43178(11) 0.36728(10) 0.32633(9) 0.0238(2) Uani 1 1 d . . . C11 C 0.29410(16) 0.34688(13) -0.04706(11) 0.0356(3) Uani 1 1 d . . . C12 C 0.21517(17) 0.12647(14) -0.01117(11) 0.0372(3) Uani 1 1 d . . . C13 C 0.00550(15) 0.23204(13) -0.04389(10) 0.0343(3) Uani 1 1 d . . . C21 C 0.26497(17) 0.56398(13) 0.12706(11) 0.0360(3) Uani 1 1 d . . . C22 C 0.18403(15) 0.52905(12) 0.30768(11) 0.0319(3) Uani 1 1 d . . . C23 C -0.02341(17) 0.45080(15) 0.13616(12) 0.0423(3) Uani 1 1 d . . . C31 C 0.30874(12) 0.05712(10) 0.23984(9) 0.0247(2) Uani 1 1 d . . . C32 C 0.50674(15) 0.09819(13) 0.40135(11) 0.0364(3) Uani 1 1 d . . . C33 C 0.35427(13) -0.12596(12) 0.29011(10) 0.0300(2) Uani 1 1 d . . . C34 C 0.43827(15) -0.08720(13) 0.11230(11) 0.0346(3) Uani 1 1 d . . . C35 C 0.58634(13) 0.13843(12) 0.22781(11) 0.0304(2) Uani 1 1 d . . . C36 C 0.62596(14) -0.05900(13) 0.27314(12) 0.0342(3) Uani 1 1 d . . . C41 C 0.26268(12) 0.31839(10) 0.44452(9) 0.0243(2) Uani 1 1 d . . . C42 C 0.16688(14) 0.11826(12) 0.49980(10) 0.0316(3) Uani 1 1 d . . . C43 C 0.33966(14) 0.32516(11) 0.63241(10) 0.0293(2) Uani 1 1 d . . . C44 C 0.14631(14) 0.44505(12) 0.59843(11) 0.0327(3) Uani 1 1 d . . . C45 C -0.01855(14) 0.23547(12) 0.46938(10) 0.0323(3) Uani 1 1 d . . . C46 C 0.07967(14) 0.25319(13) 0.66590(10) 0.0331(3) Uani 1 1 d . . . F1 F -0.01535(8) 0.02224(7) 0.24964(7) 0.03923(19) Uani 1 1 d . . . F2 F -0.08561(7) 0.19747(8) 0.19827(7) 0.03744(18) Uani 1 1 d . . . F3 F 0.51685(8) 0.39941(7) 0.18263(6) 0.03200(16) Uani 1 1 d . . . F4 F 0.56065(8) 0.40274(8) 0.37859(6) 0.03626(18) Uani 1 1 d . . . N2 N 0.33080(10) 0.34030(9) 0.38283(8) 0.02555(19) Uani 1 1 d . . . N1 N 0.20869(11) 0.08871(9) 0.22963(8) 0.02645(19) Uani 1 1 d . . . O11 O 0.36370(15) 0.39218(12) -0.09277(10) 0.0585(3) Uani 1 1 d . . . O12 O 0.23649(17) 0.03538(12) -0.03218(11) 0.0643(4) Uani 1 1 d . . . O13 O -0.10510(12) 0.20804(13) -0.08270(9) 0.0528(3) Uani 1 1 d . . . O21 O 0.33517(15) 0.63243(10) 0.09930(10) 0.0534(3) Uani 1 1 d . . . O22 O 0.20451(14) 0.57733(10) 0.39409(9) 0.0479(3) Uani 1 1 d . . . O23 O -0.13317(15) 0.45232(15) 0.11664(12) 0.0719(4) Uani 1 1 d . . . O32 O 0.52490(15) 0.15409(13) 0.48648(9) 0.0605(4) Uani 1 1 d . . . O33 O 0.28255(12) -0.20183(10) 0.31014(9) 0.0429(2) Uani 1 1 d . . . O34 O 0.42160(15) -0.13990(12) 0.02648(9) 0.0546(3) Uani 1 1 d . . . O35 O 0.65241(11) 0.21877(10) 0.21060(10) 0.0422(2) Uani 1 1 d . . . O36 O 0.71562(12) -0.09952(11) 0.27961(11) 0.0512(3) Uani 1 1 d . . . O42 O 0.16939(13) 0.02036(10) 0.46809(10) 0.0484(3) Uani 1 1 d . . . O43 O 0.44725(11) 0.34869(10) 0.67835(8) 0.0419(2) Uani 1 1 d . . . O44 O 0.13229(13) 0.53954(10) 0.62463(11) 0.0507(3) Uani 1 1 d . . . O45 O -0.12634(11) 0.20636(11) 0.42255(9) 0.0474(3) Uani 1 1 d . . . O46 O 0.03429(13) 0.23828(13) 0.73641(9) 0.0524(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02513(8) 0.02614(8) 0.02100(7) 0.00777(6) 0.00357(6) 0.00653(6) Co2 0.02881(8) 0.02331(8) 0.02569(8) 0.00950(6) 0.00397(6) 0.01040(6) Cr3 0.02109(9) 0.02456(9) 0.02787(9) 0.00853(7) 0.00220(7) 0.00732(7) Cr4 0.02353(9) 0.02302(9) 0.02347(9) 0.00862(7) 0.00594(7) 0.00318(7) C1 0.0191(5) 0.0237(5) 0.0312(5) 0.0101(4) 0.0045(4) 0.0014(4) C2 0.0167(4) 0.0264(5) 0.0288(5) 0.0088(4) 0.0041(4) 0.0055(4) C3 0.0215(5) 0.0232(5) 0.0232(5) 0.0081(4) 0.0036(4) 0.0079(4) C4 0.0225(5) 0.0217(5) 0.0229(5) 0.0087(4) 0.0053(4) 0.0067(4) C5 0.0196(5) 0.0224(5) 0.0272(5) 0.0103(4) 0.0070(4) 0.0035(4) C6 0.0180(4) 0.0239(5) 0.0274(5) 0.0092(4) 0.0012(4) 0.0017(4) C11 0.0387(7) 0.0389(7) 0.0289(6) 0.0112(5) 0.0091(5) 0.0092(6) C12 0.0459(8) 0.0353(7) 0.0283(6) 0.0060(5) 0.0042(5) 0.0133(6) C13 0.0331(6) 0.0417(7) 0.0243(5) 0.0083(5) 0.0031(5) 0.0069(5) C21 0.0495(8) 0.0289(6) 0.0338(6) 0.0122(5) 0.0093(6) 0.0151(6) C22 0.0374(7) 0.0274(6) 0.0350(6) 0.0118(5) 0.0094(5) 0.0133(5) C23 0.0452(8) 0.0440(8) 0.0408(7) 0.0097(6) 0.0003(6) 0.0250(7) C31 0.0246(5) 0.0208(5) 0.0278(5) 0.0085(4) 0.0036(4) 0.0041(4) C32 0.0318(6) 0.0384(7) 0.0363(7) 0.0083(6) 0.0009(5) 0.0109(5) C33 0.0290(6) 0.0286(6) 0.0328(6) 0.0096(5) 0.0028(5) 0.0097(5) C34 0.0341(6) 0.0332(6) 0.0375(7) 0.0121(5) 0.0070(5) 0.0101(5) C35 0.0219(5) 0.0321(6) 0.0395(6) 0.0119(5) 0.0054(5) 0.0109(5) C36 0.0289(6) 0.0338(6) 0.0442(7) 0.0181(6) 0.0066(5) 0.0096(5) C41 0.0241(5) 0.0220(5) 0.0245(5) 0.0070(4) 0.0008(4) 0.0035(4) C42 0.0316(6) 0.0309(6) 0.0320(6) 0.0127(5) 0.0067(5) 0.0047(5) C43 0.0325(6) 0.0269(6) 0.0263(5) 0.0079(4) 0.0072(4) 0.0045(5) C44 0.0273(6) 0.0309(6) 0.0378(6) 0.0100(5) 0.0091(5) 0.0049(5) C45 0.0319(6) 0.0312(6) 0.0326(6) 0.0101(5) 0.0080(5) 0.0062(5) C46 0.0297(6) 0.0377(7) 0.0325(6) 0.0140(5) 0.0079(5) 0.0066(5) F1 0.0294(4) 0.0332(4) 0.0583(5) 0.0250(4) 0.0121(4) 0.0003(3) F2 0.0170(3) 0.0450(5) 0.0564(5) 0.0226(4) 0.0088(3) 0.0110(3) F3 0.0225(3) 0.0399(4) 0.0374(4) 0.0198(3) 0.0129(3) 0.0040(3) F4 0.0203(3) 0.0462(5) 0.0374(4) 0.0154(4) -0.0044(3) 0.0004(3) N2 0.0256(5) 0.0249(5) 0.0248(4) 0.0090(4) 0.0032(4) 0.0036(4) N1 0.0241(5) 0.0234(5) 0.0312(5) 0.0091(4) 0.0022(4) 0.0058(4) O11 0.0628(8) 0.0626(8) 0.0540(7) 0.0274(6) 0.0293(6) 0.0083(6) O12 0.0925(11) 0.0429(7) 0.0571(8) 0.0044(6) 0.0041(7) 0.0352(7) O13 0.0313(5) 0.0780(9) 0.0400(6) 0.0129(6) -0.0016(4) 0.0083(5) O21 0.0745(9) 0.0355(6) 0.0550(7) 0.0224(5) 0.0229(6) 0.0105(6) O22 0.0670(8) 0.0413(6) 0.0327(5) 0.0064(4) 0.0105(5) 0.0165(5) O23 0.0517(8) 0.0904(11) 0.0754(10) 0.0146(8) -0.0069(7) 0.0432(8) O32 0.0650(9) 0.0683(9) 0.0349(6) -0.0011(6) -0.0027(6) 0.0197(7) O33 0.0445(6) 0.0358(5) 0.0493(6) 0.0188(5) 0.0097(5) 0.0056(4) O34 0.0722(9) 0.0513(7) 0.0338(6) 0.0070(5) 0.0112(5) 0.0128(6) O35 0.0299(5) 0.0392(5) 0.0643(7) 0.0240(5) 0.0136(5) 0.0111(4) O36 0.0346(5) 0.0558(7) 0.0827(9) 0.0404(7) 0.0154(6) 0.0234(5) O42 0.0578(7) 0.0295(5) 0.0564(7) 0.0109(5) 0.0125(6) 0.0121(5) O43 0.0337(5) 0.0442(6) 0.0397(5) 0.0076(5) -0.0033(4) 0.0064(4) O44 0.0461(6) 0.0314(5) 0.0709(8) 0.0088(5) 0.0168(6) 0.0117(5) O45 0.0329(5) 0.0541(7) 0.0491(6) 0.0125(5) -0.0028(5) 0.0091(5) O46 0.0491(7) 0.0747(9) 0.0419(6) 0.0306(6) 0.0207(5) 0.0140(6) _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 C12 1.8087(15) . ? Co1 C13 1.8261(14) . ? Co1 C11 1.8456(14) . ? Co1 C4 1.9343(11) . y Co1 C3 1.9777(11) . y Co1 Co2 2.4714(3) . ? Co2 C22 1.8178(14) . ? Co2 C21 1.8316(15) . ? Co2 C23 1.8416(15) . ? Co2 C3 1.9315(11) . y Co2 C4 1.9804(11) . y Cr3 C33 1.9064(13) . ? Cr3 C36 1.9102(14) . ? Cr3 C32 1.9119(15) . ? Cr3 C34 1.9180(14) . ? Cr3 C31 1.9244(12) . ? Cr3 C35 1.9249(13) . ? Cr4 C46 1.9042(13) . ? Cr4 C42 1.9082(14) . ? Cr4 C43 1.9100(13) . ? Cr4 C44 1.9206(14) . ? Cr4 C45 1.9227(14) . ? Cr4 C41 1.9310(12) . ? C1 F1 1.3396(13) . ? C1 C2 1.3408(17) . ? C1 N1 1.3538(15) . ? C2 F2 1.3423(13) . ? C2 C3 1.4231(16) . ? C3 C4 1.3622(15) . ? C4 C5 1.4286(15) . ? C5 C6 1.3383(16) . ? C5 F3 1.3430(12) . ? C6 F4 1.3400(12) . ? C6 N2 1.3543(15) . ? C11 O11 1.1227(18) . ? C12 O12 1.1265(19) . ? C13 O13 1.1289(17) . ? C21 O21 1.1266(18) . ? C22 O22 1.1281(17) . ? C23 O23 1.124(2) . ? C31 N1 1.1727(16) . ? C32 O32 1.1325(18) . ? C33 O33 1.1373(17) . ? C34 O34 1.1323(18) . ? C35 O35 1.1336(17) . ? C36 O36 1.1349(17) . ? C41 N2 1.1733(16) . ? C42 O42 1.1370(17) . ? C43 O43 1.1392(16) . ? C44 O44 1.1347(18) . ? C45 O45 1.1378(17) . ? C46 O46 1.1380(17) . ? 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 C12 Co1 C13 100.23(7) . . ? C12 Co1 C11 99.39(7) . . ? C13 Co1 C11 104.81(6) . . ? C12 Co1 C4 100.02(6) . . ? C13 Co1 C4 139.40(5) . . ? C11 Co1 C4 106.08(6) . . ? C12 Co1 C3 100.47(6) . . ? C13 Co1 C3 100.88(5) . . ? C11 Co1 C3 143.94(6) . . ? C4 Co1 C3 40.74(5) . . ? C12 Co1 Co2 148.53(5) . . ? C13 Co1 Co2 96.57(5) . . ? C11 Co1 Co2 101.77(5) . . ? C4 Co1 Co2 51.69(3) . . ? C3 Co1 Co2 49.96(3) . . ? C22 Co2 C21 98.78(6) . . ? C22 Co2 C23 99.41(7) . . ? C21 Co2 C23 105.40(7) . . ? C22 Co2 C3 101.06(5) . . ? C21 Co2 C3 140.80(6) . . ? C23 Co2 C3 104.25(6) . . ? C22 Co2 C4 98.84(5) . . ? C21 Co2 C4 102.95(6) . . ? C23 Co2 C4 143.27(6) . . ? C3 Co2 C4 40.73(5) . . ? C22 Co2 Co1 147.88(4) . . ? C21 Co2 Co1 96.50(4) . . ? C23 Co2 Co1 103.51(5) . . ? C3 Co2 Co1 51.62(3) . . ? C4 Co2 Co1 50.03(3) . . ? C33 Cr3 C36 90.22(6) . . ? C33 Cr3 C32 89.22(6) . . ? C36 Cr3 C32 91.50(6) . . ? C33 Cr3 C34 92.39(6) . . ? C36 Cr3 C34 88.89(6) . . ? C32 Cr3 C34 178.34(6) . . ? C33 Cr3 C31 86.75(5) . . ? C36 Cr3 C31 176.63(5) . . ? C32 Cr3 C31 89.93(6) . . ? C34 Cr3 C31 89.76(6) . . ? C33 Cr3 C35 177.85(6) . . ? C36 Cr3 C35 91.38(6) . . ? C32 Cr3 C35 89.31(6) . . ? C34 Cr3 C35 89.07(6) . . ? C31 Cr3 C35 91.68(5) . . ? C46 Cr4 C42 90.39(6) . . ? C46 Cr4 C43 88.72(6) . . ? C42 Cr4 C43 90.05(6) . . ? C46 Cr4 C44 89.75(6) . . ? C42 Cr4 C44 176.89(6) . . ? C43 Cr4 C44 93.05(6) . . ? C46 Cr4 C45 90.83(6) . . ? C42 Cr4 C45 88.69(6) . . ? C43 Cr4 C45 178.67(5) . . ? C44 Cr4 C45 88.20(6) . . ? C46 Cr4 C41 174.00(5) . . ? C42 Cr4 C41 90.30(5) . . ? C43 Cr4 C41 85.32(5) . . ? C44 Cr4 C41 89.88(5) . . ? C45 Cr4 C41 95.14(5) . . ? F1 C1 C2 121.26(11) . . ? F1 C1 N1 114.69(11) . . ? C2 C1 N1 124.01(11) . . ? C1 C2 F2 117.08(10) . . ? C1 C2 C3 126.46(10) . . ? F2 C2 C3 116.30(10) . . ? C4 C3 C2 143.07(11) . . ? C4 C3 Co2 71.56(7) . . ? C2 C3 Co2 138.68(9) . . ? C4 C3 Co1 67.92(6) . . ? C2 C3 Co1 127.97(8) . . ? Co2 C3 Co1 78.42(4) . . ? C3 C4 C5 141.15(11) . . ? C3 C4 Co1 71.34(7) . . ? C5 C4 Co1 140.59(9) . . ? C3 C4 Co2 67.71(7) . . ? C5 C4 Co2 128.07(8) . . ? Co1 C4 Co2 78.29(4) . . ? C6 C5 F3 117.79(10) . . ? C6 C5 C4 125.28(10) . . ? F3 C5 C4 116.75(10) . . ? C5 C6 F4 121.83(10) . . ? C5 C6 N2 123.83(10) . . ? F4 C6 N2 114.27(10) . . ? O11 C11 Co1 179.92(17) . . ? O12 C12 Co1 177.56(15) . . ? O13 C13 Co1 175.81(13) . . ? O21 C21 Co2 177.09(14) . . ? O22 C22 Co2 177.54(13) . . ? O23 C23 Co2 179.28(19) . . ? N1 C31 Cr3 179.13(11) . . ? O32 C32 Cr3 178.62(14) . . ? O33 C33 Cr3 178.59(13) . . ? O34 C34 Cr3 178.54(14) . . ? O35 C35 Cr3 178.91(12) . . ? O36 C36 Cr3 177.68(15) . . ? N2 C41 Cr4 176.27(10) . . ? O42 C42 Cr4 179.23(13) . . ? O43 C43 Cr4 177.99(12) . . ? O44 C44 Cr4 177.42(13) . . ? O45 C45 Cr4 178.33(13) . . ? O46 C46 Cr4 177.89(14) . . ? C41 N2 C6 167.98(12) . . ? C31 N1 C1 166.99(12) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 33.29 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.820 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.078 # Attachment '- EZ-8.cif' data_2cr2co _database_code_depnum_ccdc_archive 'CCDC 179718' #TrackingRef '- EZ-8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mue2-eta2-eta2[(mue-eta1-eta1-E,Z-2,3,5,6-tetrafluoro1,6-diisocyano- hexa-1,5-dien-3-in)-bis(pentacarbonylchromium)]dicobalt ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 Co2 Cr2 F4 N2 O16' _chemical_formula_weight 870.12 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.6560(10) _cell_length_b 12.1796(9) _cell_length_c 36.970(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6149.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3993 _cell_measurement_theta_min 21.1 _cell_measurement_theta_max 2.2 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 1.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER-AXS SMART 1000 CCD' _diffrn_measurement_method 'omega 2 theta scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51431 _diffrn_reflns_av_R_equivalents 0.1272 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5439 _reflns_number_gt 2910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows (Farrugia, 1997)' _computing_publication_material ? _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^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5439 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.13862(4) 0.18713(5) 0.419658(17) 0.03069(17) Uani 1 1 d . . . Co2 Co 1.02724(5) 0.34556(5) 0.426104(18) 0.03202(18) Uani 1 1 d . . . Cr3 Cr 0.80584(6) 0.06184(7) 0.24169(2) 0.0364(2) Uani 1 1 d . . . Cr4 Cr 0.89323(6) -0.21209(7) 0.38838(2) 0.0416(2) Uani 1 1 d . . . F3 F 0.96827(19) 0.1984(2) 0.50280(7) 0.0462(8) Uani 1 1 d . . . F4 F 0.8704(2) 0.0129(2) 0.50204(8) 0.0546(9) Uani 1 1 d . . . O13 O 1.1648(3) -0.0504(3) 0.41396(10) 0.0575(12) Uani 1 1 d . . . C5 C 0.9620(3) 0.1448(4) 0.47080(12) 0.0286(12) Uani 1 1 d . . . F2 F 0.8541(2) 0.1268(2) 0.38284(8) 0.0517(8) Uani 1 1 d . . . O36 O 0.7179(3) -0.0029(3) 0.16961(10) 0.0696(13) Uani 1 1 d . . . F1 F 1.0479(2) 0.2154(3) 0.32870(7) 0.0685(10) Uani 1 1 d . . . C6 C 0.9135(4) 0.0505(5) 0.47181(14) 0.0367(14) Uani 1 1 d . . . C1 C 0.9627(4) 0.1750(4) 0.33989(14) 0.0418(14) Uani 1 1 d . . . O44 O 0.7843(3) -0.3423(3) 0.44541(10) 0.0657(12) Uani 1 1 d . . . N1 N 0.9031(3) 0.1417(3) 0.31249(11) 0.0446(12) Uani 1 1 d . . . C2 C 0.9441(3) 0.1675(4) 0.37445(13) 0.0278(12) Uani 1 1 d . . . O46 O 0.8718(3) -0.3956(3) 0.33377(11) 0.0744(13) Uani 1 1 d . . . N2 N 0.9069(3) -0.0217(3) 0.44362(12) 0.0372(11) Uani 1 1 d . . . C3 C 1.0050(3) 0.2016(4) 0.40409(12) 0.0256(12) Uani 1 1 d . . . O11 O 1.2557(3) 0.2587(3) 0.35655(10) 0.0624(12) Uani 1 1 d . . . O33 O 0.6212(3) 0.1944(3) 0.25418(11) 0.0736(13) Uani 1 1 d . . . C41 C 0.9031(3) -0.0955(4) 0.42262(15) 0.0403(14) Uani 1 1 d . . . C4 C 1.0104(3) 0.1951(4) 0.44078(12) 0.0289(12) Uani 1 1 d . . . O34 O 0.7153(3) -0.1306(3) 0.28170(11) 0.0686(13) Uani 1 1 d . . . C44 C 0.8251(4) -0.2917(4) 0.42356(15) 0.0458(15) Uani 1 1 d . . . C21 C 1.0548(4) 0.4262(4) 0.38693(15) 0.0435(15) Uani 1 1 d . . . O12 O 1.2647(3) 0.2244(3) 0.48334(10) 0.0673(13) Uani 1 1 d . . . O21 O 1.0691(3) 0.4757(3) 0.36065(11) 0.0742(14) Uani 1 1 d . . . O32 O 0.9048(3) 0.2553(4) 0.20570(12) 0.0946(17) Uani 1 1 d . . . C32 C 0.8662(4) 0.1818(5) 0.21888(15) 0.0539(16) Uani 1 1 d . . . C22 C 1.0909(4) 0.4166(4) 0.46169(16) 0.0525(17) Uani 1 1 d . . . C45 C 1.0096(4) -0.2736(4) 0.40645(16) 0.0530(17) Uani 1 1 d . . . O43 O 0.7005(3) -0.1167(3) 0.36217(10) 0.0639(12) Uani 1 1 d . . . C13 C 1.1554(3) 0.0412(4) 0.41548(13) 0.0363(14) Uani 1 1 d . . . C33 C 0.6917(4) 0.1443(4) 0.25011(14) 0.0453(15) Uani 1 1 d . . . C11 C 1.2130(4) 0.2319(4) 0.38111(14) 0.0392(14) Uani 1 1 d . . . O42 O 1.0024(3) -0.0724(3) 0.33398(12) 0.0846(15) Uani 1 1 d . . . C34 C 0.7483(4) -0.0575(4) 0.26615(14) 0.0476(15) Uani 1 1 d . . . C43 C 0.7735(4) -0.1522(5) 0.37150(15) 0.0505(16) Uani 1 1 d . . . C12 C 1.2178(4) 0.2115(4) 0.45822(14) 0.0466(15) Uani 1 1 d . . . C36 C 0.7518(4) 0.0189(4) 0.19746(14) 0.0486(16) Uani 1 1 d . . . C42 C 0.9612(4) -0.1265(4) 0.35444(17) 0.0535(17) Uani 1 1 d . . . O45 O 1.0789(3) -0.3146(3) 0.41764(13) 0.0778(14) Uani 1 1 d . . . C31 C 0.8639(4) 0.1107(4) 0.28559(14) 0.0409(14) Uani 1 1 d . . . C46 C 0.8808(4) -0.3258(4) 0.35466(16) 0.0515(16) Uani 1 1 d . . . O22 O 1.1316(3) 0.4635(3) 0.48379(12) 0.0856(15) Uani 1 1 d . . . C23 C 0.9074(4) 0.3910(4) 0.43684(14) 0.0435(15) Uani 1 1 d . . . O23 O 0.8286(3) 0.4154(3) 0.44500(10) 0.0624(12) Uani 1 1 d . . . O35 O 0.9876(3) -0.0738(4) 0.22735(11) 0.0793(14) Uani 1 1 d . . . C35 C 0.9180(4) -0.0226(5) 0.23308(15) 0.0498(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0293(4) 0.0351(4) 0.0276(4) -0.0027(3) 0.0002(4) -0.0008(3) Co2 0.0353(4) 0.0307(4) 0.0301(4) -0.0063(3) -0.0028(4) -0.0009(3) Cr3 0.0426(6) 0.0408(5) 0.0258(5) -0.0015(4) -0.0049(5) -0.0050(4) Cr4 0.0406(6) 0.0362(5) 0.0481(6) -0.0014(5) 0.0018(5) -0.0013(4) F3 0.056(2) 0.056(2) 0.0260(16) -0.0082(15) 0.0061(15) -0.0024(16) F4 0.051(2) 0.067(2) 0.046(2) 0.0150(16) 0.0085(18) -0.0065(16) O13 0.074(3) 0.045(2) 0.054(3) -0.004(2) 0.006(2) 0.012(2) C5 0.025(3) 0.039(3) 0.022(3) -0.012(3) -0.005(2) 0.001(3) F2 0.0359(19) 0.068(2) 0.051(2) 0.0045(16) -0.0110(16) -0.0147(16) O36 0.081(3) 0.083(3) 0.044(3) -0.017(2) -0.018(3) -0.016(2) F1 0.062(2) 0.114(3) 0.0300(19) 0.0015(19) 0.0035(18) -0.019(2) C6 0.033(4) 0.054(4) 0.023(3) 0.010(3) 0.008(3) 0.005(3) C1 0.047(4) 0.043(4) 0.036(4) -0.011(3) -0.004(3) 0.002(3) O44 0.074(3) 0.066(3) 0.058(3) 0.009(2) 0.002(2) -0.013(2) N1 0.062(3) 0.041(3) 0.031(3) -0.010(2) -0.022(3) 0.009(2) C2 0.031(3) 0.021(3) 0.031(3) -0.002(2) -0.005(3) 0.004(2) O46 0.102(4) 0.058(3) 0.063(3) -0.013(2) -0.007(3) 0.001(3) N2 0.029(3) 0.035(3) 0.048(3) 0.004(2) 0.001(2) -0.001(2) C3 0.025(3) 0.025(3) 0.028(3) -0.005(2) 0.000(2) 0.001(2) O11 0.069(3) 0.069(3) 0.050(3) 0.005(2) 0.028(2) -0.010(2) O33 0.073(3) 0.073(3) 0.074(3) 0.002(3) -0.006(3) 0.028(3) C41 0.034(3) 0.044(4) 0.044(4) 0.008(3) 0.001(3) 0.007(3) C4 0.033(3) 0.033(3) 0.021(3) -0.005(2) 0.003(2) -0.004(2) O34 0.089(3) 0.048(3) 0.069(3) 0.007(2) 0.018(3) -0.006(2) C44 0.047(4) 0.044(4) 0.047(4) -0.007(3) -0.009(3) -0.001(3) C21 0.053(4) 0.034(3) 0.044(4) -0.015(3) 0.000(3) 0.004(3) O12 0.055(3) 0.098(3) 0.049(3) -0.018(2) -0.023(2) 0.003(2) O21 0.102(4) 0.066(3) 0.055(3) 0.019(2) 0.023(3) 0.016(3) O32 0.096(4) 0.104(4) 0.083(4) 0.043(3) -0.031(3) -0.054(3) C32 0.049(4) 0.070(5) 0.042(4) 0.001(3) -0.019(3) -0.009(3) C22 0.065(5) 0.040(4) 0.053(4) -0.013(3) -0.004(4) 0.008(3) C45 0.036(4) 0.048(4) 0.075(5) -0.016(3) 0.002(3) -0.004(3) O43 0.057(3) 0.078(3) 0.056(3) 0.013(2) -0.007(3) 0.009(3) C13 0.035(3) 0.049(4) 0.025(3) -0.003(3) -0.004(3) 0.006(3) C33 0.056(4) 0.037(4) 0.043(4) 0.006(3) -0.016(3) -0.001(3) C11 0.043(4) 0.032(3) 0.043(4) -0.003(3) 0.003(3) 0.000(3) O42 0.098(4) 0.045(3) 0.111(4) 0.005(3) 0.054(3) 0.004(2) C34 0.056(4) 0.038(4) 0.049(4) -0.009(3) 0.002(3) 0.010(3) C43 0.057(4) 0.048(4) 0.046(4) 0.003(3) -0.003(3) -0.001(3) C12 0.047(4) 0.054(4) 0.039(4) -0.004(3) 0.003(3) 0.004(3) C36 0.054(4) 0.058(4) 0.034(4) -0.004(3) -0.005(3) -0.008(3) C42 0.058(4) 0.033(4) 0.069(5) 0.000(3) 0.023(4) 0.004(3) O45 0.046(3) 0.069(3) 0.118(4) -0.006(3) -0.021(3) 0.006(2) C31 0.050(4) 0.036(3) 0.037(3) 0.001(3) 0.001(3) 0.004(3) C46 0.058(4) 0.045(4) 0.052(4) 0.002(3) -0.003(3) -0.004(3) O22 0.106(4) 0.064(3) 0.086(3) -0.031(3) -0.050(3) 0.001(3) C23 0.053(4) 0.029(3) 0.049(4) -0.014(3) -0.003(3) 0.000(3) O23 0.051(3) 0.069(3) 0.067(3) -0.028(2) 0.000(2) 0.010(2) O35 0.063(3) 0.095(4) 0.081(3) -0.009(3) 0.013(3) 0.017(3) C35 0.049(4) 0.062(4) 0.038(4) -0.015(3) 0.001(3) -0.008(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 Co1 C13 1.798(5) . ? Co1 C12 1.814(6) . ? Co1 C11 1.833(5) . ? Co1 C4 1.920(4) . ? Co1 C3 1.921(4) . ? Co1 Co2 2.4686(9) . ? Co2 C23 1.773(6) . ? Co2 C21 1.790(6) . ? Co2 C22 1.799(6) . ? Co2 C4 1.925(5) . ? Co2 C3 1.956(4) . ? Cr3 C36 1.869(5) . ? Cr3 C35 1.873(6) . ? Cr3 C32 1.878(6) . ? Cr3 C33 1.880(6) . ? Cr3 C34 1.884(6) . ? Cr3 C31 1.902(5) . ? Cr4 C44 1.870(6) . ? Cr4 C46 1.871(6) . ? Cr4 C42 1.877(6) . ? Cr4 C45 1.880(6) . ? Cr4 C43 1.895(6) . ? Cr4 C41 1.907(6) . ? F3 C5 1.354(5) . ? F4 C6 1.343(5) . ? O13 C13 1.125(5) . ? C5 C6 1.327(6) . ? C5 C4 1.429(6) . ? F2 C2 1.361(5) . ? O36 C36 1.160(5) . ? F1 C1 1.330(6) . ? C6 N2 1.366(6) . ? C1 C2 1.306(6) . ? C1 N1 1.361(6) . ? O44 C44 1.159(6) . ? N1 C31 1.191(6) . ? C2 C3 1.437(6) . ? O46 C46 1.156(6) . ? N2 C41 1.189(6) . ? C3 C4 1.361(6) . ? O11 C11 1.127(5) . ? O33 C33 1.150(6) . ? O34 C34 1.150(6) . ? C21 O21 1.160(6) . ? O12 C12 1.139(5) . ? O32 C32 1.147(6) . ? C22 O22 1.141(6) . ? C45 O45 1.147(6) . ? O43 C43 1.141(5) . ? O42 C42 1.150(6) . ? C23 O23 1.157(5) . ? O35 C35 1.156(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 C13 Co1 C12 98.8(2) . . ? C13 Co1 C11 99.0(2) . . ? C12 Co1 C11 103.4(2) . . ? C13 Co1 C4 101.6(2) . . ? C12 Co1 C4 102.5(2) . . ? C11 Co1 C4 143.8(2) . . ? C13 Co1 C3 100.7(2) . . ? C12 Co1 C3 141.9(2) . . ? C11 Co1 C3 105.4(2) . . ? C4 Co1 C3 41.49(16) . . ? C13 Co1 Co2 149.22(16) . . ? C12 Co1 Co2 99.41(16) . . ? C11 Co1 Co2 100.61(15) . . ? C4 Co1 Co2 50.15(13) . . ? C3 Co1 Co2 51.09(13) . . ? C23 Co2 C21 101.8(2) . . ? C23 Co2 C22 97.6(2) . . ? C21 Co2 C22 103.1(2) . . ? C23 Co2 C4 97.1(2) . . ? C21 Co2 C4 140.9(2) . . ? C22 Co2 C4 108.0(2) . . ? C23 Co2 C3 103.3(2) . . ? C21 Co2 C3 100.8(2) . . ? C22 Co2 C3 144.1(2) . . ? C4 Co2 C3 41.04(16) . . ? C23 Co2 Co1 146.57(16) . . ? C21 Co2 Co1 102.78(16) . . ? C22 Co2 Co1 98.55(17) . . ? C4 Co2 Co1 49.98(13) . . ? C3 Co2 Co1 49.83(13) . . ? C36 Cr3 C35 91.2(2) . . ? C36 Cr3 C32 89.9(2) . . ? C35 Cr3 C32 89.5(3) . . ? C36 Cr3 C33 88.1(2) . . ? C35 Cr3 C33 178.9(2) . . ? C32 Cr3 C33 91.3(2) . . ? C36 Cr3 C34 92.3(2) . . ? C35 Cr3 C34 90.0(2) . . ? C32 Cr3 C34 177.8(2) . . ? C33 Cr3 C34 89.2(2) . . ? C36 Cr3 C31 177.4(2) . . ? C35 Cr3 C31 88.6(2) . . ? C32 Cr3 C31 87.5(2) . . ? C33 Cr3 C31 92.1(2) . . ? C34 Cr3 C31 90.3(2) . . ? C44 Cr4 C46 92.0(2) . . ? C44 Cr4 C42 177.4(2) . . ? C46 Cr4 C42 90.6(2) . . ? C44 Cr4 C45 88.1(2) . . ? C46 Cr4 C45 91.1(2) . . ? C42 Cr4 C45 92.3(3) . . ? C44 Cr4 C43 90.0(2) . . ? C46 Cr4 C43 89.2(2) . . ? C42 Cr4 C43 89.6(2) . . ? C45 Cr4 C43 178.1(2) . . ? C44 Cr4 C41 87.7(2) . . ? C46 Cr4 C41 178.8(2) . . ? C42 Cr4 C41 89.7(2) . . ? C45 Cr4 C41 90.1(2) . . ? C43 Cr4 C41 89.6(2) . . ? C6 C5 F3 115.1(5) . . ? C6 C5 C4 128.6(4) . . ? F3 C5 C4 116.3(4) . . ? C5 C6 F4 122.5(5) . . ? C5 C6 N2 124.7(5) . . ? F4 C6 N2 112.7(5) . . ? C2 C1 F1 120.0(5) . . ? C2 C1 N1 126.2(5) . . ? F1 C1 N1 113.7(5) . . ? C31 N1 C1 169.9(5) . . ? C1 C2 F2 115.1(5) . . ? C1 C2 C3 127.8(5) . . ? F2 C2 C3 117.0(4) . . ? C41 N2 C6 170.9(5) . . ? C4 C3 C2 140.7(5) . . ? C4 C3 Co1 69.2(3) . . ? C2 C3 Co1 138.7(3) . . ? C4 C3 Co2 68.3(3) . . ? C2 C3 Co2 131.8(3) . . ? Co1 C3 Co2 79.08(17) . . ? N2 C41 Cr4 178.2(5) . . ? C3 C4 C5 140.8(5) . . ? C3 C4 Co1 69.3(3) . . ? C5 C4 Co1 135.7(4) . . ? C3 C4 Co2 70.7(3) . . ? C5 C4 Co2 133.0(3) . . ? Co1 C4 Co2 79.87(17) . . ? O44 C44 Cr4 178.8(5) . . ? O21 C21 Co2 176.6(5) . . ? O32 C32 Cr3 178.2(5) . . ? O22 C22 Co2 178.6(6) . . ? O45 C45 Cr4 177.5(5) . . ? O13 C13 Co1 177.8(5) . . ? O33 C33 Cr3 177.9(5) . . ? O11 C11 Co1 177.3(5) . . ? O34 C34 Cr3 178.1(5) . . ? O43 C43 Cr4 178.3(5) . . ? O12 C12 Co1 177.1(5) . . ? O36 C36 Cr3 176.9(5) . . ? O42 C42 Cr4 178.8(5) . . ? N1 C31 Cr3 177.9(5) . . ? O46 C46 Cr4 179.1(6) . . ? O23 C23 Co2 176.2(5) . . ? O35 C35 Cr3 179.0(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.470 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.081 # Attachment '- E3d.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 836248' #TrackingRef '- E3d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H9 Cr F2 N O5 Si' _chemical_formula_weight 377.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.1314(18) _cell_length_b 11.701(2) _cell_length_c 23.613(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.923(5) _cell_angle_gamma 90.00 _cell_volume 1690.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 945 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.8 _exptl_crystal_description platelett _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; the ratio T_min/T_max is given by the program ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19666 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.35 _reflns_number_total 3458 _reflns_number_gt 2520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0553P)^2^+1.9700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3458 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.97246(7) 0.45492(4) 0.15360(2) 0.02300(16) Uani 1 1 d . . . C1 C 1.1145(5) 0.5444(3) 0.21285(14) 0.0300(7) Uani 1 1 d . . . C2 C 0.8616(5) 0.3547(3) 0.20870(13) 0.0303(7) Uani 1 1 d . . . C3 C 1.2234(5) 0.3599(3) 0.15247(14) 0.0299(7) Uani 1 1 d . . . C4 C 0.7204(5) 0.5504(3) 0.15465(15) 0.0345(8) Uani 1 1 d . . . C5 C 1.0857(5) 0.5493(3) 0.09579(14) 0.0327(7) Uani 1 1 d . . . C6 C 0.8214(5) 0.3641(3) 0.09492(13) 0.0280(7) Uani 1 1 d . . . C7 C 0.5999(5) 0.2418(3) 0.02386(14) 0.0329(7) Uani 1 1 d . . . C8 C 0.4149(6) 0.2716(3) -0.00370(15) 0.0360(8) Uani 1 1 d . . . C9 C 0.2852(6) 0.2021(3) -0.04179(14) 0.0341(8) Uani 1 1 d . . . C10 C 0.1761(5) 0.1421(3) -0.07311(14) 0.0331(7) Uani 1 1 d . . . C11 C -0.1716(6) -0.0418(3) -0.08746(17) 0.0439(9) Uani 1 1 d . . . H11A H -0.0828 -0.0897 -0.0608 0.066 Uiso 1 1 calc R . . H11B H -0.2547 -0.0905 -0.1150 0.066 Uiso 1 1 calc R . . H11C H -0.2730 0.0040 -0.0665 0.066 Uiso 1 1 calc R . . C12 C 0.2044(6) -0.0290(3) -0.16584(16) 0.0422(9) Uani 1 1 d . . . H12A H 0.3169 0.0225 -0.1788 0.063 Uiso 1 1 calc R . . H12B H 0.1261 -0.0649 -0.1988 0.063 Uiso 1 1 calc R . . H12C H 0.2735 -0.0882 -0.1413 0.063 Uiso 1 1 calc R . . C13 C -0.1528(7) 0.1561(3) -0.17113(16) 0.0451(9) Uani 1 1 d . . . H13A H -0.2487 0.2006 -0.1480 0.068 Uiso 1 1 calc R . . H13B H -0.2415 0.1139 -0.2002 0.068 Uiso 1 1 calc R . . H13C H -0.0534 0.2078 -0.1894 0.068 Uiso 1 1 calc R . . F1 F 0.6757(4) 0.1366(2) 0.01775(12) 0.0750(9) Uani 1 1 d . . . F2 F 0.3470(5) 0.3788(2) 0.00491(14) 0.0887(11) Uani 1 1 d . . . N1 N 0.7236(5) 0.3076(3) 0.06077(12) 0.0368(7) Uani 1 1 d . . . O1 O 1.1971(4) 0.5964(2) 0.24884(11) 0.0457(7) Uani 1 1 d . . . O2 O 0.7998(4) 0.2938(2) 0.24135(10) 0.0472(7) Uani 1 1 d . . . O3 O 1.3753(4) 0.3033(2) 0.15222(12) 0.0472(7) Uani 1 1 d . . . O4 O 0.5702(4) 0.6077(2) 0.15498(13) 0.0551(8) Uani 1 1 d . . . O5 O 1.1537(4) 0.6028(2) 0.06098(11) 0.0490(7) Uani 1 1 d . . . Si1 Si 0.00839(14) 0.05389(7) -0.12529(4) 0.0277(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0206(2) 0.0275(3) 0.0205(3) -0.0024(2) -0.00166(18) -0.0037(2) C1 0.0309(16) 0.0312(17) 0.0273(17) 0.0029(14) -0.0036(14) -0.0019(14) C2 0.0317(17) 0.0344(18) 0.0247(17) -0.0071(15) 0.0010(14) -0.0040(14) C3 0.0271(16) 0.0312(17) 0.0311(18) -0.0031(14) -0.0007(13) -0.0052(14) C4 0.0275(17) 0.0383(19) 0.0371(19) -0.0018(16) -0.0014(14) -0.0035(15) C5 0.0265(16) 0.0384(18) 0.0322(18) -0.0032(16) -0.0046(14) -0.0008(14) C6 0.0230(15) 0.0374(18) 0.0236(16) -0.0011(14) 0.0017(13) -0.0054(13) C7 0.0350(18) 0.0384(19) 0.0250(17) -0.0059(14) 0.0002(14) -0.0061(15) C8 0.0416(19) 0.0303(17) 0.0353(19) -0.0060(15) -0.0035(16) -0.0039(15) C9 0.0359(18) 0.0370(19) 0.0287(18) 0.0016(15) -0.0036(15) -0.0051(15) C10 0.0318(17) 0.0343(18) 0.0324(18) -0.0027(15) -0.0043(14) -0.0047(14) C11 0.040(2) 0.044(2) 0.047(2) -0.0015(18) 0.0003(17) -0.0102(17) C12 0.044(2) 0.042(2) 0.040(2) -0.0005(17) -0.0005(17) 0.0055(17) C13 0.055(2) 0.0334(19) 0.043(2) -0.0046(17) -0.0196(18) 0.0059(17) F1 0.0680(17) 0.0576(16) 0.093(2) -0.0337(15) -0.0431(15) 0.0228(13) F2 0.0839(19) 0.0468(15) 0.127(3) -0.0416(16) -0.0570(18) 0.0211(14) N1 0.0333(15) 0.0536(19) 0.0234(14) -0.0049(14) 0.0008(12) -0.0167(14) O1 0.0593(17) 0.0400(14) 0.0351(14) -0.0041(12) -0.0172(13) -0.0096(13) O2 0.0592(17) 0.0463(16) 0.0373(15) 0.0043(13) 0.0117(13) -0.0101(13) O3 0.0312(13) 0.0445(15) 0.0663(18) 0.0008(13) 0.0063(12) 0.0056(12) O4 0.0346(15) 0.0549(18) 0.076(2) -0.0028(15) 0.0027(14) 0.0136(13) O5 0.0549(16) 0.0507(16) 0.0427(16) 0.0132(13) 0.0120(13) -0.0049(13) Si1 0.0289(5) 0.0268(4) 0.0263(5) -0.0022(4) -0.0060(4) -0.0025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C3 1.900(3) . ? Cr1 C4 1.909(3) . ? Cr1 C1 1.909(3) . ? Cr1 C2 1.911(3) . ? Cr1 C5 1.922(4) . ? Cr1 C6 1.931(3) . ? C1 O1 1.135(4) . ? C2 O2 1.134(4) . ? C3 O3 1.143(4) . ? C4 O4 1.139(4) . ? C5 O5 1.135(4) . ? C6 N1 1.175(4) . ? C7 C8 1.315(5) . ? C7 F1 1.327(4) . ? C7 N1 1.356(4) . ? C8 F2 1.341(4) . ? C8 C9 1.416(5) . ? C9 C10 1.191(5) . ? C10 Si1 1.862(3) . ? C11 Si1 1.845(4) . ? C12 Si1 1.860(4) . ? C13 Si1 1.852(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Cr1 C4 179.94(17) . . ? C3 Cr1 C1 90.11(14) . . ? C4 Cr1 C1 89.92(14) . . ? C3 Cr1 C2 88.67(14) . . ? C4 Cr1 C2 91.39(14) . . ? C1 Cr1 C2 90.19(13) . . ? C3 Cr1 C5 89.65(14) . . ? C4 Cr1 C5 90.29(14) . . ? C1 Cr1 C5 92.09(14) . . ? C2 Cr1 C5 177.17(14) . . ? C3 Cr1 C6 90.98(14) . . ? C4 Cr1 C6 89.00(14) . . ? C1 Cr1 C6 178.35(13) . . ? C2 Cr1 C6 88.60(13) . . ? C5 Cr1 C6 89.16(14) . . ? O1 C1 Cr1 178.7(3) . . ? O2 C2 Cr1 178.5(3) . . ? O3 C3 Cr1 179.4(3) . . ? O4 C4 Cr1 179.6(4) . . ? O5 C5 Cr1 178.4(3) . . ? N1 C6 Cr1 177.3(3) . . ? C8 C7 F1 119.3(3) . . ? C8 C7 N1 126.4(3) . . ? F1 C7 N1 114.3(3) . . ? C7 C8 F2 116.1(3) . . ? C7 C8 C9 126.1(3) . . ? F2 C8 C9 117.8(3) . . ? C10 C9 C8 178.8(4) . . ? C9 C10 Si1 176.8(3) . . ? C6 N1 C7 176.1(3) . . ? C11 Si1 C13 111.21(19) . . ? C11 Si1 C12 111.20(18) . . ? C13 Si1 C12 111.93(18) . . ? C11 Si1 C10 109.73(17) . . ? C13 Si1 C10 106.09(16) . . ? C12 Si1 C10 106.42(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.596 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.079 # Attachment '- Z-3h.CIF' data_bencr _database_code_depnum_ccdc_archive 'CCDC 836249' #TrackingRef '- Z-3h.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 Cr F7 N O5' _chemical_formula_weight 447.15 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.850(5) _cell_length_b 6.184(2) _cell_length_c 11.752(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.566(10) _cell_angle_gamma 90.00 _cell_volume 1570.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 25.5 _exptl_crystal_description platelett _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6271 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS 2008/1 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART CCD' _diffrn_measurement_method 'omegea scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16978 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3220 _reflns_number_gt 2423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0576P)^2^+1.0779P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3220 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.37306(2) 0.56262(7) 0.58885(4) 0.01895(14) Uani 1 1 d . . . C1 C 0.43631(13) 0.6858(5) 0.5128(2) 0.0248(6) Uani 1 1 d . . . C2 C 0.43544(13) 0.4351(5) 0.7021(2) 0.0243(6) Uani 1 1 d . . . C3 C 0.37300(13) 0.3086(5) 0.4955(2) 0.0248(6) Uani 1 1 d . . . C4 C 0.31211(13) 0.6934(5) 0.4774(3) 0.0257(6) Uani 1 1 d . . . C5 C 0.37237(13) 0.8124(5) 0.6841(2) 0.0254(6) Uani 1 1 d . . . C6 C 0.30827(13) 0.4371(5) 0.6619(2) 0.0237(6) Uani 1 1 d . . . C7 C 0.21767(14) 0.2947(5) 0.7501(3) 0.0305(7) Uani 1 1 d . . . C8 C 0.15972(14) 0.3343(5) 0.7077(3) 0.0312(7) Uani 1 1 d . . . C9 C 0.13648(13) 0.4688(5) 0.6075(3) 0.0301(7) Uani 1 1 d . . . C10 C 0.16100(14) 0.6713(5) 0.5905(3) 0.0317(7) Uani 1 1 d . . . C11 C 0.14064(16) 0.7971(6) 0.4950(3) 0.0394(8) Uani 1 1 d . . . C12 C 0.09366(17) 0.7219(7) 0.4151(3) 0.0467(10) Uani 1 1 d . . . C13 C 0.06679(15) 0.5260(7) 0.4302(3) 0.0453(10) Uani 1 1 d . . . C14 C 0.08808(15) 0.4006(6) 0.5244(3) 0.0393(8) Uani 1 1 d . . . F1 F 0.23208(9) 0.1739(4) 0.84472(18) 0.0501(6) Uani 1 1 d . . . F2 F 0.11583(9) 0.2405(4) 0.76063(19) 0.0518(6) Uani 1 1 d . . . F3 F 0.20468(9) 0.7562(3) 0.66965(16) 0.0382(5) Uani 1 1 d . . . F4 F 0.16630(10) 0.9898(3) 0.4818(2) 0.0532(6) Uani 1 1 d . . . F5 F 0.07345(11) 0.8409(5) 0.3218(2) 0.0747(8) Uani 1 1 d . . . F6 F 0.01987(9) 0.4532(5) 0.35264(19) 0.0691(8) Uani 1 1 d . . . F7 F 0.06197(9) 0.2085(4) 0.5368(2) 0.0548(6) Uani 1 1 d . . . N1 N 0.26754(11) 0.3630(4) 0.7037(2) 0.0275(6) Uani 1 1 d . . . O1 O 0.47348(10) 0.7571(4) 0.46580(19) 0.0364(5) Uani 1 1 d . . . O2 O 0.47253(10) 0.3614(4) 0.76773(19) 0.0380(6) Uani 1 1 d . . . O3 O 0.37278(11) 0.1573(4) 0.4415(2) 0.0371(5) Uani 1 1 d . . . O4 O 0.27583(10) 0.7744(4) 0.4117(2) 0.0369(5) Uani 1 1 d . . . O5 O 0.37124(12) 0.9612(4) 0.7403(2) 0.0421(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0200(2) 0.0193(2) 0.0178(2) 0.00041(18) 0.00345(16) 0.00080(18) C1 0.0266(15) 0.0232(14) 0.0243(15) -0.0023(12) 0.0027(12) 0.0044(12) C2 0.0253(15) 0.0268(14) 0.0224(14) -0.0008(13) 0.0085(12) 0.0008(13) C3 0.0272(15) 0.0250(15) 0.0223(15) 0.0050(12) 0.0037(12) 0.0001(12) C4 0.0251(15) 0.0276(15) 0.0259(15) -0.0026(13) 0.0085(12) -0.0022(13) C5 0.0264(15) 0.0291(15) 0.0210(15) 0.0041(13) 0.0042(12) 0.0007(12) C6 0.0247(15) 0.0232(14) 0.0218(14) 0.0005(12) -0.0010(12) 0.0044(12) C7 0.0316(17) 0.0313(16) 0.0309(16) 0.0108(13) 0.0116(13) 0.0001(13) C8 0.0269(16) 0.0341(16) 0.0354(18) 0.0032(14) 0.0137(13) -0.0055(13) C9 0.0218(15) 0.0404(18) 0.0286(16) -0.0021(14) 0.0059(12) 0.0059(13) C10 0.0285(16) 0.0407(18) 0.0267(16) 0.0007(14) 0.0072(13) 0.0113(14) C11 0.0327(18) 0.048(2) 0.0394(19) 0.0057(16) 0.0126(15) 0.0124(16) C12 0.036(2) 0.075(3) 0.0291(19) 0.0050(19) 0.0064(15) 0.026(2) C13 0.0216(16) 0.081(3) 0.0318(19) -0.0195(19) -0.0029(14) 0.0170(18) C14 0.0231(16) 0.053(2) 0.043(2) -0.0169(17) 0.0096(14) 0.0020(15) F1 0.0449(12) 0.0587(13) 0.0488(12) 0.0330(11) 0.0142(10) 0.0061(10) F2 0.0332(11) 0.0645(15) 0.0627(14) 0.0189(12) 0.0232(10) -0.0094(10) F3 0.0399(11) 0.0345(10) 0.0392(11) 0.0010(8) 0.0028(9) -0.0002(8) F4 0.0539(13) 0.0470(12) 0.0612(14) 0.0224(11) 0.0169(11) 0.0163(10) F5 0.0608(16) 0.121(2) 0.0402(13) 0.0280(15) -0.0005(11) 0.0321(16) F6 0.0291(11) 0.126(2) 0.0487(14) -0.0359(15) -0.0070(10) 0.0130(13) F7 0.0291(11) 0.0592(14) 0.0771(16) -0.0254(12) 0.0110(10) -0.0063(10) N1 0.0233(13) 0.0287(13) 0.0311(14) 0.0055(11) 0.0055(11) 0.0007(10) O1 0.0351(13) 0.0395(13) 0.0382(13) 0.0040(11) 0.0171(11) -0.0039(10) O2 0.0334(13) 0.0486(14) 0.0299(12) 0.0063(11) -0.0023(10) 0.0103(11) O3 0.0466(14) 0.0269(11) 0.0384(13) -0.0082(10) 0.0084(11) -0.0016(10) O4 0.0317(12) 0.0408(13) 0.0350(12) 0.0076(11) -0.0057(10) 0.0050(10) O5 0.0607(16) 0.0300(12) 0.0365(13) -0.0092(11) 0.0107(12) 0.0011(11) _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 Cr1 C4 1.903(3) . ? Cr1 C5 1.909(3) . ? Cr1 C1 1.912(3) . ? Cr1 C3 1.916(3) . ? Cr1 C6 1.925(3) . ? Cr1 C2 1.926(3) . ? C1 O1 1.137(4) . ? C2 O2 1.129(3) . ? C3 O3 1.131(4) . ? C4 O4 1.137(4) . ? C5 O5 1.135(4) . ? C6 N1 1.172(4) . ? C7 C8 1.313(4) . ? C7 F1 1.338(3) . ? C7 N1 1.357(4) . ? C8 F2 1.349(3) . ? C8 C9 1.468(4) . ? C9 C10 1.388(5) . ? C9 C14 1.394(4) . ? C10 F3 1.337(4) . ? C10 C11 1.383(5) . ? C11 F4 1.336(4) . ? C11 C12 1.365(5) . ? C12 F5 1.339(4) . ? C12 C13 1.370(6) . ? C13 F6 1.344(4) . ? C13 C14 1.374(5) . ? C14 F7 1.335(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Cr1 C5 89.66(13) . . ? C4 Cr1 C1 89.40(12) . . ? C5 Cr1 C1 91.23(12) . . ? C4 Cr1 C3 90.77(12) . . ? C5 Cr1 C3 178.84(12) . . ? C1 Cr1 C3 89.86(12) . . ? C4 Cr1 C6 89.56(12) . . ? C5 Cr1 C6 89.67(12) . . ? C1 Cr1 C6 178.62(12) . . ? C3 Cr1 C6 89.25(12) . . ? C4 Cr1 C2 179.00(13) . . ? C5 Cr1 C2 89.57(12) . . ? C1 Cr1 C2 89.98(12) . . ? C3 Cr1 C2 90.01(12) . . ? C6 Cr1 C2 91.07(12) . . ? O1 C1 Cr1 178.8(3) . . ? O2 C2 Cr1 179.2(3) . . ? O3 C3 Cr1 179.1(3) . . ? O4 C4 Cr1 179.0(3) . . ? O5 C5 Cr1 179.2(3) . . ? N1 C6 Cr1 178.0(3) . . ? C8 C7 F1 120.9(3) . . ? C8 C7 N1 125.2(3) . . ? F1 C7 N1 113.9(3) . . ? C7 C8 F2 117.1(3) . . ? C7 C8 C9 127.5(3) . . ? F2 C8 C9 115.4(3) . . ? C10 C9 C14 116.1(3) . . ? C10 C9 C8 122.1(3) . . ? C14 C9 C8 121.8(3) . . ? F3 C10 C11 117.0(3) . . ? F3 C10 C9 120.3(3) . . ? C11 C10 C9 122.7(3) . . ? F4 C11 C12 120.6(3) . . ? F4 C11 C10 120.4(3) . . ? C12 C11 C10 119.0(4) . . ? F5 C12 C11 119.9(4) . . ? F5 C12 C13 119.8(4) . . ? C11 C12 C13 120.3(3) . . ? F6 C13 C12 120.4(4) . . ? F6 C13 C14 119.3(4) . . ? C12 C13 C14 120.2(3) . . ? F7 C14 C13 119.4(3) . . ? F7 C14 C9 119.0(3) . . ? C13 C14 C9 121.6(4) . . ? C6 N1 C7 174.8(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.545 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.077 # Attachment '- ZZ-9.CIF' data_1monika _database_code_depnum_ccdc_archive 'CCDC 836250' #TrackingRef '- ZZ-9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 Co4 Cr2 F4 N2 O22' _chemical_formula_weight 1180.06 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.994(3) _cell_length_b 11.837(3) _cell_length_c 24.944(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4131.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 960 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 2.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS ASMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32362 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.12 _reflns_number_total 3671 _reflns_number_gt 3152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0413P)^2^+46.0795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3671 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.60533(7) 0.15626(8) 0.53666(4) 0.0285(3) Uani 1 1 d . . . Co2 Co 0.51324(8) 0.18593(8) 0.45337(4) 0.0302(3) Uani 1 1 d . . . Cr3 Cr 0.54155(12) 0.45359(12) 0.71005(5) 0.0446(4) Uani 1 1 d . . . F2 F 0.3030(3) 0.1332(4) 0.5367(2) 0.0495(13) Uani 1 1 d . . . C3 C 0.4697(5) 0.1528(6) 0.5265(3) 0.0300(16) Uani 1 1 d . . . O7 O 0.6387(5) 0.3986(5) 0.5576(2) 0.0465(15) Uani 1 1 d . . . N1 N 0.4454(5) 0.3033(5) 0.6236(3) 0.0392(16) Uani 1 1 d . . . C2 C 0.3835(6) 0.1809(6) 0.5567(3) 0.0291(16) Uani 1 1 d . . . O11 O 0.5429(6) 0.4316(6) 0.4410(3) 0.073(2) Uani 1 1 d . . . O1 O 0.6164(7) 0.6148(7) 0.7943(3) 0.081(3) Uani 1 1 d . . . O2 O 0.4471(6) 0.3126(7) 0.7963(3) 0.076(2) Uani 1 1 d . . . C4 C 0.5070(5) 0.0594(6) 0.5033(3) 0.0275(15) Uani 1 1 d . . . O9 O 0.3270(4) 0.1635(6) 0.4012(3) 0.0509(16) Uani 1 1 d . . . O4 O 0.6546(6) 0.5932(6) 0.6299(3) 0.066(2) Uani 1 1 d . . . O8 O 0.7886(4) 0.0866(5) 0.4902(3) 0.0514(16) Uani 1 1 d . . . C10O C 0.3988(6) 0.1737(7) 0.4213(3) 0.0368(18) Uani 1 1 d . . . F1 F 0.2880(4) 0.2623(5) 0.6194(2) 0.0567(14) Uani 1 1 d . . . C4O C 0.6109(8) 0.5402(8) 0.6585(4) 0.051(2) Uani 1 1 d . . . C11O C 0.5914(6) 0.1240(8) 0.4027(4) 0.041(2) Uani 1 1 d . . . O6 O 0.6106(6) 0.0720(6) 0.6470(3) 0.063(2) Uani 1 1 d . . . C9O C 0.7193(6) 0.1112(6) 0.5082(3) 0.0335(17) Uani 1 1 d . . . O10 O 0.6358(5) 0.0780(7) 0.3726(3) 0.071(2) Uani 1 1 d . . . C12O C 0.5312(7) 0.3380(7) 0.4456(3) 0.045(2) Uani 1 1 d . . . C7O C 0.6110(6) 0.1032(7) 0.6048(4) 0.043(2) Uani 1 1 d . . . C6O C 0.4827(7) 0.3590(7) 0.6561(3) 0.041(2) Uani 1 1 d . . . C1 C 0.3744(6) 0.2470(7) 0.5988(3) 0.0368(18) Uani 1 1 d . . . C8O C 0.6283(6) 0.3055(7) 0.5500(3) 0.0375(18) Uani 1 1 d . . . C5O C 0.6495(9) 0.3560(9) 0.7151(4) 0.059(3) Uani 1 1 d . . . C3O C 0.4347(10) 0.5503(11) 0.7049(5) 0.076(3) Uani 1 1 d . . . O5 O 0.7133(7) 0.2989(8) 0.7186(4) 0.098(3) Uani 1 1 d . . . C2O C 0.4800(8) 0.3661(8) 0.7638(4) 0.054(2) Uani 1 1 d . . . C1O C 0.5897(9) 0.5523(8) 0.7640(4) 0.059(3) Uani 1 1 d . . . O3 O 0.3717(8) 0.6090(10) 0.6981(5) 0.119(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0343(6) 0.0226(5) 0.0287(5) 0.0022(4) -0.0032(4) -0.0036(4) Co2 0.0388(6) 0.0239(5) 0.0281(5) 0.0050(4) -0.0040(4) -0.0049(4) Cr3 0.0671(10) 0.0343(7) 0.0323(7) -0.0044(6) 0.0023(7) -0.0001(7) F2 0.033(3) 0.056(3) 0.059(3) -0.004(3) 0.003(2) -0.004(2) C3 0.036(4) 0.023(4) 0.031(4) 0.005(3) 0.005(3) -0.002(3) O7 0.062(4) 0.027(3) 0.050(4) -0.003(3) 0.001(3) -0.009(3) N1 0.062(5) 0.027(3) 0.029(3) 0.000(3) 0.002(3) 0.004(3) C2 0.042(4) 0.029(4) 0.017(3) 0.006(3) -0.004(3) 0.004(3) O11 0.111(6) 0.034(4) 0.072(5) 0.019(3) -0.035(5) -0.021(4) O1 0.136(8) 0.057(5) 0.051(4) -0.014(4) -0.011(5) -0.019(5) O2 0.109(7) 0.074(5) 0.044(4) -0.003(4) 0.024(4) -0.026(5) C4 0.029(4) 0.024(4) 0.029(4) 0.003(3) -0.005(3) -0.003(3) O9 0.044(4) 0.056(4) 0.053(4) 0.010(3) -0.012(3) -0.003(3) O4 0.109(6) 0.045(4) 0.044(4) 0.003(3) 0.002(4) -0.017(4) O8 0.039(3) 0.047(4) 0.069(4) 0.018(3) 0.009(3) 0.003(3) C10O 0.046(5) 0.031(4) 0.033(4) 0.006(3) 0.004(4) 0.003(4) F1 0.054(3) 0.064(4) 0.052(3) 0.002(3) 0.012(3) 0.018(3) C4O 0.081(7) 0.039(5) 0.034(5) -0.003(4) -0.004(5) -0.003(5) C11O 0.039(5) 0.045(5) 0.039(5) 0.004(4) -0.004(4) -0.013(4) O6 0.095(6) 0.064(4) 0.031(3) 0.015(3) -0.003(3) -0.010(4) C9O 0.034(4) 0.026(4) 0.041(4) 0.006(3) -0.002(4) -0.003(3) O10 0.058(4) 0.082(5) 0.073(5) -0.034(4) 0.018(4) -0.015(4) C12O 0.062(6) 0.032(5) 0.039(5) 0.012(4) -0.017(4) -0.008(4) C7O 0.049(5) 0.029(4) 0.052(6) -0.006(4) 0.002(4) -0.008(4) C6O 0.053(5) 0.030(4) 0.040(5) 0.004(4) 0.010(4) 0.004(4) C1 0.043(5) 0.035(4) 0.033(4) 0.012(4) 0.006(4) 0.013(4) C8O 0.035(4) 0.036(5) 0.042(5) 0.002(4) -0.005(4) -0.006(3) C5O 0.072(7) 0.049(6) 0.055(6) 0.008(5) 0.005(5) -0.003(5) C3O 0.084(9) 0.063(7) 0.082(9) -0.018(6) -0.014(7) 0.017(7) O5 0.086(6) 0.084(6) 0.125(8) 0.040(6) 0.016(6) 0.026(5) C2O 0.077(7) 0.052(6) 0.033(5) -0.015(4) 0.005(5) -0.010(5) C1O 0.091(8) 0.036(5) 0.051(6) -0.003(4) -0.008(6) -0.005(5) O3 0.107(8) 0.111(8) 0.140(10) -0.035(7) -0.016(7) 0.058(7) _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 C7O 1.813(10) . ? Co1 C9O 1.826(9) . ? Co1 C8O 1.826(8) . ? Co1 C3 1.915(8) . ? Co1 C4 1.975(7) . ? Co1 Co2 2.4699(15) . ? Co2 C10O 1.796(9) . ? Co2 C11O 1.826(10) . ? Co2 C12O 1.828(8) . ? Co2 C4 1.950(7) . ? Co2 C3 1.963(7) . ? Cr3 C3O 1.888(13) . ? Cr3 C2O 1.901(10) . ? Cr3 C1O 1.905(10) . ? Cr3 C5O 1.906(12) . ? Cr3 C4O 1.911(10) . ? Cr3 C6O 1.936(9) . ? F2 C2 1.356(9) . ? C3 C4 1.353(11) . ? C3 C2 1.460(10) . ? O7 C8O 1.128(10) . ? N1 C6O 1.168(11) . ? N1 C1 1.347(11) . ? C2 C1 1.315(11) . ? O11 C12O 1.125(10) . ? O1 C1O 1.121(11) . ? O2 C2O 1.127(11) . ? C4 C4 1.429(14) 5_656 ? O9 C10O 1.129(10) . ? O4 C4O 1.129(11) . ? O8 C9O 1.107(10) . ? F1 C1 1.327(9) . ? C11O O10 1.115(11) . ? O6 C7O 1.116(11) . ? C5O O5 1.124(13) . ? C3O O3 1.134(14) . ? 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 C7O Co1 C9O 103.0(4) . . ? C7O Co1 C8O 99.1(4) . . ? C9O Co1 C8O 101.5(4) . . ? C7O Co1 C3 99.2(4) . . ? C9O Co1 C3 143.9(3) . . ? C8O Co1 C3 102.6(3) . . ? C7O Co1 C4 103.0(3) . . ? C9O Co1 C4 105.9(3) . . ? C8O Co1 C4 139.5(3) . . ? C3 Co1 C4 40.7(3) . . ? C7O Co1 Co2 149.4(3) . . ? C9O Co1 Co2 99.8(3) . . ? C8O Co1 Co2 96.1(3) . . ? C3 Co1 Co2 51.3(2) . . ? C4 Co1 Co2 50.5(2) . . ? C10O Co2 C11O 101.1(4) . . ? C10O Co2 C12O 98.9(4) . . ? C11O Co2 C12O 103.9(4) . . ? C10O Co2 C4 100.5(3) . . ? C11O Co2 C4 99.2(4) . . ? C12O Co2 C4 146.1(3) . . ? C10O Co2 C3 97.0(3) . . ? C11O Co2 C3 138.6(4) . . ? C12O Co2 C3 109.7(4) . . ? C4 Co2 C3 40.5(3) . . ? C10O Co2 Co1 145.9(3) . . ? C11O Co2 Co1 102.3(3) . . ? C12O Co2 Co1 99.0(3) . . ? C4 Co2 Co1 51.5(2) . . ? C3 Co2 Co1 49.6(2) . . ? C3O Cr3 C2O 91.2(6) . . ? C3O Cr3 C1O 87.5(5) . . ? C2O Cr3 C1O 89.8(4) . . ? C3O Cr3 C5O 179.9(6) . . ? C2O Cr3 C5O 89.0(5) . . ? C1O Cr3 C5O 92.6(5) . . ? C3O Cr3 C4O 91.7(5) . . ? C2O Cr3 C4O 176.3(5) . . ? C1O Cr3 C4O 88.1(4) . . ? C5O Cr3 C4O 88.1(4) . . ? C3O Cr3 C6O 88.1(5) . . ? C2O Cr3 C6O 89.0(4) . . ? C1O Cr3 C6O 175.4(5) . . ? C5O Cr3 C6O 91.9(4) . . ? C4O Cr3 C6O 93.3(4) . . ? C4 C3 C2 136.5(7) . . ? C4 C3 Co1 72.0(5) . . ? C2 C3 Co1 138.2(6) . . ? C4 C3 Co2 69.2(4) . . ? C2 C3 Co2 133.7(5) . . ? Co1 C3 Co2 79.1(3) . . ? C6O N1 C1 158.1(8) . . ? C1 C2 F2 117.4(7) . . ? C1 C2 C3 128.9(8) . . ? F2 C2 C3 113.7(6) . . ? C3 C4 C4 143.2(9) . 5_656 ? C3 C4 Co2 70.3(4) . . ? C4 C4 Co2 133.5(8) 5_656 . ? C3 C4 Co1 67.3(4) . . ? C4 C4 Co1 135.7(7) 5_656 . ? Co2 C4 Co1 78.0(3) . . ? O9 C10O Co2 178.4(7) . . ? O4 C4O Cr3 176.8(9) . . ? O10 C11O Co2 174.4(8) . . ? O8 C9O Co1 178.1(7) . . ? O11 C12O Co2 179.5(9) . . ? O6 C7O Co1 177.0(9) . . ? N1 C6O Cr3 178.5(8) . . ? C2 C1 F1 118.6(8) . . ? C2 C1 N1 126.1(8) . . ? F1 C1 N1 115.3(7) . . ? O7 C8O Co1 177.2(8) . . ? O5 C5O Cr3 179.3(12) . . ? O3 C3O Cr3 175.4(13) . . ? O2 C2O Cr3 177.2(11) . . ? O1 C1O Cr3 176.6(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.564 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.138