data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Lescouezec, Rodrigue' _publ_contact_author_email rodrigue.lescouezec@upmc.fr _publ_section_title ; [FeIIlsCoIIIls]2 [FeIIIlsCoIIhs]2 photoinduced conversion in a cyano-bridged heterobimetallic molecular square ; loop_ _publ_author_name 'Julie Mercurol' E.Pardo O.Risset M.Seuleiman Y.Li H.Rousseliare ; R.Lescouezec ; M.Julve data_RLN16 _database_code_depnum_ccdc_archive 'CCDC 781469' #TrackingRef '- RLN16.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H64 B2 Co2 Fe2 N38 O4, 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C66 H68 B2 Cl2 Co2 Fe2 N38 O14' _chemical_formula_weight 1939.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.887(4) _cell_length_b 16.1792(18) _cell_length_c 28.955(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8380(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 252 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 0.839 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 48893 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.70 _reflns_number_total 11526 _reflns_number_gt 7170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Due to the poor diffracting power of the crystal, the diffraction measured fraction of theta is low (94%). Model of disorder was introduced, for two moieties of the molecule : -one, on a cycle of a "B(pz)4" ligand (with Nitrogen atoms N18 and N19 and Carbon atoms C31 to C33), -and another, on the ligand "BIK" (with Nitrogen atoms N16 and N17, Carbon atoms C24 to C26, C29, C30, and Oxygen atom O2). They are disordered over two positions. Moreover, these atoms, and Oxygen atoms of the perchlorate, were refined isotropically and some geometrical restraints were introduced. Thus, because of disorder, Uij's of these Oxygen atoms were constrained and some residual density is located around the perchlorate. 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^)+(0.1346P)^2^+16.3968P] 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 SHELXL _refine_ls_extinction_coef 0.0023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11526 _refine_ls_number_parameters 540 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2480 _refine_ls_wR_factor_gt 0.2188 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.052 _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 Fe1 Fe 0.87939(3) 0.07402(4) 0.415941(18) 0.02434(17) Uani 1 1 d . . . Co1 Co 1.02230(3) 0.19546(3) 0.541286(17) 0.02433(17) Uani 1 1 d . . . O1 O 1.0275(2) 0.3146(3) 0.39843(13) 0.0554(11) Uani 1 1 d . . . N1 N 0.96657(19) 0.1337(2) 0.49856(11) 0.0293(8) Uani 1 1 d . . . N2 N 0.9343(2) -0.0988(2) 0.43471(12) 0.0301(8) Uani 1 1 d . . . N3 N 0.7409(2) 0.0296(3) 0.47252(16) 0.0494(11) Uani 1 1 d . . . N4 N 0.8285(2) 0.0469(2) 0.35577(12) 0.0302(8) Uani 1 1 d . . . N5 N 0.8333(2) 0.0989(2) 0.31836(11) 0.0334(8) Uani 1 1 d . B . N6 N 0.8440(2) 0.1892(2) 0.40916(11) 0.0273(7) Uani 1 1 d . . . N7 N 0.8468(2) 0.2259(2) 0.36693(11) 0.0323(8) Uani 1 1 d . B . N8 N 0.9678(2) 0.1020(2) 0.37678(12) 0.0304(8) Uani 1 1 d . . . N9 N 0.9601(2) 0.1489(2) 0.33764(12) 0.0334(8) Uani 1 1 d . B . N10 N 0.9775(2) 0.2949(2) 0.51782(14) 0.0339(8) Uani 1 1 d . . . N11 N 1.09990(19) 0.2010(2) 0.49465(12) 0.0278(7) Uani 1 1 d . . . N12 N 0.9465(3) 0.3977(3) 0.47104(18) 0.0464(11) Uani 1 1 d . . . N13 N 1.1556(2) 0.2192(3) 0.42734(13) 0.0364(9) Uani 1 1 d . . . N14 N 0.9443(2) 0.1784(2) 0.58728(12) 0.0329(8) Uani 1 1 d D . . N15 N 1.0783(2) 0.2617(2) 0.58433(12) 0.0321(8) Uani 1 1 d . . . N16A N 0.8936(5) 0.1453(6) 0.6526(3) 0.037(2) Uiso 0.60 1 d P A 1 N17A N 1.1180(4) 0.3184(5) 0.6489(2) 0.0362(16) Uiso 0.60 1 d P A 1 C24A C 0.9525(6) 0.1802(6) 0.6320(3) 0.032(2) Uiso 0.60 1 d PD A 1 C25A C 1.0185(5) 0.2117(6) 0.6561(3) 0.0383(19) Uiso 0.60 1 d P A 1 C26A C 1.0700(5) 0.2642(6) 0.6297(3) 0.0306(18) Uiso 0.60 1 d P A 1 C29A C 1.1292(7) 0.3366(7) 0.6984(4) 0.056(2) Uiso 0.60 1 d P A 1 H291 H 1.1618 0.3833 0.7016 0.084 Uiso 0.60 1 calc PR A 1 H292 H 1.1512 0.2895 0.7133 0.084 Uiso 0.60 1 calc PR A 1 H293 H 1.0819 0.3488 0.7125 0.084 Uiso 0.60 1 calc PR A 1 C30A C 0.8805(6) 0.1273(7) 0.7025(4) 0.052(3) Uiso 0.60 1 d P A 1 H301 H 0.8387 0.0905 0.7056 0.078 Uiso 0.60 1 calc PR A 1 H302 H 0.8700 0.1779 0.7186 0.078 Uiso 0.60 1 calc PR A 1 H303 H 0.9243 0.1021 0.7155 0.078 Uiso 0.60 1 calc PR A 1 O2A O 1.0285(4) 0.1970(5) 0.6977(3) 0.0564(17) Uiso 0.60 1 d P A 1 N16B N 0.9058(6) 0.1244(8) 0.6553(4) 0.032(3) Uiso 0.40 1 d PD A 2 N17B N 1.1386(7) 0.2901(8) 0.6496(4) 0.046(3) Uiso 0.40 1 d PD A 2 C24B C 0.9653(8) 0.1611(10) 0.6333(4) 0.031(3) Uiso 0.40 1 d PD A 2 C25B C 1.0376(8) 0.1808(9) 0.6562(4) 0.038(3) Uiso 0.40 1 d P A 2 C26B C 1.0853(8) 0.2381(10) 0.6297(5) 0.037(3) Uiso 0.40 1 d P A 2 C29B C 1.1540(12) 0.2953(13) 0.6995(6) 0.072(5) Uiso 0.40 1 d P A 2 H294 H 1.1078 0.2935 0.7163 0.107 Uiso 0.40 1 calc PR A 2 H295 H 1.1794 0.3462 0.7061 0.107 Uiso 0.40 1 calc PR A 2 H296 H 1.1849 0.2496 0.7086 0.107 Uiso 0.40 1 calc PR A 2 C30B C 0.9020(9) 0.1025(10) 0.7062(5) 0.042(3) Uiso 0.40 1 d P A 2 H304 H 0.9435 0.0676 0.7140 0.064 Uiso 0.40 1 calc PR A 2 H305 H 0.8561 0.0739 0.7124 0.064 Uiso 0.40 1 calc PR A 2 H306 H 0.9041 0.1522 0.7243 0.064 Uiso 0.40 1 calc PR A 2 O2B O 1.0533(6) 0.1579(7) 0.6933(4) 0.055(2) Uiso 0.40 1 d P A 2 C23 C 0.8466(3) 0.1189(4) 0.62099(19) 0.0472(12) Uani 1 1 d D . . H231 H 0.8030 0.0887 0.6256 0.057 Uiso 0.60 1 calc PR A 1 H232 H 0.7980 0.1007 0.6261 0.057 Uiso 0.40 1 d PR A 2 C27 C 1.1595(3) 0.3494(4) 0.61436(18) 0.0509(14) Uani 1 1 d D . . H271 H 1.2001 0.3848 0.6173 0.061 Uiso 0.60 1 calc PR A 1 H272 H 1.1867 0.3978 0.6184 0.061 Uiso 0.40 1 d PR A 2 N18A N 0.8694(5) 0.2297(6) 0.2825(3) 0.029(2) Uiso 0.50 1 d P B 3 N19A N 0.8106(5) 0.2310(6) 0.2548(3) 0.034(2) Uiso 0.50 1 d P B 3 C31A C 0.9140(7) 0.2989(7) 0.2757(4) 0.035(2) Uiso 0.50 1 d P B 3 H311 H 0.9581 0.3117 0.2911 0.042 Uiso 0.50 1 calc PR B 3 C32A C 0.8796(7) 0.3449(7) 0.2417(3) 0.0292(18) Uiso 0.50 1 d P B 3 H321 H 0.8951 0.3949 0.2291 0.035 Uiso 0.50 1 calc PR B 3 C33A C 0.8170(6) 0.2990(6) 0.2307(3) 0.035(2) Uiso 0.50 1 d P B 3 H331 H 0.7826 0.3149 0.2083 0.042 Uiso 0.50 1 calc PR B 3 N18B N 0.8893(5) 0.2421(6) 0.2864(3) 0.030(2) Uiso 0.50 1 d P B 4 N19B N 0.8345(5) 0.2483(6) 0.2539(3) 0.0336(19) Uiso 0.50 1 d P B 4 C31B C 0.9321(7) 0.3121(8) 0.2858(4) 0.042(3) Uiso 0.50 1 d P B 4 H312 H 0.9722 0.3237 0.3052 0.050 Uiso 0.50 1 calc PR B 4 C32B C 0.9056(7) 0.3618(7) 0.2516(4) 0.042(2) Uiso 0.50 1 d P B 4 H322 H 0.9248 0.4126 0.2424 0.050 Uiso 0.50 1 calc PR B 4 C33B C 0.8448(7) 0.3213(7) 0.2336(3) 0.0314(19) Uiso 0.50 1 d P B 4 H332 H 0.8146 0.3422 0.2101 0.038 Uiso 0.50 1 calc PR B 4 C1 C 0.9322(2) 0.1068(3) 0.46823(13) 0.0274(8) Uani 1 1 d . . . C2 C 0.9133(2) -0.0340(3) 0.42530(13) 0.0278(8) Uani 1 1 d . . . C3 C 0.7928(2) 0.0464(3) 0.45140(14) 0.0308(9) Uani 1 1 d . . . C4 C 0.7929(3) -0.0203(3) 0.34141(16) 0.0408(11) Uani 1 1 d . . . H41 H 0.7817 -0.0656 0.3599 0.049 Uiso 1 1 calc R . . C5 C 0.7745(3) -0.0134(4) 0.29466(17) 0.0516(14) Uani 1 1 d . . . H51 H 0.7499 -0.0520 0.2764 0.062 Uiso 1 1 calc R . . C6 C 0.8005(3) 0.0622(4) 0.28166(15) 0.0424(12) Uani 1 1 d . . . H61 H 0.7963 0.0850 0.2523 0.051 Uiso 1 1 calc R . . C7 C 0.8155(2) 0.2444(3) 0.43792(14) 0.0316(9) Uani 1 1 d . . . H71 H 0.8078 0.2357 0.4693 0.038 Uiso 1 1 calc R . . C8 C 0.7984(3) 0.3176(3) 0.41453(16) 0.0384(11) Uani 1 1 d . . . H81 H 0.7771 0.3654 0.4265 0.046 Uiso 1 1 calc R . . C9 C 0.8202(3) 0.3028(3) 0.36974(16) 0.0399(11) Uani 1 1 d . . . H91 H 0.8170 0.3403 0.3454 0.048 Uiso 1 1 calc R . . C10 C 1.0379(3) 0.0733(3) 0.37691(17) 0.0365(10) Uani 1 1 d . . . H101 H 1.0585 0.0405 0.4000 0.044 Uiso 1 1 calc R . . C11 C 1.0757(3) 0.0994(4) 0.33763(19) 0.0467(12) Uani 1 1 d . . . H111 H 1.1246 0.0874 0.3292 0.056 Uiso 1 1 calc R . . C12 C 1.0245(3) 0.1472(3) 0.31379(17) 0.0416(11) Uani 1 1 d . . . H121 H 1.0332 0.1738 0.2858 0.050 Uiso 1 1 calc R . . C13 C 0.9294(3) 0.3457(4) 0.5401(2) 0.0500(13) Uani 1 1 d . . . H131 H 0.9122 0.3386 0.5701 0.060 Uiso 1 1 calc R . . C14 C 0.9103(3) 0.4085(4) 0.5116(3) 0.0589(16) Uani 1 1 d . . . H141 H 0.8779 0.4516 0.5187 0.071 Uiso 1 1 calc R . . C15 C 0.9878(3) 0.3275(3) 0.47540(17) 0.0352(10) Uani 1 1 d . . . C16 C 1.0360(3) 0.2945(3) 0.43899(17) 0.0387(11) Uani 1 1 d . . . C17 C 1.0955(3) 0.2395(3) 0.45360(14) 0.0325(9) Uani 1 1 d . . . C18 C 1.1975(3) 0.1667(3) 0.45179(17) 0.0418(11) Uani 1 1 d . . . H181 H 1.2419 0.1422 0.4422 0.050 Uiso 1 1 calc R . . C19 C 1.1635(3) 0.1556(3) 0.49323(16) 0.0376(10) Uani 1 1 d . . . H191 H 1.1811 0.1221 0.5170 0.045 Uiso 1 1 calc R . . C20 C 1.1763(3) 0.2540(4) 0.38171(17) 0.0499(13) Uani 1 1 d . . . H201 H 1.2223 0.2297 0.3715 0.075 Uiso 1 1 calc R . . H202 H 1.1823 0.3127 0.3843 0.075 Uiso 1 1 calc R . . H203 H 1.1375 0.2420 0.3598 0.075 Uiso 1 1 calc R . . C21 C 0.9456(4) 0.4557(4) 0.4326(3) 0.0649(18) Uani 1 1 d . . . H211 H 0.9158 0.5029 0.4406 0.097 Uiso 1 1 calc R . . H212 H 0.9246 0.4293 0.4059 0.097 Uiso 1 1 calc R . . H213 H 0.9957 0.4732 0.4259 0.097 Uiso 1 1 calc R . . C22 C 0.8753(3) 0.1451(3) 0.58005(18) 0.0399(11) Uani 1 1 d . A . H221 H 0.8516 0.1409 0.5516 0.048 Uiso 1 1 calc R . . C28 C 1.1309(2) 0.3194(3) 0.57448(17) 0.0338(10) Uani 1 1 d . A . H281 H 1.1451 0.3358 0.5450 0.041 Uiso 1 1 calc R . . B1 B 0.8801(3) 0.1768(3) 0.32527(16) 0.0348(11) Uani 1 1 d . . . O3 O 0.6627(4) 0.0900(3) 0.5486(2) 0.111(2) Uani 1 1 d . . . H31 H 0.6879 0.0733 0.5248 0.167 Uiso 1 1 d R . . H32 H 0.6841 0.0586 0.5694 0.167 Uiso 1 1 d R . . Cl1 Cl 0.83580(17) 0.4384(2) 0.65669(8) 0.1247(12) Uani 1 1 d D . . O4 O 0.8293(11) 0.3557(9) 0.6462(6) 0.297(6) Uiso 1 1 d D . . O5 O 0.8793(10) 0.4421(12) 0.6987(7) 0.297(6) Uiso 1 1 d D . . O6 O 0.7733(12) 0.4824(13) 0.6770(7) 0.343(7) Uiso 1 1 d D . . O7 O 0.8714(11) 0.4795(13) 0.6223(6) 0.343(7) Uiso 1 1 d 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 Fe1 0.0274(3) 0.0272(3) 0.0184(3) 0.0017(2) -0.0022(2) -0.0015(2) Co1 0.0245(3) 0.0278(3) 0.0207(2) -0.0009(2) -0.00214(19) 0.0012(2) O1 0.065(3) 0.065(3) 0.0365(19) 0.0153(18) -0.0116(17) 0.002(2) N1 0.0315(18) 0.035(2) 0.0219(15) -0.0006(14) -0.0038(13) 0.0006(15) N2 0.0302(18) 0.033(2) 0.0276(16) 0.0058(15) -0.0047(14) -0.0021(15) N3 0.034(2) 0.057(3) 0.057(3) 0.017(2) 0.012(2) -0.002(2) N4 0.0295(18) 0.037(2) 0.0239(15) 0.0002(14) -0.0034(13) -0.0001(16) N5 0.038(2) 0.043(2) 0.0195(15) -0.0002(14) -0.0016(14) 0.0073(17) N6 0.0316(18) 0.0320(19) 0.0184(14) 0.0027(13) -0.0004(13) -0.0007(15) N7 0.043(2) 0.033(2) 0.0209(15) 0.0061(14) 0.0049(15) 0.0059(17) N8 0.0345(19) 0.033(2) 0.0234(15) 0.0030(14) 0.0008(14) 0.0003(15) N9 0.039(2) 0.037(2) 0.0238(16) 0.0034(15) 0.0054(14) 0.0017(17) N10 0.0315(19) 0.033(2) 0.0374(19) -0.0050(16) -0.0028(15) 0.0058(16) N11 0.0272(17) 0.0309(19) 0.0253(15) 0.0003(14) 0.0001(13) -0.0007(14) N12 0.044(2) 0.029(2) 0.066(3) 0.006(2) -0.010(2) 0.0087(19) N13 0.036(2) 0.042(2) 0.0306(18) -0.0033(16) 0.0063(16) -0.0063(17) N14 0.0315(19) 0.039(2) 0.0285(17) -0.0059(15) 0.0035(15) -0.0046(16) N15 0.0289(18) 0.037(2) 0.0299(17) -0.0033(15) 0.0001(14) -0.0046(16) C23 0.037(3) 0.052(3) 0.052(3) -0.008(2) 0.009(2) -0.008(2) C27 0.044(3) 0.064(4) 0.045(3) -0.016(3) 0.001(2) -0.022(3) C1 0.028(2) 0.029(2) 0.0244(18) 0.0042(15) 0.0020(15) 0.0018(17) C2 0.027(2) 0.035(2) 0.0210(17) 0.0010(16) -0.0029(15) -0.0035(18) C3 0.033(2) 0.030(2) 0.0292(19) 0.0030(16) -0.0050(17) 0.0009(18) C4 0.041(3) 0.050(3) 0.032(2) -0.009(2) -0.0024(19) -0.007(2) C5 0.049(3) 0.074(4) 0.032(2) -0.021(2) -0.005(2) -0.010(3) C6 0.043(3) 0.063(3) 0.0214(19) -0.012(2) -0.0051(18) 0.008(2) C7 0.035(2) 0.036(2) 0.0246(19) -0.0020(17) 0.0013(16) 0.0003(19) C8 0.046(3) 0.035(3) 0.034(2) -0.0014(19) 0.008(2) 0.008(2) C9 0.050(3) 0.037(3) 0.033(2) 0.0082(19) 0.009(2) 0.015(2) C10 0.032(2) 0.040(3) 0.038(2) 0.005(2) -0.0004(18) -0.0010(19) C11 0.039(3) 0.054(3) 0.047(3) 0.002(2) 0.010(2) -0.001(2) C12 0.049(3) 0.040(3) 0.036(2) 0.000(2) 0.015(2) -0.002(2) C13 0.042(3) 0.046(3) 0.062(3) -0.006(3) 0.007(3) 0.011(2) C14 0.046(3) 0.040(3) 0.091(5) -0.005(3) -0.005(3) 0.013(3) C15 0.036(2) 0.027(2) 0.043(2) 0.0040(19) -0.011(2) 0.0041(18) C16 0.039(3) 0.040(3) 0.037(2) 0.009(2) -0.007(2) -0.004(2) C17 0.039(2) 0.035(2) 0.0239(19) 0.0011(16) 0.0008(17) -0.0031(19) C18 0.033(2) 0.052(3) 0.040(2) -0.004(2) 0.008(2) 0.001(2) C19 0.029(2) 0.048(3) 0.036(2) 0.000(2) -0.0009(18) 0.007(2) C20 0.062(3) 0.054(3) 0.034(2) 0.000(2) 0.018(2) -0.012(3) C21 0.068(4) 0.039(3) 0.088(5) 0.019(3) -0.020(4) 0.010(3) C22 0.029(2) 0.048(3) 0.042(2) -0.004(2) 0.0002(19) 0.001(2) C28 0.029(2) 0.031(2) 0.041(2) -0.0050(18) 0.0004(18) -0.0030(18) B1 0.046(3) 0.039(3) 0.0195(19) 0.0032(18) 0.0043(19) 0.014(2) O3 0.165(7) 0.061(3) 0.108(5) -0.028(3) 0.054(5) 0.000(4) Cl1 0.1138(19) 0.199(3) 0.0614(11) -0.0392(15) 0.0185(12) -0.084(2) _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 Fe1 C1 1.861(4) . ? Fe1 C2 1.869(5) . ? Fe1 C3 1.911(5) . ? Fe1 N6 1.977(4) . ? Fe1 N8 1.997(4) . ? Fe1 N4 2.014(3) . ? Co1 N1 1.877(3) . ? Co1 N2 1.879(4) 5_756 ? Co1 N10 1.921(4) . ? Co1 N15 1.925(4) . ? Co1 N11 1.939(3) . ? Co1 N14 1.948(4) . ? O1 C16 1.228(6) . ? N1 C1 1.158(5) . ? N2 C2 1.147(6) . ? N2 Co1 1.879(4) 5_756 ? N3 C3 1.145(6) . ? N4 C4 1.326(6) . ? N4 N5 1.374(5) . ? N5 C6 1.351(6) . ? N5 B1 1.527(7) . ? N6 C7 1.324(5) . ? N6 N7 1.361(4) . ? N7 C9 1.335(6) . ? N7 B1 1.563(6) . ? N8 C10 1.337(6) . ? N8 N9 1.371(5) . ? N9 C12 1.343(6) . ? N9 B1 1.542(7) . ? N10 C15 1.349(6) . ? N10 C13 1.354(6) . ? N11 C17 1.345(5) . ? N11 C19 1.354(6) . ? N12 C14 1.353(8) . ? N12 C15 1.359(6) . ? N12 C21 1.457(7) . ? N13 C18 1.335(7) . ? N13 C17 1.357(6) . ? N13 C20 1.483(6) . ? N14 C24A 1.303(9) . ? N14 C22 1.364(6) . ? N14 C24B 1.413(12) . ? N15 C26A 1.324(8) . ? N15 C28 1.355(6) . ? N15 C26B 1.375(14) . ? N16A C23 1.315(10) . ? N16A C24A 1.337(12) . ? N16A C30A 1.492(13) . ? N17A C27 1.343(9) . ? N17A C26A 1.347(11) . ? N17A C29A 1.476(12) . ? C24A C25A 1.463(13) . ? C25A O2A 1.241(11) . ? C25A C26A 1.468(12) . ? C29A H291 0.9600 . ? C29A H292 0.9600 . ? C29A H293 0.9600 . ? C30A H301 0.9600 . ? C30A H302 0.9600 . ? C30A H303 0.9600 . ? N16B C24B 1.376(18) . ? N16B C23 1.454(11) . ? N16B C30B 1.516(18) . ? N17B C26B 1.396(18) . ? N17B C27 1.449(11) . ? N17B C29B 1.47(2) . ? C24B C25B 1.487(19) . ? C25B O2B 1.171(16) . ? C25B C26B 1.475(19) . ? C29B H294 0.9600 . ? C29B H295 0.9600 . ? C29B H296 0.9600 . ? C30B H304 0.9600 . ? C30B H305 0.9600 . ? C30B H306 0.9600 . ? C23 C22 1.359(7) . ? C23 H231 0.9300 . ? C23 H232 0.9300 . ? C27 C28 1.353(7) . ? C27 H271 0.9300 . ? C27 H272 0.9300 . ? N18A N19A 1.322(13) . ? N18A C31A 1.388(15) . ? N18A B1 1.518(10) . ? N19A C33A 1.309(14) . ? C31A C32A 1.380(15) . ? C31A H311 0.9300 . ? C32A C33A 1.382(14) . ? C32A H321 0.9300 . ? C33A H331 0.9300 . ? N18B N19B 1.363(12) . ? N18B C31B 1.367(16) . ? N18B B1 1.554(10) . ? N19B C33B 1.333(14) . ? C31B C32B 1.359(16) . ? C31B H312 0.9300 . ? C32B C33B 1.374(15) . ? C32B H322 0.9300 . ? C33B H332 0.9300 . ? C4 C5 1.397(7) . ? C4 H41 0.9300 . ? C5 C6 1.361(8) . ? C5 H51 0.9300 . ? C6 H61 0.9300 . ? C7 C8 1.398(7) . ? C7 H71 0.9300 . ? C8 C9 1.375(6) . ? C8 H81 0.9300 . ? C9 H91 0.9300 . ? C10 C11 1.389(7) . ? C10 H101 0.9300 . ? C11 C12 1.382(8) . ? C11 H111 0.9300 . ? C12 H121 0.9300 . ? C13 C14 1.353(9) . ? C13 H131 0.9300 . ? C14 H141 0.9300 . ? C15 C16 1.463(7) . ? C16 C17 1.451(7) . ? C18 C19 1.357(6) . ? C18 H181 0.9300 . ? C19 H191 0.9300 . ? C20 H201 0.9600 . ? C20 H202 0.9600 . ? C20 H203 0.9600 . ? C21 H211 0.9600 . ? C21 H212 0.9600 . ? C21 H213 0.9600 . ? C22 H221 0.9300 . ? C28 H281 0.9300 . ? O3 H31 0.8678 . ? O3 H32 0.8749 . ? Cl1 O7 1.357(15) . ? Cl1 O4 1.376(14) . ? Cl1 O5 1.444(19) . ? Cl1 O6 1.450(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 89.08(17) . . ? C1 Fe1 C3 92.31(18) . . ? C2 Fe1 C3 88.05(19) . . ? C1 Fe1 N6 88.55(16) . . ? C2 Fe1 N6 177.34(15) . . ? C3 Fe1 N6 90.83(17) . . ? C1 Fe1 N8 89.76(16) . . ? C2 Fe1 N8 92.16(17) . . ? C3 Fe1 N8 177.92(16) . . ? N6 Fe1 N8 89.04(15) . . ? C1 Fe1 N4 174.21(17) . . ? C2 Fe1 N4 93.92(16) . . ? C3 Fe1 N4 92.74(16) . . ? N6 Fe1 N4 88.55(15) . . ? N8 Fe1 N4 85.18(15) . . ? N1 Co1 N2 91.18(16) . 5_756 ? N1 Co1 N10 89.49(16) . . ? N2 Co1 N10 179.01(17) 5_756 . ? N1 Co1 N15 178.32(17) . . ? N2 Co1 N15 90.50(16) 5_756 . ? N10 Co1 N15 88.83(17) . . ? N1 Co1 N11 86.88(15) . . ? N2 Co1 N11 89.99(15) 5_756 . ? N10 Co1 N11 90.78(16) . . ? N15 Co1 N11 93.02(15) . . ? N1 Co1 N14 89.72(16) . . ? N2 Co1 N14 85.72(17) 5_756 . ? N10 Co1 N14 93.55(17) . . ? N15 Co1 N14 90.50(16) . . ? N11 Co1 N14 174.48(16) . . ? C1 N1 Co1 169.4(4) . . ? C2 N2 Co1 169.8(3) . 5_756 ? C4 N4 N5 106.5(4) . . ? C4 N4 Fe1 131.8(3) . . ? N5 N4 Fe1 121.4(3) . . ? C6 N5 N4 108.9(4) . . ? C6 N5 B1 134.7(4) . . ? N4 N5 B1 115.8(3) . . ? C7 N6 N7 106.5(3) . . ? C7 N6 Fe1 134.2(3) . . ? N7 N6 Fe1 119.3(3) . . ? C9 N7 N6 109.8(3) . . ? C9 N7 B1 131.1(4) . . ? N6 N7 B1 119.0(4) . . ? C10 N8 N9 106.8(4) . . ? C10 N8 Fe1 131.5(3) . . ? N9 N8 Fe1 121.0(3) . . ? C12 N9 N8 109.1(4) . . ? C12 N9 B1 133.0(4) . . ? N8 N9 B1 116.5(3) . . ? C15 N10 C13 106.4(4) . . ? C15 N10 Co1 126.4(3) . . ? C13 N10 Co1 127.2(4) . . ? C17 N11 C19 105.8(4) . . ? C17 N11 Co1 126.6(3) . . ? C19 N11 Co1 126.7(3) . . ? C14 N12 C15 106.7(5) . . ? C14 N12 C21 125.1(5) . . ? C15 N12 C21 128.0(5) . . ? C18 N13 C17 107.6(4) . . ? C18 N13 C20 125.0(4) . . ? C17 N13 C20 127.2(4) . . ? C24A N14 C22 105.2(5) . . ? C22 N14 C24B 107.8(7) . . ? C24A N14 Co1 126.6(5) . . ? C22 N14 Co1 126.8(3) . . ? C24B N14 Co1 118.9(6) . . ? C26A N15 C28 105.4(5) . . ? C28 N15 C26B 109.3(7) . . ? C26A N15 Co1 127.0(4) . . ? C28 N15 Co1 127.5(3) . . ? C26B N15 Co1 120.7(6) . . ? C23 N16A C24A 109.2(7) . . ? C23 N16A C30A 120.7(8) . . ? C24A N16A C30A 129.8(8) . . ? C27 N17A C26A 106.7(6) . . ? C27 N17A C29A 125.0(7) . . ? C26A N17A C29A 128.1(8) . . ? N14 C24A N16A 110.3(8) . . ? N14 C24A C25A 124.9(8) . . ? N16A C24A C25A 124.7(8) . . ? O2A C25A C24A 120.9(8) . . ? O2A C25A C26A 121.7(8) . . ? C24A C25A C26A 117.4(8) . . ? N15 C26A N17A 111.0(7) . . ? N15 C26A C25A 124.7(7) . . ? N17A C26A C25A 124.2(7) . . ? C24B N16B C23 105.8(9) . . ? C24B N16B C30B 125.8(11) . . ? C23 N16B C30B 128.1(10) . . ? C26B N17B C27 106.6(10) . . ? C26B N17B C29B 124.5(13) . . ? C27 N17B C29B 127.2(12) . . ? N16B C24B N14 108.5(10) . . ? N16B C24B C25B 123.9(10) . . ? N14 C24B C25B 127.5(11) . . ? O2B C25B C26B 122.5(13) . . ? O2B C25B C24B 123.4(13) . . ? C26B C25B C24B 113.9(11) . . ? N15 C26B N17B 106.7(10) . . ? N15 C26B C25B 128.3(11) . . ? N17B C26B C25B 124.0(12) . . ? N17B C29B H294 109.5 . . ? N17B C29B H295 109.5 . . ? H294 C29B H295 109.5 . . ? N17B C29B H296 109.5 . . ? H294 C29B H296 109.5 . . ? H295 C29B H296 109.5 . . ? N16B C30B H304 109.5 . . ? N16B C30B H305 109.5 . . ? H304 C30B H305 109.5 . . ? N16B C30B H306 109.5 . . ? H304 C30B H306 109.5 . . ? H305 C30B H306 109.5 . . ? N16A C23 C22 105.4(6) . . ? C22 C23 N16B 107.6(6) . . ? N16A C23 H231 127.3 . . ? C22 C23 H231 127.3 . . ? N16B C23 H231 122.9 . . ? N16A C23 H232 126.1 . . ? C22 C23 H232 126.3 . . ? N16B C23 H232 126.1 . . ? N17A C27 C28 107.1(5) . . ? C28 C27 N17B 105.4(6) . . ? N17A C27 H271 126.5 . . ? C28 C27 H271 126.5 . . ? N17B C27 H271 123.0 . . ? N17A C27 H272 120.7 . . ? C28 C27 H272 127.3 . . ? N17B C27 H272 127.2 . . ? N19A N18A C31A 111.0(9) . . ? N19A N18A B1 127.2(8) . . ? C31A N18A B1 119.8(9) . . ? C33A N19A N18A 105.5(10) . . ? C32A C31A N18A 106.3(10) . . ? C32A C31A H311 126.9 . . ? N18A C31A H311 126.9 . . ? C31A C32A C33A 103.6(9) . . ? C31A C32A H321 128.2 . . ? C33A C32A H321 128.2 . . ? N19A C33A C32A 113.5(9) . . ? N19A C33A H331 123.2 . . ? C32A C33A H331 123.2 . . ? N19B N18B C31B 109.5(10) . . ? N19B N18B B1 118.3(8) . . ? C31B N18B B1 129.2(9) . . ? C33B N19B N18B 105.7(9) . . ? C32B C31B N18B 107.7(12) . . ? C32B C31B H312 126.2 . . ? N18B C31B H312 126.2 . . ? C31B C32B C33B 105.8(11) . . ? C31B C32B H322 127.1 . . ? C33B C32B H322 127.1 . . ? N19B C33B C32B 111.3(9) . . ? N19B C33B H332 124.4 . . ? C32B C33B H332 124.4 . . ? N1 C1 Fe1 173.7(4) . . ? N2 C2 Fe1 174.6(4) . . ? N3 C3 Fe1 179.7(5) . . ? N4 C4 C5 110.6(5) . . ? N4 C4 H41 124.7 . . ? C5 C4 H41 124.7 . . ? C6 C5 C4 105.0(4) . . ? C6 C5 H51 127.5 . . ? C4 C5 H51 127.5 . . ? N5 C6 C5 109.0(4) . . ? N5 C6 H61 125.5 . . ? C5 C6 H61 125.5 . . ? N6 C7 C8 110.6(4) . . ? N6 C7 H71 124.7 . . ? C8 C7 H71 124.7 . . ? C9 C8 C7 104.3(4) . . ? C9 C8 H81 127.8 . . ? C7 C8 H81 127.8 . . ? N7 C9 C8 108.7(4) . . ? N7 C9 H91 125.7 . . ? C8 C9 H91 125.7 . . ? N8 C10 C11 110.4(4) . . ? N8 C10 H101 124.8 . . ? C11 C10 H101 124.8 . . ? C12 C11 C10 104.9(4) . . ? C12 C11 H111 127.5 . . ? C10 C11 H111 127.5 . . ? N9 C12 C11 108.8(4) . . ? N9 C12 H121 125.6 . . ? C11 C12 H121 125.6 . . ? C14 C13 N10 109.1(5) . . ? C14 C13 H131 125.5 . . ? N10 C13 H131 125.5 . . ? C13 C14 N12 108.1(5) . . ? C13 C14 H141 125.9 . . ? N12 C14 H141 125.9 . . ? N10 C15 N12 109.7(4) . . ? N10 C15 C16 126.4(4) . . ? N12 C15 C16 123.9(5) . . ? O1 C16 C17 122.2(5) . . ? O1 C16 C15 121.3(5) . . ? C17 C16 C15 116.5(4) . . ? N11 C17 N13 109.7(4) . . ? N11 C17 C16 125.8(4) . . ? N13 C17 C16 124.5(4) . . ? N13 C18 C19 107.5(4) . . ? N13 C18 H181 126.2 . . ? C19 C18 H181 126.2 . . ? N11 C19 C18 109.4(4) . . ? N11 C19 H191 125.3 . . ? C18 C19 H191 125.3 . . ? N13 C20 H201 109.5 . . ? N13 C20 H202 109.5 . . ? H201 C20 H202 109.5 . . ? N13 C20 H203 109.5 . . ? H201 C20 H203 109.5 . . ? H202 C20 H203 109.5 . . ? N12 C21 H211 109.5 . . ? N12 C21 H212 109.5 . . ? H211 C21 H212 109.5 . . ? N12 C21 H213 109.5 . . ? H211 C21 H213 109.5 . . ? H212 C21 H213 109.5 . . ? C23 C22 N14 109.4(4) . . ? C23 C22 H221 125.3 . . ? N14 C22 H221 125.3 . . ? C27 C28 N15 109.2(4) . . ? C27 C28 H281 125.4 . . ? N15 C28 H281 125.4 . . ? N18A B1 N5 106.8(5) . . ? N18A B1 N9 118.2(5) . . ? N5 B1 N9 107.4(4) . . ? N5 B1 N18B 121.6(5) . . ? N9 B1 N18B 105.6(5) . . ? N18A B1 N7 107.1(5) . . ? N5 B1 N7 108.2(4) . . ? N9 B1 N7 108.9(4) . . ? N18B B1 N7 104.7(5) . . ? H31 O3 H32 97.8 . . ? O7 Cl1 O4 110.7(12) . . ? O7 Cl1 O5 110.2(11) . . ? O4 Cl1 O5 105.8(11) . . ? O7 Cl1 O6 114.8(13) . . ? O4 Cl1 O6 120.1(12) . . ? O5 Cl1 O6 93.1(10) . . ? _diffrn_reflns_theta_max 30.02 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.570 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.143