# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Valerie Marvaud' _publ_contact_author_email VALERIE.MARVAUD@UPMC.FR _publ_section_title ; Hexacyanidometalate Molecular Chemistry : di, tri, tetra, penta (cis-trans) and heptanuclear Chromium-Copper and Cobalt-Copper complexes. ; loop_ _publ_author_name 'Valerie Marvaud' 'Jean-Louis Cantin' 'Lise-Marie Chamoreau' 'Maria Hernandez-Molina' ; J.Long ; 'Jurgen von Bardeleben' # Attachment 'Co2Cu5.cif' data_jl777c1 _database_code_depnum_ccdc_archive 'CCDC 719593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C52 H120 Co2 Cu5 N32)4+, 4 (Cl O4)-,4 (H2 O)' _chemical_formula_sum 'C52 H128 Cl4 Co2 Cu5 N32 O20' _chemical_formula_weight 2099.22 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.223(6) _cell_length_b 12.263(2) _cell_length_c 28.284(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.020(9) _cell_angle_gamma 90.00 _cell_volume 9371(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 241 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 22.1 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4364 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.781 _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 69094 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 30.01 _reflns_number_total 13591 _reflns_number_gt 8493 _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 ; A model of disorder was introduced for two of the ligands. Bond lenght restraints were introduced on the N22 - C22 - C21 part. Uij's of C23 a and b, on the one hand, and C24 a and b, on the other hand, were constrained to be equal. 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^)+(0.1057P)^2^+32.6718P] 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 0.00037(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13591 _refine_ls_number_parameters 575 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.2039 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.040 _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 0.328752(18) 0.28755(4) 0.172865(17) 0.02156(13) Uani 1 1 d . . . Cu1 Cu 0.2500 0.2500 0.0000 0.03178(18) Uani 1 2 d S . . Cu2 Cu 0.489539(19) 0.24259(5) 0.115630(18) 0.03448(15) Uani 1 1 d . D . Cu3 Cu 0.208823(19) 0.19800(4) 0.289772(18) 0.03141(14) Uani 1 1 d . B . N1 N 0.24687(16) 0.2965(4) 0.08812(15) 0.0485(10) Uani 1 1 d . . . N2 N 0.40481(13) 0.2474(3) 0.10366(13) 0.0360(8) Uani 1 1 d . . . N3 N 0.25567(14) 0.3220(3) 0.24602(13) 0.0353(8) Uani 1 1 d . . . N4 N 0.34463(17) 0.5328(3) 0.16026(15) 0.0495(10) Uani 1 1 d . . . N5 N 0.41227(15) 0.2778(4) 0.25561(14) 0.0462(10) Uani 1 1 d . . . N6 N 0.31027(17) 0.0422(3) 0.18204(16) 0.0479(10) Uani 1 1 d . . . C1 C 0.27692(15) 0.2935(3) 0.12105(14) 0.0294(8) Uani 1 1 d . . . C2 C 0.37529(14) 0.2620(3) 0.12912(13) 0.0265(8) Uani 1 1 d . . . C3 C 0.28326(14) 0.3116(3) 0.21773(14) 0.0264(8) Uani 1 1 d . . . C4 C 0.33892(15) 0.4408(3) 0.16541(14) 0.0297(8) Uani 1 1 d . . . C5 C 0.38095(15) 0.2817(3) 0.22521(14) 0.0297(8) Uani 1 1 d . . . C6 C 0.31833(15) 0.1346(3) 0.17835(14) 0.0301(8) Uani 1 1 d . . . N11 N 0.31928(15) 0.1920(3) 0.00982(14) 0.0429(9) Uani 1 1 d . . . H11A H 0.3334 0.2003 -0.0171 0.051 Uiso 1 1 calc R . . H11B H 0.3372 0.2302 0.0330 0.051 Uiso 1 1 calc R . . N12 N 0.22860(15) 0.0850(3) 0.01047(13) 0.0400(9) Uani 1 1 d . . . C11 C 0.3196(2) 0.0740(5) 0.0232(2) 0.0682(18) Uani 1 1 d . . . H11C H 0.3221 0.0668 0.0575 0.082 Uiso 1 1 calc R . . H11D H 0.3480 0.0383 0.0124 0.082 Uiso 1 1 calc R . . C12 C 0.2725(3) 0.0208(5) 0.0004(2) 0.0665(17) Uani 1 1 d . . . H12A H 0.2730 0.0159 -0.0338 0.080 Uiso 1 1 calc R . . H12B H 0.2702 -0.0526 0.0127 0.080 Uiso 1 1 calc R . . C13 C 0.1848(3) 0.0469(5) -0.0237(2) 0.0701(19) Uani 1 1 d . . . H13A H 0.1899 0.0656 -0.0557 0.105 Uiso 1 1 calc R . . H13B H 0.1552 0.0816 -0.0159 0.105 Uiso 1 1 calc R . . H13C H 0.1814 -0.0308 -0.0212 0.105 Uiso 1 1 calc R . . C14 C 0.2144(3) 0.0633(6) 0.0585(2) 0.081(2) Uani 1 1 d . . . H14A H 0.2003 -0.0083 0.0592 0.121 Uiso 1 1 calc R . . H14B H 0.1906 0.1165 0.0658 0.121 Uiso 1 1 calc R . . H14C H 0.2433 0.0676 0.0816 0.121 Uiso 1 1 calc R . . N21 N 0.15891(16) 0.3116(4) 0.30117(18) 0.0528(11) Uani 1 1 d . B . H21A H 0.1427 0.2909 0.3256 0.063 Uiso 1 1 calc R . . H21B H 0.1745 0.3749 0.3092 0.063 Uiso 1 1 calc R . . N22 N 0.16020(18) 0.1670(4) 0.22599(17) 0.0584(13) Uani 1 1 d D . . N23 N 0.25699(16) 0.0777(3) 0.27945(15) 0.0492(10) Uani 1 1 d . . . H23A H 0.2419 0.0125 0.2803 0.059 Uiso 1 1 calc R B . H23B H 0.2676 0.0854 0.2507 0.059 Uiso 1 1 calc R . . N24 N 0.25314(17) 0.2188(4) 0.35593(16) 0.0498(10) Uani 1 1 d . . . C21 C 0.1221(3) 0.3288(6) 0.2572(3) 0.085(2) Uani 1 1 d D . . H21C H 0.0908 0.2954 0.2622 0.102 Uiso 0.50 1 calc PR A 1 H21D H 0.1164 0.4064 0.2526 0.102 Uiso 0.50 1 calc PR A 1 H21E H 0.1348 0.3782 0.2348 0.102 Uiso 0.50 1 d PR A 2 H21F H 0.0907 0.3560 0.2652 0.102 Uiso 0.50 1 d PR A 2 C22A C 0.1382(4) 0.2845(8) 0.2157(3) 0.044(2) Uani 0.50 1 d PD B 1 H22A H 0.1633 0.3314 0.2049 0.052 Uiso 0.50 1 calc PR B 1 H22B H 0.1106 0.2808 0.1906 0.052 Uiso 0.50 1 calc PR B 1 C23A C 0.1171(5) 0.0988(12) 0.2345(4) 0.073(3) Uani 0.50 1 d P B 1 H23C H 0.0973 0.1372 0.2549 0.109 Uiso 0.50 1 calc PR B 1 H23D H 0.1285 0.0316 0.2494 0.109 Uiso 0.50 1 calc PR B 1 H23E H 0.0975 0.0834 0.2047 0.109 Uiso 0.50 1 calc PR B 1 C24A C 0.1802(13) 0.121(3) 0.1873(12) 0.095(10) Uani 0.50 1 d P B 1 H24A H 0.1971 0.0543 0.1973 0.143 Uiso 0.50 1 calc PR B 1 H24B H 0.2031 0.1709 0.1759 0.143 Uiso 0.50 1 calc PR B 1 H24C H 0.1541 0.1052 0.1623 0.143 Uiso 0.50 1 calc PR B 1 C22B C 0.1175(7) 0.2083(15) 0.2373(7) 0.107(7) Uani 0.50 1 d PD B 2 H22C H 0.1053 0.1618 0.2611 0.128 Uiso 0.50 1 calc PR B 2 H22D H 0.0932 0.2071 0.2092 0.128 Uiso 0.50 1 calc PR B 2 C23B C 0.1588(6) 0.0378(11) 0.2147(5) 0.073(3) Uani 0.50 1 d P B 2 H23F H 0.1454 -0.0004 0.2399 0.109 Uiso 0.50 1 calc PR B 2 H23G H 0.1918 0.0123 0.2124 0.109 Uiso 0.50 1 calc PR B 2 H23H H 0.1384 0.0247 0.1851 0.109 Uiso 0.50 1 calc PR B 2 C24B C 0.1826(13) 0.179(3) 0.1821(12) 0.095(10) Uani 0.50 1 d P B 2 H24D H 0.1612 0.1473 0.1562 0.143 Uiso 0.50 1 calc PR B 2 H24E H 0.2140 0.1420 0.1854 0.143 Uiso 0.50 1 calc PR B 2 H24F H 0.1874 0.2547 0.1759 0.143 Uiso 0.50 1 calc PR B 2 C25 C 0.3002(2) 0.0828(5) 0.3178(2) 0.0652(16) Uani 1 1 d . B . H25A H 0.3160 0.0120 0.3219 0.078 Uiso 1 1 calc R . . H25B H 0.3245 0.1350 0.3093 0.078 Uiso 1 1 calc R . . C26 C 0.2813(2) 0.1167(5) 0.3624(2) 0.0600(15) Uani 1 1 d . B . H26A H 0.2602 0.0597 0.3725 0.072 Uiso 1 1 calc R . . H26B H 0.3089 0.1265 0.3871 0.072 Uiso 1 1 calc R . . C27 C 0.2876(2) 0.3136(5) 0.3558(2) 0.0661(17) Uani 1 1 d . B . H27A H 0.3088 0.3162 0.3855 0.099 Uiso 1 1 calc R . . H27B H 0.2688 0.3799 0.3516 0.099 Uiso 1 1 calc R . . H27C H 0.3074 0.3056 0.3301 0.099 Uiso 1 1 calc R . . C28 C 0.2247(2) 0.2366(6) 0.3968(2) 0.0642(17) Uani 1 1 d . B . H28A H 0.2032 0.1755 0.3997 0.096 Uiso 1 1 calc R . . H28B H 0.2052 0.3018 0.3916 0.096 Uiso 1 1 calc R . . H28C H 0.2472 0.2441 0.4255 0.096 Uiso 1 1 calc R . . N31 N 0.49438(18) 0.1673(5) 0.05275(15) 0.0599(13) Uani 1 1 d . . . H31A H 0.4693 0.1898 0.0312 0.072 Uiso 1 1 calc R . . H31B H 0.5230 0.1865 0.0420 0.072 Uiso 1 1 calc R . . N32 N 0.49359(17) 0.0835(4) 0.14248(15) 0.0512(11) Uani 1 1 d . . . N33 N 0.49340(14) 0.3129(3) 0.18092(13) 0.0408(9) Uani 1 1 d . D . H33A H 0.4675 0.2912 0.1955 0.049 Uiso 1 1 calc R . . H33B H 0.5213 0.2914 0.1989 0.049 Uiso 1 1 calc R . . N34 N 0.50439(17) 0.3993(4) 0.09312(16) 0.0562(12) Uani 1 1 d . . . C31 C 0.4924(3) 0.0469(6) 0.0570(2) 0.0711(18) Uani 1 1 d . . . H31C H 0.5255 0.0170 0.0579 0.085 Uiso 1 1 calc R . . H31D H 0.4722 0.0167 0.0296 0.085 Uiso 1 1 calc R . . C32 C 0.4711(2) 0.0156(5) 0.1017(2) 0.0600(15) Uani 1 1 d . . . H32A H 0.4355 0.0263 0.0972 0.072 Uiso 1 1 calc R . . H32B H 0.4776 -0.0609 0.1086 0.072 Uiso 1 1 calc R . . C33 C 0.5469(2) 0.0561(6) 0.1553(3) 0.081(2) Uani 1 1 d . . . H33C H 0.5502 -0.0203 0.1624 0.121 Uiso 1 1 calc R . . H33D H 0.5601 0.0976 0.1827 0.121 Uiso 1 1 calc R . . H33E H 0.5648 0.0733 0.1291 0.121 Uiso 1 1 calc R . . C34 C 0.4660(3) 0.0617(5) 0.1842(2) 0.0730(19) Uani 1 1 d . . . H34A H 0.4323 0.0848 0.1768 0.109 Uiso 1 1 calc R . . H34B H 0.4813 0.1013 0.2114 0.109 Uiso 1 1 calc R . . H34C H 0.4669 -0.0149 0.1912 0.109 Uiso 1 1 calc R . . C35 C 0.4930(2) 0.4337(5) 0.1767(2) 0.0598(15) Uani 1 1 d . . . H35A H 0.4682 0.4635 0.1949 0.072 Uiso 0.50 1 calc PR C 1 H35B H 0.5250 0.4622 0.1900 0.072 Uiso 0.50 1 calc PR C 1 H35C H 0.5083 0.4660 0.2062 0.072 Uiso 0.50 1 d PR C 2 H35D H 0.4592 0.4597 0.1707 0.072 Uiso 0.50 1 d PR C 2 C36A C 0.4825(5) 0.4685(10) 0.1272(5) 0.061(3) Uani 0.50 1 d P D 1 H36A H 0.4946 0.5424 0.1246 0.073 Uiso 0.50 1 calc PR D 1 H36B H 0.4469 0.4700 0.1186 0.073 Uiso 0.50 1 calc PR D 1 C37A C 0.5602(6) 0.4089(15) 0.1005(8) 0.100(6) Uani 0.50 1 d P D 1 H37A H 0.5694 0.4845 0.1012 0.151 Uiso 0.50 1 calc PR D 1 H37B H 0.5737 0.3732 0.0748 0.151 Uiso 0.50 1 calc PR D 1 H37C H 0.5728 0.3750 0.1301 0.151 Uiso 0.50 1 calc PR D 1 C38A C 0.4850(10) 0.4190(16) 0.0446(6) 0.122(8) Uani 0.50 1 d P D 1 H38A H 0.4572 0.3719 0.0358 0.183 Uiso 0.50 1 calc PR D 1 H38B H 0.5102 0.4046 0.0244 0.183 Uiso 0.50 1 calc PR D 1 H38C H 0.4746 0.4936 0.0410 0.183 Uiso 0.50 1 calc PR D 1 C36B C 0.5207(5) 0.4665(11) 0.1368(4) 0.061(3) Uani 0.50 1 d P D 2 H36C H 0.5559 0.4564 0.1461 0.074 Uiso 0.50 1 calc PR D 2 H36D H 0.5149 0.5431 0.1296 0.074 Uiso 0.50 1 calc PR D 2 C37B C 0.5451(5) 0.4037(13) 0.0611(6) 0.071(4) Uani 0.50 1 d P D 2 H37D H 0.5533 0.4784 0.0556 0.106 Uiso 0.50 1 calc PR D 2 H37E H 0.5339 0.3692 0.0313 0.106 Uiso 0.50 1 calc PR D 2 H37F H 0.5738 0.3665 0.0762 0.106 Uiso 0.50 1 calc PR D 2 C38B C 0.4602(5) 0.4531(11) 0.0658(5) 0.064(3) Uani 0.50 1 d P D 2 H38D H 0.4332 0.4534 0.0847 0.095 Uiso 0.50 1 calc PR D 2 H38E H 0.4507 0.4136 0.0368 0.095 Uiso 0.50 1 calc PR D 2 H38F H 0.4684 0.5268 0.0583 0.095 Uiso 0.50 1 calc PR D 2 Cl1 Cl 0.62363(5) 0.22298(12) -0.00551(6) 0.0575(4) Uani 1 1 d . . . O1 O 0.6213(3) 0.1585(6) -0.0483(2) 0.128(2) Uani 1 1 d . . . O2 O 0.6009(3) 0.1669(7) 0.0287(3) 0.142(3) Uani 1 1 d . . . O3 O 0.6000(3) 0.3229(5) -0.0196(3) 0.128(2) Uani 1 1 d . . . O4 O 0.6730(2) 0.2406(6) 0.0080(3) 0.117(2) Uani 1 1 d . . . Cl2 Cl 0.42667(6) 0.23767(13) -0.07061(5) 0.0576(4) Uani 1 1 d . . . O5 O 0.4059(5) 0.1569(10) -0.0562(9) 0.371(13) Uani 1 1 d . . . O6 O 0.4015(4) 0.3195(9) -0.0587(7) 0.294(10) Uani 1 1 d . . . O7 O 0.4778(3) 0.2389(11) -0.0584(3) 0.212(6) Uani 1 1 d . . . O8 O 0.4298(6) 0.2354(18) -0.1118(4) 0.358(13) Uani 1 1 d . . . O1W O 0.08932(18) 0.2081(4) 0.36469(19) 0.0786(14) Uani 1 1 d . . . O2W O -0.0008(3) 0.2520(8) 0.3141(6) 0.209(5) 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 0.0257(2) 0.0206(2) 0.0180(2) 0.00064(18) 0.00091(18) 0.00014(18) Cu1 0.0379(4) 0.0232(3) 0.0309(4) 0.0018(3) -0.0092(3) 0.0007(3) Cu2 0.0294(3) 0.0501(3) 0.0237(3) -0.0026(2) 0.00206(19) 0.0053(2) Cu3 0.0352(3) 0.0252(3) 0.0317(3) -0.00604(19) -0.0046(2) 0.00148(19) N1 0.044(2) 0.060(3) 0.038(2) 0.0100(19) -0.0098(17) -0.0058(19) N2 0.0296(17) 0.048(2) 0.0302(18) -0.0021(16) 0.0047(14) 0.0042(16) N3 0.0400(19) 0.0297(18) 0.038(2) -0.0022(15) 0.0119(16) -0.0010(15) N4 0.068(3) 0.029(2) 0.049(2) 0.0072(17) -0.001(2) -0.0077(19) N5 0.040(2) 0.061(3) 0.035(2) -0.0001(18) -0.0039(17) 0.0027(19) N6 0.065(3) 0.0250(19) 0.056(3) 0.0022(17) 0.014(2) 0.0012(18) C1 0.0319(19) 0.030(2) 0.0259(19) 0.0014(15) 0.0012(15) -0.0018(16) C2 0.0288(18) 0.030(2) 0.0197(18) -0.0008(14) -0.0030(14) 0.0001(15) C3 0.0332(19) 0.0170(17) 0.0287(19) 0.0023(14) 0.0023(15) -0.0025(14) C4 0.034(2) 0.028(2) 0.027(2) 0.0018(15) 0.0029(15) 0.0004(16) C5 0.033(2) 0.034(2) 0.0213(18) 0.0012(15) 0.0005(15) 0.0016(16) C6 0.036(2) 0.026(2) 0.028(2) -0.0018(15) 0.0043(16) 0.0033(15) N11 0.044(2) 0.046(2) 0.036(2) -0.0026(17) -0.0055(16) 0.0088(18) N12 0.059(2) 0.0308(19) 0.0283(18) 0.0017(15) -0.0031(17) -0.0027(17) C11 0.071(4) 0.043(3) 0.082(4) 0.000(3) -0.025(3) 0.019(3) C12 0.087(4) 0.039(3) 0.068(4) -0.004(3) -0.015(3) 0.010(3) C13 0.097(5) 0.053(4) 0.055(3) 0.007(3) -0.011(3) -0.034(3) C14 0.146(7) 0.053(4) 0.045(3) 0.006(3) 0.018(4) -0.027(4) N21 0.046(2) 0.043(2) 0.070(3) 0.003(2) 0.010(2) -0.0025(19) N22 0.060(3) 0.060(3) 0.051(3) 0.014(2) -0.012(2) -0.020(2) N23 0.064(3) 0.035(2) 0.051(2) -0.0035(18) 0.013(2) -0.0044(19) N24 0.052(2) 0.049(3) 0.046(2) 0.0037(19) -0.0024(19) -0.011(2) C21 0.058(4) 0.062(4) 0.126(7) 0.016(4) -0.027(4) 0.006(3) C22A 0.039(5) 0.051(6) 0.038(5) 0.012(4) -0.009(4) 0.000(4) C23A 0.085(7) 0.068(6) 0.056(5) -0.001(4) -0.027(5) -0.011(5) C24A 0.066(5) 0.16(3) 0.057(8) -0.055(18) 0.003(5) -0.045(17) C22B 0.133(16) 0.087(12) 0.115(14) 0.032(10) 0.075(13) 0.037(11) C23B 0.085(7) 0.068(6) 0.056(5) -0.001(4) -0.027(5) -0.011(5) C24B 0.066(5) 0.16(3) 0.057(8) -0.055(18) 0.003(5) -0.045(17) C25 0.063(4) 0.054(4) 0.074(4) -0.011(3) -0.010(3) 0.017(3) C26 0.051(3) 0.064(4) 0.064(4) -0.016(3) 0.000(3) -0.001(3) C27 0.071(4) 0.052(4) 0.070(4) -0.004(3) -0.015(3) -0.015(3) C28 0.071(4) 0.085(5) 0.035(3) -0.017(3) 0.003(3) -0.017(3) N31 0.053(3) 0.096(4) 0.032(2) -0.007(2) 0.0119(19) 0.006(3) N32 0.057(3) 0.052(3) 0.042(2) -0.0079(19) -0.0033(19) 0.015(2) N33 0.0361(19) 0.054(3) 0.0304(19) -0.0059(17) -0.0024(15) -0.0035(17) N34 0.059(3) 0.065(3) 0.048(3) 0.010(2) 0.017(2) -0.005(2) C31 0.083(4) 0.076(5) 0.052(3) -0.028(3) 0.000(3) 0.006(4) C32 0.064(4) 0.056(4) 0.058(3) -0.014(3) 0.000(3) 0.000(3) C33 0.066(4) 0.066(4) 0.100(5) -0.020(4) -0.031(4) 0.026(3) C34 0.113(6) 0.055(4) 0.052(4) 0.014(3) 0.015(3) 0.017(4) C35 0.077(4) 0.047(3) 0.055(3) -0.010(3) 0.011(3) -0.005(3) C36A 0.064(8) 0.046(6) 0.074(8) 0.005(6) 0.012(6) -0.004(6) C37A 0.080(11) 0.095(13) 0.140(16) -0.020(12) 0.067(12) -0.028(9) C38A 0.22(3) 0.090(14) 0.062(10) 0.047(9) 0.034(13) 0.033(15) C36B 0.067(8) 0.062(8) 0.056(7) 0.003(6) 0.008(6) -0.011(6) C37B 0.064(8) 0.082(10) 0.073(9) 0.015(8) 0.031(7) -0.005(7) C38B 0.075(8) 0.054(8) 0.061(8) 0.017(6) 0.003(6) 0.003(6) Cl1 0.0427(7) 0.0483(7) 0.0826(10) 0.0072(7) 0.0113(6) 0.0063(5) O1 0.168(7) 0.108(5) 0.100(5) -0.017(4) -0.018(4) 0.012(5) O2 0.121(5) 0.145(6) 0.178(7) 0.070(6) 0.092(5) 0.021(5) O3 0.118(5) 0.071(4) 0.193(7) 0.024(4) 0.015(5) 0.045(4) O4 0.068(4) 0.155(7) 0.122(5) 0.009(4) -0.017(3) -0.023(4) Cl2 0.0659(8) 0.0641(9) 0.0427(7) 0.0054(6) 0.0053(6) 0.0174(7) O5 0.233(13) 0.148(10) 0.79(4) 0.113(17) 0.31(2) 0.012(9) O6 0.184(10) 0.130(8) 0.59(3) -0.172(13) 0.149(14) -0.014(7) O7 0.079(5) 0.403(18) 0.152(8) 0.052(9) 0.006(5) 0.045(7) O8 0.253(15) 0.73(4) 0.078(6) 0.042(11) -0.012(8) 0.121(18) O1W 0.077(3) 0.070(3) 0.093(4) 0.001(3) 0.030(3) 0.009(2) O2W 0.080(5) 0.168(9) 0.376(17) 0.008(9) 0.008(8) -0.001(5) _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 C3 1.901(4) . ? Co1 C2 1.902(4) . ? Co1 C6 1.906(4) . ? Co1 C1 1.908(4) . ? Co1 C4 1.915(4) . ? Co1 C5 1.924(4) . ? Cu1 N11 2.003(4) 7 ? Cu1 N11 2.003(4) . ? Cu1 N12 2.136(4) . ? Cu1 N12 2.136(4) 7 ? Cu2 N31 2.022(4) . ? Cu2 N33 2.029(4) . ? Cu2 N34 2.079(5) . ? Cu2 N32 2.092(5) . ? Cu2 N2 2.291(4) . ? Cu3 N21 2.000(4) . ? Cu3 N23 2.019(4) . ? Cu3 N24 2.114(4) . ? Cu3 N22 2.137(4) . ? Cu3 N3 2.420(4) . ? N1 C1 1.163(5) . ? N2 C2 1.157(5) . ? N3 C3 1.170(5) . ? N4 C4 1.151(6) . ? N5 C5 1.136(5) . ? N6 C6 1.161(6) . ? N11 C11 1.495(7) . ? N11 H11A 0.9000 . ? N11 H11B 0.9000 . ? N12 C14 1.480(7) . ? N12 C12 1.487(8) . ? N12 C13 1.516(7) . ? C11 C12 1.513(9) . ? C11 H11C 0.9700 . ? C11 H11D 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N21 C21 1.513(8) . ? N21 H21A 0.9000 . ? N21 H21B 0.9000 . ? N22 C22B 1.344(13) . ? N22 C24A 1.40(3) . ? N22 C24B 1.45(3) . ? N22 C23A 1.485(15) . ? N22 C22A 1.574(10) . ? N22 C23B 1.616(14) . ? N23 C25 1.501(7) . ? N23 H23A 0.9000 . ? N23 H23B 0.9000 . ? N24 C26 1.468(8) . ? N24 C28 1.484(8) . ? N24 C27 1.495(7) . ? C21 C22A 1.413(11) . ? C21 C22B 1.58(2) . ? C21 H21C 0.9700 . ? C21 H21D 0.9700 . ? C21 H21E 0.9700 . ? C21 H21F 0.9700 . ? C22A H21E 1.2783 . ? C22A H22A 0.9700 . ? C22A H22B 0.9700 . ? C23A H23C 0.9600 . ? C23A H23D 0.9600 . ? C23A H23E 0.9600 . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C22B H22C 0.9700 . ? C22B H22D 0.9700 . ? C23B H23F 0.9600 . ? C23B H23G 0.9600 . ? C23B H23H 0.9600 . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? C25 C26 1.478(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N31 C31 1.484(9) . ? N31 H31A 0.9000 . ? N31 H31B 0.9000 . ? N32 C33 1.491(7) . ? N32 C32 1.492(7) . ? N32 C34 1.498(8) . ? N33 C35 1.486(7) . ? N33 H33A 0.9000 . ? N33 H33B 0.9000 . ? N34 C38A 1.429(17) . ? N34 C36A 1.466(13) . ? N34 C38B 1.502(13) . ? N34 C36B 1.506(13) . ? N34 C37A 1.511(17) . ? N34 C37B 1.515(13) . ? C31 C32 1.503(9) . ? C31 H31C 0.9700 . ? C31 H31D 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33C 0.9600 . ? C33 H33D 0.9600 . ? C33 H33E 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36A 1.456(14) . ? C35 C36B 1.488(13) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C35 H35D 0.9700 . ? C36A H36A 0.9700 . ? C36A H36B 0.9700 . ? C37A H37A 0.9600 . ? C37A H37B 0.9600 . ? C37A H37C 0.9600 . ? C38A H38A 0.9600 . ? C38A H38B 0.9600 . ? C38A H38C 0.9600 . ? C36B H36C 0.9700 . ? C36B H36D 0.9700 . ? C37B H37D 0.9600 . ? C37B H37E 0.9600 . ? C37B H37F 0.9600 . ? C38B H38D 0.9600 . ? C38B H38E 0.9600 . ? C38B H38F 0.9600 . ? Cl1 O4 1.370(6) . ? Cl1 O2 1.391(6) . ? Cl1 O3 1.418(6) . ? Cl1 O1 1.440(7) . ? Cl2 O8 1.180(11) . ? Cl2 O5 1.234(10) . ? Cl2 O6 1.283(9) . ? Cl2 O7 1.393(8) . ? 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 Co1 C2 178.67(16) . . ? C3 Co1 C6 89.00(16) . . ? C2 Co1 C6 90.49(17) . . ? C3 Co1 C1 91.48(17) . . ? C2 Co1 C1 89.74(17) . . ? C6 Co1 C1 89.80(17) . . ? C3 Co1 C4 92.07(16) . . ? C2 Co1 C4 88.47(17) . . ? C6 Co1 C4 178.36(17) . . ? C1 Co1 C4 88.93(17) . . ? C3 Co1 C5 88.41(17) . . ? C2 Co1 C5 90.36(16) . . ? C6 Co1 C5 90.22(17) . . ? C1 Co1 C5 179.9(2) . . ? C4 Co1 C5 91.05(17) . . ? N11 Cu1 N11 180.0(2) 7 . ? N11 Cu1 N12 95.02(17) 7 . ? N11 Cu1 N12 84.98(17) . . ? N11 Cu1 N12 84.98(17) 7 7 ? N11 Cu1 N12 95.02(17) . 7 ? N12 Cu1 N12 180.00(19) . 7 ? N31 Cu2 N33 173.04(18) . . ? N31 Cu2 N34 96.7(2) . . ? N33 Cu2 N34 84.01(18) . . ? N31 Cu2 N32 83.5(2) . . ? N33 Cu2 N32 94.10(17) . . ? N34 Cu2 N32 165.81(18) . . ? N31 Cu2 N2 93.12(17) . . ? N33 Cu2 N2 93.60(15) . . ? N34 Cu2 N2 99.27(17) . . ? N32 Cu2 N2 94.88(16) . . ? N21 Cu3 N23 177.17(18) . . ? N21 Cu3 N24 95.7(2) . . ? N23 Cu3 N24 84.58(18) . . ? N21 Cu3 N22 84.1(2) . . ? N23 Cu3 N22 95.4(2) . . ? N24 Cu3 N22 174.92(17) . . ? N21 Cu3 N3 93.17(16) . . ? N23 Cu3 N3 89.61(15) . . ? N24 Cu3 N3 95.60(15) . . ? N22 Cu3 N3 89.49(16) . . ? C2 N2 Cu2 132.5(3) . . ? C3 N3 Cu3 134.7(3) . . ? N1 C1 Co1 177.0(4) . . ? N2 C2 Co1 177.8(3) . . ? N3 C3 Co1 177.2(4) . . ? N4 C4 Co1 179.0(4) . . ? N5 C5 Co1 178.9(4) . . ? N6 C6 Co1 177.5(4) . . ? C11 N11 Cu1 110.8(4) . . ? C11 N11 H11A 109.5 . . ? Cu1 N11 H11A 109.5 . . ? C11 N11 H11B 109.5 . . ? Cu1 N11 H11B 109.5 . . ? H11A N11 H11B 108.1 . . ? C14 N12 C12 112.7(5) . . ? C14 N12 C13 104.9(5) . . ? C12 N12 C13 107.6(4) . . ? C14 N12 Cu1 113.8(3) . . ? C12 N12 Cu1 103.7(3) . . ? C13 N12 Cu1 114.3(3) . . ? N11 C11 C12 109.3(4) . . ? N11 C11 H11C 109.8 . . ? C12 C11 H11C 109.8 . . ? N11 C11 H11D 109.8 . . ? C12 C11 H11D 109.8 . . ? H11C C11 H11D 108.3 . . ? N12 C12 C11 110.4(5) . . ? N12 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N12 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N12 C13 H13A 109.5 . . ? N12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N12 C14 H14A 109.5 . . ? N12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 N21 Cu3 111.1(4) . . ? C21 N21 H21A 109.4 . . ? Cu3 N21 H21A 109.4 . . ? C21 N21 H21B 109.4 . . ? Cu3 N21 H21B 109.4 . . ? H21A N21 H21B 108.0 . . ? C22B N22 C24A 140.4(19) . . ? C22B N22 C24B 129(2) . . ? C24A N22 C24B 30(2) . . ? C22B N22 C23A 56.5(10) . . ? C24A N22 C23A 106.8(10) . . ? C24B N22 C23A 128.0(10) . . ? C22B N22 C22A 51.6(8) . . ? C24A N22 C22A 113.7(17) . . ? C24B N22 C22A 86.6(17) . . ? C23A N22 C22A 104.8(8) . . ? C22B N22 C23B 114.7(11) . . ? C24A N22 C23B 56.6(13) . . ? C24B N22 C23B 86.0(13) . . ? C23A N22 C23B 58.7(8) . . ? C22A N22 C23B 149.6(6) . . ? C22B N22 Cu3 101.3(11) . . ? C24A N22 Cu3 118.1(15) . . ? C24B N22 Cu3 114.9(12) . . ? C23A N22 Cu3 112.6(5) . . ? C22A N22 Cu3 100.1(4) . . ? C23B N22 Cu3 109.8(5) . . ? C25 N23 Cu3 109.3(3) . . ? C25 N23 H23A 109.8 . . ? Cu3 N23 H23A 109.8 . . ? C25 N23 H23B 109.8 . . ? Cu3 N23 H23B 109.8 . . ? H23A N23 H23B 108.3 . . ? C26 N24 C28 110.1(5) . . ? C26 N24 C27 110.1(5) . . ? C28 N24 C27 106.0(5) . . ? C26 N24 Cu3 103.9(3) . . ? C28 N24 Cu3 114.3(3) . . ? C27 N24 Cu3 112.4(4) . . ? C22A C21 N21 112.8(6) . . ? C22A C21 C22B 50.5(7) . . ? N21 C21 C22B 100.3(9) . . ? C22A C21 H21C 109.0 . . ? N21 C21 H21C 109.0 . . ? C22B C21 H21C 67.9 . . ? C22A C21 H21D 109.0 . . ? N21 C21 H21D 109.0 . . ? C22B C21 H21D 149.8 . . ? H21C C21 H21D 107.8 . . ? C22A C21 H21E 61.6 . . ? N21 C21 H21E 111.7 . . ? C22B C21 H21E 111.7 . . ? H21C C21 H21E 138.4 . . ? H21D C21 H21E 50.5 . . ? C22A C21 H21F 134.4 . . ? N21 C21 H21F 111.7 . . ? C22B C21 H21F 111.7 . . ? H21C C21 H21F 45.4 . . ? H21D C21 H21F 64.1 . . ? H21E C21 H21F 109.5 . . ? C21 C22A N22 110.4(7) . . ? C21 C22A H21E 41.9 . . ? N22 C22A H21E 142.2 . . ? C21 C22A H22A 109.6 . . ? N22 C22A H22A 109.6 . . ? H21E C22A H22A 72.0 . . ? C21 C22A H22B 109.6 . . ? N22 C22A H22B 109.6 . . ? H21E C22A H22B 105.2 . . ? H22A C22A H22B 108.1 . . ? N22 C23A H23C 109.5 . . ? N22 C23A H23D 109.5 . . ? H23C C23A H23D 109.5 . . ? N22 C23A H23E 109.5 . . ? H23C C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? N22 C24A H24A 109.5 . . ? N22 C24A H24B 109.5 . . ? N22 C24A H24C 109.5 . . ? N22 C22B C21 113.8(15) . . ? N22 C22B H22C 108.8 . . ? C21 C22B H22C 108.8 . . ? N22 C22B H22D 108.8 . . ? C21 C22B H22D 108.8 . . ? H22C C22B H22D 107.7 . . ? N22 C23B H23F 109.5 . . ? N22 C23B H23G 109.5 . . ? H23F C23B H23G 109.5 . . ? N22 C23B H23H 109.5 . . ? H23F C23B H23H 109.5 . . ? H23G C23B H23H 109.5 . . ? N22 C24B H24D 109.5 . . ? N22 C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? N22 C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C26 C25 N23 107.7(5) . . ? C26 C25 H25A 110.2 . . ? N23 C25 H25A 110.2 . . ? C26 C25 H25B 110.2 . . ? N23 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? N24 C26 C25 111.4(5) . . ? N24 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? N24 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? N24 C27 H27A 109.5 . . ? N24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N24 C28 H28A 109.5 . . ? N24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 N31 Cu2 112.1(4) . . ? C31 N31 H31A 109.2 . . ? Cu2 N31 H31A 109.2 . . ? C31 N31 H31B 109.2 . . ? Cu2 N31 H31B 109.2 . . ? H31A N31 H31B 107.9 . . ? C33 N32 C32 111.0(4) . . ? C33 N32 C34 109.5(5) . . ? C32 N32 C34 108.2(5) . . ? C33 N32 Cu2 107.8(4) . . ? C32 N32 Cu2 104.0(3) . . ? C34 N32 Cu2 116.3(3) . . ? C35 N33 Cu2 110.5(3) . . ? C35 N33 H33A 109.5 . . ? Cu2 N33 H33A 109.5 . . ? C35 N33 H33B 109.5 . . ? Cu2 N33 H33B 109.5 . . ? H33A N33 H33B 108.1 . . ? C38A N34 C36A 113.7(11) . . ? C38A N34 C38B 41.6(9) . . ? C36A N34 C38B 73.7(8) . . ? C38A N34 C36B 137.1(10) . . ? C36A N34 C36B 41.1(7) . . ? C38B N34 C36B 108.6(9) . . ? C38A N34 C37A 111.5(13) . . ? C36A N34 C37A 110.3(10) . . ? C38B N34 C37A 139.9(10) . . ? C36B N34 C37A 69.7(9) . . ? C38A N34 C37B 68.4(11) . . ? C36A N34 C37B 139.3(9) . . ? C38B N34 C37B 106.0(9) . . ? C36B N34 C37B 107.8(9) . . ? C37A N34 C37B 44.3(8) . . ? C38A N34 Cu2 112.8(9) . . ? C36A N34 Cu2 102.9(5) . . ? C38B N34 Cu2 113.0(6) . . ? C36B N34 Cu2 107.7(5) . . ? C37A N34 Cu2 105.0(8) . . ? C37B N34 Cu2 113.6(7) . . ? N31 C31 C32 110.1(5) . . ? N31 C31 H31C 109.6 . . ? C32 C31 H31C 109.6 . . ? N31 C31 H31D 109.6 . . ? C32 C31 H31D 109.6 . . ? H31C C31 H31D 108.2 . . ? N32 C32 C31 110.1(5) . . ? N32 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? N32 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.2 . . ? N32 C33 H33C 109.5 . . ? N32 C33 H33D 109.5 . . ? H33C C33 H33D 109.5 . . ? N32 C33 H33E 109.5 . . ? H33C C33 H33E 109.5 . . ? H33D C33 H33E 109.5 . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36A C35 N33 111.6(6) . . ? C36A C35 C36B 41.5(7) . . ? N33 C35 C36B 109.4(7) . . ? C36A C35 H35A 109.3 . . ? N33 C35 H35A 109.3 . . ? C36B C35 H35A 138.8 . . ? C36A C35 H35B 109.3 . . ? N33 C35 H35B 109.3 . . ? C36B C35 H35B 71.6 . . ? H35A C35 H35B 108.0 . . ? C36A C35 H35C 136.0 . . ? N33 C35 H35C 109.8 . . ? C36B C35 H35C 109.8 . . ? H35A C35 H35C 69.1 . . ? H35B C35 H35C 41.3 . . ? C36A C35 H35D 70.5 . . ? N33 C35 H35D 109.8 . . ? C36B C35 H35D 109.8 . . ? H35A C35 H35D 42.2 . . ? H35B C35 H35D 137.4 . . ? H35C C35 H35D 108.2 . . ? C35 C36A N34 114.5(9) . . ? C35 C36A H35D 38.9 . . ? N34 C36A H35D 140.2 . . ? C35 C36A H36A 108.6 . . ? N34 C36A H36A 108.6 . . ? H35D C36A H36A 108.8 . . ? C35 C36A H36B 108.6 . . ? N34 C36A H36B 108.6 . . ? H35D C36A H36B 71.8 . . ? H36A C36A H36B 107.6 . . ? N34 C37A H37A 109.5 . . ? N34 C37A H37B 109.5 . . ? N34 C37A H37C 109.5 . . ? N34 C38A H38A 109.5 . . ? N34 C38A H38B 109.5 . . ? N34 C38A H38C 109.5 . . ? C35 C36B N34 110.3(9) . . ? C35 C36B H36C 109.6 . . ? N34 C36B H36C 109.6 . . ? C35 C36B H36D 109.6 . . ? N34 C36B H36D 109.6 . . ? H36C C36B H36D 108.1 . . ? N34 C37B H37D 109.5 . . ? N34 C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? N34 C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? N34 C38B H38D 109.5 . . ? N34 C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? N34 C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? O4 Cl1 O2 112.9(5) . . ? O4 Cl1 O3 109.8(5) . . ? O2 Cl1 O3 113.4(4) . . ? O4 Cl1 O1 105.2(5) . . ? O2 Cl1 O1 109.6(5) . . ? O3 Cl1 O1 105.4(5) . . ? O8 Cl2 O5 113.5(15) . . ? O8 Cl2 O6 112.5(13) . . ? O5 Cl2 O6 105.1(9) . . ? O8 Cl2 O7 93.2(9) . . ? O5 Cl2 O7 114.2(10) . . ? O6 Cl2 O7 118.4(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.724 _refine_diff_density_min -1.137 _refine_diff_density_rms 0.139 # Attachment 'CoCu.cif' data_val100 _database_code_depnum_ccdc_archive 'CCDC 719843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H24 Co Cu N10, C24 H20 P, 7(H2 O)' _chemical_formula_sum 'C38 H58 Co Cu N10 O7 P' _chemical_formula_weight 920.38 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1341(8) _cell_length_b 12.7726(13) _cell_length_c 18.652(2) _cell_angle_alpha 73.261(12) _cell_angle_beta 81.953(8) _cell_angle_gamma 85.288(10) _cell_volume 2287.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 124 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 19.4 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22253 _diffrn_reflns_av_R_equivalents 0.1226 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10479 _reflns_number_gt 6081 _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 'SIR-92 (Giacovazzo, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; _diffrn_measured_fraction_theta_max 0.786 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.856 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^)+(0.0000P)^2^+7.1480P] 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 10479 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1440 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Co1 Co 0.28868(6) 0.82237(5) 0.83318(4) 0.02518(17) Uani 1 1 d . . . N1 N 0.0152(4) 0.7659(4) 0.9187(3) 0.0456(12) Uani 1 1 d . . . N2 N 0.1502(5) 0.8907(4) 0.6911(3) 0.0589(14) Uani 1 1 d . . . N3 N 0.2437(5) 1.0522(4) 0.8494(3) 0.0516(13) Uani 1 1 d . . . N4 N 0.5573(4) 0.8832(4) 0.7405(3) 0.0475(12) Uani 1 1 d . . . N5 N 0.4143(5) 0.7532(5) 0.9790(3) 0.0560(14) Uani 1 1 d . . . N6 N 0.3436(5) 0.5929(4) 0.8170(3) 0.0494(12) Uani 1 1 d . . . C1 C 0.1200(5) 0.7854(4) 0.8881(3) 0.0314(11) Uani 1 1 d . . . C2 C 0.2054(5) 0.8653(4) 0.7436(3) 0.0358(12) Uani 1 1 d . . . C3 C 0.2613(5) 0.9660(4) 0.8443(3) 0.0343(11) Uani 1 1 d . . . C4 C 0.4554(5) 0.8601(4) 0.7759(3) 0.0318(11) Uani 1 1 d . . . C5 C 0.3675(5) 0.7788(4) 0.9236(3) 0.0364(12) Uani 1 1 d . . . C6 C 0.3198(4) 0.6788(4) 0.8229(3) 0.0321(11) Uani 1 1 d . . . Cu1 Cu -0.19961(5) 0.78737(5) 0.89394(3) 0.02973(17) Uani 1 1 d . A . N7 N -0.2910(4) 0.7126(3) 0.9952(2) 0.0370(10) Uani 1 1 d . . . H7A H -0.2514 0.7284 1.0309 0.044 Uiso 1 1 calc R . . H7B H -0.3766 0.7378 0.9991 0.044 Uiso 1 1 calc R . . N8 N -0.1966(4) 0.6339(3) 0.8755(3) 0.0379(10) Uani 1 1 d . . . N9 N -0.2330(4) 0.9448(4) 0.9073(3) 0.0408(11) Uani 1 1 d . . . N10 N -0.1612(4) 0.8663(3) 0.7846(2) 0.0398(10) Uani 1 1 d . . . H10A H -0.0813 0.8425 0.7660 0.048 Uiso 1 1 calc R A . H10B H -0.2236 0.8519 0.7592 0.048 Uiso 1 1 calc R . . C7 C -0.2868(7) 0.5930(5) 1.0082(4) 0.0615(18) Uani 1 1 d . . . H7C H -0.2636 0.5570 1.0585 0.074 Uiso 1 1 calc R . . H7D H -0.3742 0.5702 1.0050 0.074 Uiso 1 1 calc R . . C8 C -0.1883(7) 0.5602(5) 0.9522(4) 0.0616(18) Uani 1 1 d . . . H8A H -0.2033 0.4859 0.9527 0.074 Uiso 1 1 calc R . . H8B H -0.0994 0.5611 0.9656 0.074 Uiso 1 1 calc R . . C81 C -0.3208(7) 0.6196(6) 0.8478(5) 0.074(2) Uani 1 1 d . . . H81A H -0.3291 0.5435 0.8525 0.111 Uiso 1 1 calc R . . H81B H -0.3190 0.6609 0.7958 0.111 Uiso 1 1 calc R . . H81C H -0.3954 0.6451 0.8770 0.111 Uiso 1 1 calc R . . C82 C -0.0813(7) 0.6078(6) 0.8249(5) 0.074(2) Uani 1 1 d . . . H82A H -0.0004 0.6232 0.8405 0.111 Uiso 1 1 calc R . . H82B H -0.0885 0.6516 0.7741 0.111 Uiso 1 1 calc R . . H82C H -0.0800 0.5318 0.8270 0.111 Uiso 1 1 calc R . . C9 C -0.1607(8) 0.9854(5) 0.7737(4) 0.071(2) Uani 1 1 d . A . H9A H -0.0710 1.0064 0.7739 0.086 Uiso 0.52(2) 1 calc PR A 1 H9B H -0.1902 1.0243 0.7254 0.086 Uiso 0.52(2) 1 calc PR A 1 H9C H -0.0853 1.0142 0.7371 0.086 Uiso 0.48(2) 1 d PR A 2 H9D H -0.2412 1.0193 0.7525 0.086 Uiso 0.48(2) 1 d PR A 2 C1OA C -0.2480(19) 1.0137(10) 0.8330(8) 0.051(4) Uani 0.48(2) 1 d P A 1 H1O1 H -0.3393 1.0115 0.8237 0.061 Uiso 0.48(2) 1 calc PR A 1 H1O2 H -0.2329 1.0884 0.8314 0.061 Uiso 0.48(2) 1 calc PR A 1 C91A C -0.132(2) 0.9807(17) 0.9429(13) 0.064(5) Uani 0.52(2) 1 d P A 1 H91A H -0.0457 0.9721 0.9165 0.096 Uiso 0.52(2) 1 calc PR A 1 H91B H -0.1350 0.9373 0.9945 0.096 Uiso 0.52(2) 1 calc PR A 1 H91C H -0.1505 1.0563 0.9412 0.096 Uiso 0.52(2) 1 calc PR A 1 C92A C -0.3625(15) 0.9562(15) 0.9589(15) 0.069(5) Uani 0.52(2) 1 d P A 1 H92A H -0.3812 1.0319 0.9568 0.104 Uiso 0.52(2) 1 calc PR A 1 H92B H -0.3523 0.9148 1.0098 0.104 Uiso 0.52(2) 1 calc PR A 1 H92C H -0.4350 0.9291 0.9423 0.104 Uiso 0.52(2) 1 calc PR A 1 C10B C -0.154(2) 1.0146(10) 0.8366(7) 0.056(5) Uani 0.52(2) 1 d P A 2 H10C H -0.1857 1.0903 0.8288 0.068 Uiso 0.52(2) 1 calc PR A 2 H10D H -0.0608 1.0105 0.8451 0.068 Uiso 0.52(2) 1 calc PR A 2 C91B C -0.179(3) 0.957(2) 0.9726(12) 0.092(10) Uani 0.48(2) 1 d P A 2 H91D H -0.0873 0.9304 0.9715 0.138 Uiso 0.48(2) 1 calc PR A 2 H91E H -0.2293 0.9154 1.0179 0.138 Uiso 0.48(2) 1 calc PR A 2 H91F H -0.1840 1.0327 0.9715 0.138 Uiso 0.48(2) 1 calc PR A 2 C92B C -0.3762(16) 0.9782(13) 0.9054(15) 0.063(5) Uani 0.48(2) 1 d P A 2 H92D H -0.3920 1.0484 0.9150 0.094 Uiso 0.48(2) 1 calc PR A 2 H92E H -0.4288 0.9251 0.9433 0.094 Uiso 0.48(2) 1 calc PR A 2 H92F H -0.4006 0.9829 0.8566 0.094 Uiso 0.48(2) 1 calc PR A 2 P1 P 0.25433(12) 0.61361(10) 0.43044(7) 0.0307(3) Uani 1 1 d . . . C11 C 0.2872(5) 0.4901(4) 0.4030(3) 0.0354(12) Uani 1 1 d . . . C12 C 0.1834(6) 0.4197(5) 0.4148(4) 0.0536(16) Uani 1 1 d . . . H12 H 0.0982 0.4392 0.4340 0.064 Uiso 1 1 calc R . . C13 C 0.2071(7) 0.3221(5) 0.3981(4) 0.0624(18) Uani 1 1 d . . . H13 H 0.1387 0.2740 0.4070 0.075 Uiso 1 1 calc R . . C14 C 0.3323(7) 0.2952(5) 0.3682(4) 0.0594(17) Uani 1 1 d . . . H14 H 0.3482 0.2282 0.3576 0.071 Uiso 1 1 calc R . . C15 C 0.4344(6) 0.3653(5) 0.3536(4) 0.0528(16) Uani 1 1 d . . . H15 H 0.5180 0.3469 0.3318 0.063 Uiso 1 1 calc R . . C16 C 0.4123(5) 0.4634(5) 0.3717(3) 0.0419(13) Uani 1 1 d . . . H16 H 0.4812 0.5110 0.3627 0.050 Uiso 1 1 calc R . . C17 C 0.1142(5) 0.6856(4) 0.3857(3) 0.0350(12) Uani 1 1 d . . . C18 C 0.0298(5) 0.7552(5) 0.4172(4) 0.0459(14) Uani 1 1 d . . . H18 H 0.0367 0.7590 0.4656 0.055 Uiso 1 1 calc R . . C19 C -0.0651(6) 0.8193(5) 0.3756(4) 0.0594(18) Uani 1 1 d . . . H19 H -0.1230 0.8658 0.3968 0.071 Uiso 1 1 calc R . . C20 C -0.0754(6) 0.8159(6) 0.3054(4) 0.065(2) Uani 1 1 d . . . H20 H -0.1381 0.8614 0.2778 0.078 Uiso 1 1 calc R . . C21 C 0.0064(6) 0.7453(6) 0.2741(4) 0.0614(18) Uani 1 1 d . . . H21 H -0.0016 0.7422 0.2257 0.074 Uiso 1 1 calc R . . C22 C 0.1009(5) 0.6788(5) 0.3149(4) 0.0518(15) Uani 1 1 d . . . H22 H 0.1552 0.6297 0.2945 0.062 Uiso 1 1 calc R . . C23 C 0.2261(4) 0.5801(4) 0.5315(3) 0.0333(11) Uani 1 1 d . . . C24 C 0.1997(5) 0.6618(5) 0.5677(3) 0.0443(13) Uani 1 1 d . . . H24 H 0.1926 0.7347 0.5397 0.053 Uiso 1 1 calc R . . C25 C 0.1842(6) 0.6341(5) 0.6455(4) 0.0523(16) Uani 1 1 d . . . H25 H 0.1649 0.6887 0.6698 0.063 Uiso 1 1 calc R . . C26 C 0.1969(6) 0.5271(6) 0.6872(3) 0.0523(15) Uani 1 1 d . . . H26 H 0.1851 0.5090 0.7396 0.063 Uiso 1 1 calc R . . C27 C 0.2269(5) 0.4465(5) 0.6513(3) 0.0490(15) Uani 1 1 d . . . H27 H 0.2389 0.3742 0.6796 0.059 Uiso 1 1 calc R . . C28 C 0.2395(5) 0.4717(4) 0.5742(3) 0.0397(12) Uani 1 1 d . . . H28 H 0.2570 0.4164 0.5505 0.048 Uiso 1 1 calc R . . C29 C 0.3916(4) 0.7026(4) 0.3968(3) 0.0323(11) Uani 1 1 d . . . C30 C 0.4684(5) 0.7226(5) 0.4466(4) 0.0468(14) Uani 1 1 d . . . H30 H 0.4552 0.6843 0.4975 0.056 Uiso 1 1 calc R . . C31 C 0.5643(6) 0.7992(5) 0.4209(4) 0.0575(17) Uani 1 1 d . . . H31 H 0.6151 0.8138 0.4544 0.069 Uiso 1 1 calc R . . C32 C 0.5847(6) 0.8539(5) 0.3459(4) 0.0581(18) Uani 1 1 d . . . H32 H 0.6484 0.9068 0.3287 0.070 Uiso 1 1 calc R . . C33 C 0.5125(6) 0.8317(5) 0.2960(4) 0.0544(17) Uani 1 1 d . . . H33 H 0.5289 0.8678 0.2448 0.065 Uiso 1 1 calc R . . C34 C 0.4156(5) 0.7559(5) 0.3213(3) 0.0460(14) Uani 1 1 d . . . H34 H 0.3663 0.7406 0.2873 0.055 Uiso 1 1 calc R . . O1W O 0.9562(5) 0.3082(5) 0.9086(3) 0.0901(17) Uani 1 1 d . . . O2W O 0.7279(7) 1.0086(7) 0.5993(5) 0.145(3) Uani 1 1 d . . . O3W O 0.6949(5) 0.2993(5) 0.8648(3) 0.0836(16) Uani 1 1 d . . . O4W O 0.2218(4) 0.2679(3) 0.8569(3) 0.0549(11) Uani 1 1 d . . . O5W O 0.4469(4) 0.3862(3) 0.8038(3) 0.0663(13) Uani 1 1 d . . . O7W O 0.3658(13) 0.9446(12) 0.5403(8) 0.260(6) Uiso 1 1 d . . . O6W O 0.9823(5) 0.9125(5) 0.5708(3) 0.0937(17) 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 0.0204(3) 0.0245(4) 0.0293(3) -0.0062(3) -0.0023(3) 0.0005(2) N1 0.023(2) 0.054(3) 0.056(3) -0.010(2) -0.002(2) -0.0034(19) N2 0.074(4) 0.053(3) 0.052(3) -0.013(3) -0.027(3) 0.014(3) N3 0.066(3) 0.033(3) 0.057(3) -0.020(3) 0.005(3) -0.002(2) N4 0.037(3) 0.047(3) 0.054(3) -0.015(2) 0.008(2) -0.004(2) N5 0.038(3) 0.083(4) 0.041(3) -0.006(3) -0.010(2) -0.004(2) N6 0.065(3) 0.028(3) 0.055(3) -0.012(2) -0.008(3) 0.003(2) C1 0.026(3) 0.030(3) 0.038(3) -0.007(2) -0.010(2) 0.0001(19) C2 0.037(3) 0.030(3) 0.040(3) -0.010(2) -0.005(2) 0.003(2) C3 0.028(3) 0.040(3) 0.032(3) -0.006(2) 0.001(2) -0.005(2) C4 0.031(3) 0.026(3) 0.037(3) -0.007(2) -0.007(2) 0.002(2) C5 0.027(3) 0.044(3) 0.036(3) -0.009(2) 0.000(2) -0.002(2) C6 0.027(2) 0.031(3) 0.035(3) -0.003(2) -0.007(2) -0.002(2) Cu1 0.0248(3) 0.0293(3) 0.0328(3) -0.0066(3) -0.0007(2) -0.0004(2) N7 0.032(2) 0.040(3) 0.036(2) -0.007(2) -0.0013(19) -0.0018(18) N8 0.036(2) 0.031(2) 0.044(3) -0.010(2) -0.002(2) 0.0040(18) N9 0.040(3) 0.035(3) 0.047(3) -0.013(2) -0.003(2) -0.0026(19) N10 0.041(2) 0.041(3) 0.035(2) -0.006(2) -0.002(2) -0.0039(19) C7 0.085(5) 0.043(4) 0.046(4) 0.001(3) 0.004(3) -0.011(3) C8 0.082(5) 0.034(4) 0.061(4) -0.002(3) -0.013(4) 0.008(3) C81 0.085(5) 0.055(4) 0.099(6) -0.031(4) -0.045(5) -0.004(4) C82 0.077(5) 0.060(5) 0.085(6) -0.037(4) 0.021(4) 0.002(4) C9 0.103(6) 0.035(4) 0.063(5) -0.002(3) 0.015(4) -0.016(4) C1OA 0.048(10) 0.024(7) 0.077(10) -0.002(6) -0.020(8) -0.002(6) C91A 0.077(11) 0.037(11) 0.080(15) -0.009(9) -0.034(10) -0.001(8) C92A 0.049(8) 0.061(11) 0.107(16) -0.041(11) -0.003(10) 0.000(7) C10B 0.080(13) 0.033(7) 0.053(8) -0.005(6) -0.002(8) -0.020(7) C91B 0.21(3) 0.036(11) 0.040(11) -0.009(9) -0.028(13) -0.028(14) C92B 0.056(9) 0.032(8) 0.095(15) -0.019(10) 0.002(10) 0.013(6) P1 0.0278(6) 0.0302(7) 0.0318(7) -0.0062(6) -0.0012(5) -0.0011(5) C11 0.036(3) 0.038(3) 0.031(3) -0.009(2) -0.001(2) 0.001(2) C12 0.049(3) 0.052(4) 0.065(4) -0.029(3) 0.011(3) -0.015(3) C13 0.073(4) 0.053(4) 0.067(5) -0.029(4) 0.008(4) -0.020(3) C14 0.083(5) 0.041(4) 0.057(4) -0.024(3) -0.002(4) 0.006(3) C15 0.053(4) 0.057(4) 0.050(4) -0.027(3) 0.001(3) 0.012(3) C16 0.042(3) 0.046(3) 0.038(3) -0.013(3) 0.000(2) 0.003(2) C17 0.026(2) 0.038(3) 0.036(3) -0.001(2) -0.002(2) -0.004(2) C18 0.034(3) 0.049(4) 0.050(4) -0.009(3) -0.003(3) 0.005(2) C19 0.036(3) 0.052(4) 0.078(5) -0.005(4) -0.003(3) 0.006(3) C20 0.035(3) 0.063(5) 0.075(5) 0.019(4) -0.012(3) -0.004(3) C21 0.047(4) 0.085(5) 0.048(4) -0.004(4) -0.017(3) -0.013(3) C22 0.038(3) 0.065(4) 0.050(4) -0.012(3) -0.008(3) -0.002(3) C23 0.027(2) 0.032(3) 0.039(3) -0.007(2) -0.002(2) -0.002(2) C24 0.052(3) 0.035(3) 0.050(4) -0.017(3) -0.009(3) 0.004(2) C25 0.056(4) 0.066(4) 0.049(4) -0.037(3) -0.010(3) 0.002(3) C26 0.051(4) 0.071(5) 0.035(3) -0.013(3) 0.000(3) -0.015(3) C27 0.049(3) 0.047(4) 0.044(3) 0.003(3) -0.008(3) -0.013(3) C28 0.045(3) 0.031(3) 0.041(3) -0.006(2) -0.004(2) -0.002(2) C29 0.025(2) 0.028(3) 0.041(3) -0.008(2) 0.002(2) -0.0006(19) C30 0.041(3) 0.044(3) 0.052(4) -0.004(3) -0.012(3) -0.008(2) C31 0.039(3) 0.062(4) 0.073(5) -0.015(4) -0.016(3) -0.010(3) C32 0.035(3) 0.036(4) 0.093(6) -0.002(4) -0.006(3) -0.004(2) C33 0.042(3) 0.043(4) 0.061(4) 0.007(3) 0.004(3) -0.002(3) C34 0.042(3) 0.048(4) 0.042(3) -0.004(3) -0.003(3) -0.004(3) O1W 0.082(4) 0.117(5) 0.065(3) -0.023(3) -0.012(3) 0.029(3) O2W 0.116(5) 0.148(7) 0.147(7) -0.021(6) 0.020(5) 0.001(5) O3W 0.084(3) 0.097(4) 0.059(3) -0.010(3) -0.006(3) 0.011(3) O4W 0.062(3) 0.044(2) 0.065(3) -0.027(2) -0.010(2) 0.0047(19) O5W 0.077(3) 0.038(2) 0.084(4) -0.020(2) -0.003(3) -0.003(2) O6W 0.103(4) 0.097(4) 0.086(4) -0.022(3) -0.031(3) -0.013(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 C5 1.885(6) . ? Co1 C1 1.886(5) . ? Co1 C4 1.887(5) . ? Co1 C6 1.894(5) . ? Co1 C2 1.896(6) . ? Co1 C3 1.899(6) . ? N1 C1 1.143(6) . ? N1 Cu1 2.267(4) . ? N2 C2 1.147(7) . ? N3 C3 1.129(6) . ? N4 C4 1.156(6) . ? N5 C5 1.149(7) . ? N6 C6 1.137(6) . ? Cu1 N7 1.989(4) . ? Cu1 N10 1.996(4) . ? Cu1 N8 2.083(4) . ? Cu1 N9 2.091(4) . ? N7 C7 1.474(7) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? N8 C81 1.469(7) . ? N8 C82 1.475(7) . ? N8 C8 1.479(7) . ? N9 C1OA 1.432(14) . ? N9 C91B 1.46(2) . ? N9 C91A 1.46(2) . ? N9 C92B 1.481(17) . ? N9 C10B 1.524(14) . ? N9 C92A 1.539(17) . ? N10 C9 1.476(7) . ? N10 H10A 0.9000 . ? N10 H10B 0.9000 . ? C7 C8 1.469(9) . ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C9 C10B 1.343(15) . ? C9 C1OA 1.429(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C1OA H1O1 0.9700 . ? C1OA H1O2 0.9700 . ? C91A H91A 0.9600 . ? C91A H91B 0.9600 . ? C91A H91C 0.9600 . ? C92A H92A 0.9600 . ? C92A H92B 0.9600 . ? C92A H92C 0.9600 . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C91B H91D 0.9600 . ? C91B H91E 0.9600 . ? C91B H91F 0.9600 . ? C92B H92D 0.9600 . ? C92B H92E 0.9600 . ? C92B H92F 0.9600 . ? P1 C11 1.787(5) . ? P1 C23 1.795(5) . ? P1 C29 1.796(5) . ? P1 C17 1.798(5) . ? C11 C16 1.379(7) . ? C11 C12 1.393(7) . ? C12 C13 1.365(8) . ? C12 H12 0.9300 . ? C13 C14 1.371(9) . ? C13 H13 0.9300 . ? C14 C15 1.371(9) . ? C14 H14 0.9300 . ? C15 C16 1.382(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.374(8) . ? C17 C18 1.379(7) . ? C18 C19 1.383(8) . ? C18 H18 0.9300 . ? C19 C20 1.342(10) . ? C19 H19 0.9300 . ? C20 C21 1.373(10) . ? C20 H20 0.9300 . ? C21 C22 1.385(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.387(7) . ? C23 C28 1.391(7) . ? C24 C25 1.380(8) . ? C24 H24 0.9300 . ? C25 C26 1.370(9) . ? C25 H25 0.9300 . ? C26 C27 1.374(8) . ? C26 H26 0.9300 . ? C27 C28 1.370(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.374(7) . ? C29 C30 1.380(8) . ? C30 C31 1.374(8) . ? C30 H30 0.9300 . ? C31 C32 1.367(9) . ? C31 H31 0.9300 . ? C32 C33 1.363(9) . ? C32 H32 0.9300 . ? C33 C34 1.374(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Co1 C1 90.2(2) . . ? C5 Co1 C4 91.3(2) . . ? C1 Co1 C4 178.5(2) . . ? C5 Co1 C6 89.9(2) . . ? C1 Co1 C6 90.8(2) . . ? C4 Co1 C6 89.1(2) . . ? C5 Co1 C2 178.6(2) . . ? C1 Co1 C2 88.5(2) . . ? C4 Co1 C2 90.1(2) . . ? C6 Co1 C2 90.1(2) . . ? C5 Co1 C3 89.1(2) . . ? C1 Co1 C3 90.0(2) . . ? C4 Co1 C3 90.1(2) . . ? C6 Co1 C3 178.7(2) . . ? C2 Co1 C3 90.9(2) . . ? C1 N1 Cu1 139.6(4) . . ? N1 C1 Co1 176.9(5) . . ? N2 C2 Co1 177.3(5) . . ? N3 C3 Co1 178.4(5) . . ? N4 C4 Co1 179.7(5) . . ? N5 C5 Co1 179.1(5) . . ? N6 C6 Co1 177.3(5) . . ? N7 Cu1 N10 163.48(18) . . ? N7 Cu1 N8 84.17(18) . . ? N10 Cu1 N8 94.09(18) . . ? N7 Cu1 N9 94.96(18) . . ? N10 Cu1 N9 84.16(18) . . ? N8 Cu1 N9 170.92(17) . . ? N7 Cu1 N1 100.15(17) . . ? N10 Cu1 N1 96.34(18) . . ? N8 Cu1 N1 92.96(17) . . ? N9 Cu1 N1 96.10(17) . . ? C7 N7 Cu1 111.5(3) . . ? C7 N7 H7A 109.3 . . ? Cu1 N7 H7A 109.3 . . ? C7 N7 H7B 109.3 . . ? Cu1 N7 H7B 109.3 . . ? H7A N7 H7B 108.0 . . ? C81 N8 C82 109.5(5) . . ? C81 N8 C8 110.8(5) . . ? C82 N8 C8 108.4(5) . . ? C81 N8 Cu1 110.4(3) . . ? C82 N8 Cu1 115.7(4) . . ? C8 N8 Cu1 101.7(4) . . ? C1OA N9 C91B 135.3(12) . . ? C1OA N9 C91A 113.4(13) . . ? C91B N9 C91A 27.3(11) . . ? C1OA N9 C92B 72.5(14) . . ? C91B N9 C92B 114.0(15) . . ? C91A N9 C92B 130.0(12) . . ? C1OA N9 C10B 38.1(6) . . ? C91B N9 C10B 108.0(15) . . ? C91A N9 C10B 81.2(13) . . ? C92B N9 C10B 108.7(14) . . ? C1OA N9 C92A 108.0(14) . . ? C91B N9 C92A 79.5(14) . . ? C91A N9 C92A 102.8(11) . . ? C92B N9 C92A 37.9(8) . . ? C10B N9 C92A 137.8(13) . . ? C1OA N9 Cu1 104.5(6) . . ? C91B N9 Cu1 113.0(11) . . ? C91A N9 Cu1 115.6(9) . . ? C92B N9 Cu1 109.8(7) . . ? C10B N9 Cu1 102.6(6) . . ? C92A N9 Cu1 112.5(7) . . ? C9 N10 Cu1 110.5(4) . . ? C9 N10 H10A 109.5 . . ? Cu1 N10 H10A 109.5 . . ? C9 N10 H10B 109.5 . . ? Cu1 N10 H10B 109.5 . . ? H10A N10 H10B 108.1 . . ? C8 C7 N7 110.6(5) . . ? C8 C7 H7C 109.5 . . ? N7 C7 H7C 109.5 . . ? C8 C7 H7D 109.5 . . ? N7 C7 H7D 109.5 . . ? H7C C7 H7D 108.1 . . ? C7 C8 N8 111.6(5) . . ? C7 C8 H8A 109.3 . . ? N8 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? N8 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N8 C81 H81A 109.5 . . ? N8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N8 C82 H82A 109.5 . . ? N8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C10B C9 C1OA 40.8(7) . . ? C10B C9 N10 114.7(7) . . ? C1OA C9 N10 109.4(7) . . ? C10B C9 H9A 70.3 . . ? C1OA C9 H9A 109.8 . . ? N10 C9 H9A 109.8 . . ? C10B C9 H9B 132.9 . . ? C1OA C9 H9B 109.8 . . ? N10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C10B C9 H9C 108.5 . . ? C1OA C9 H9C 139.4 . . ? N10 C9 H9C 108.5 . . ? H9A C9 H9C 42.2 . . ? H9B C9 H9C 69.4 . . ? C10B C9 H9D 108.7 . . ? C1OA C9 H9D 73.1 . . ? N10 C9 H9D 108.6 . . ? H9A C9 H9D 137.5 . . ? H9B C9 H9D 40.1 . . ? H9C C9 H9D 107.6 . . ? C9 C1OA N9 115.0(10) . . ? C9 C1OA H9D 39.0 . . ? N9 C1OA H9D 145.7 . . ? C9 C1OA H1O1 108.5 . . ? N9 C1OA H1O1 108.5 . . ? H9D C1OA H1O1 74.1 . . ? C9 C1OA H1O2 108.5 . . ? N9 C1OA H1O2 108.5 . . ? H9D C1OA H1O2 102.7 . . ? H1O1 C1OA H1O2 107.5 . . ? N9 C91A H91A 109.5 . . ? N9 C91A H91B 109.5 . . ? N9 C91A H91C 109.5 . . ? N9 C92A H92A 109.5 . . ? N9 C92A H92B 109.5 . . ? N9 C92A H92C 109.5 . . ? C9 C10B N9 114.4(11) . . ? C9 C10B H10C 108.6 . . ? N9 C10B H10C 108.6 . . ? C9 C10B H10D 108.6 . . ? N9 C10B H10D 108.6 . . ? H10C C10B H10D 107.6 . . ? N9 C91B H91D 109.5 . . ? N9 C91B H91E 109.5 . . ? H91D C91B H91E 109.5 . . ? N9 C91B H91F 109.5 . . ? H91D C91B H91F 109.5 . . ? H91E C91B H91F 109.5 . . ? N9 C92B H92D 109.5 . . ? N9 C92B H92E 109.5 . . ? H92D C92B H92E 109.5 . . ? N9 C92B H92F 109.5 . . ? H92D C92B H92F 109.5 . . ? H92E C92B H92F 109.5 . . ? C11 P1 C23 109.0(2) . . ? C11 P1 C29 111.4(2) . . ? C23 P1 C29 109.1(2) . . ? C11 P1 C17 107.8(2) . . ? C23 P1 C17 113.2(2) . . ? C29 P1 C17 106.4(2) . . ? C16 C11 C12 120.2(5) . . ? C16 C11 P1 121.4(4) . . ? C12 C11 P1 118.4(4) . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.5(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 119.5(5) . . ? C11 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C22 C17 C18 120.0(5) . . ? C22 C17 P1 118.1(4) . . ? C18 C17 P1 121.6(4) . . ? C17 C18 C19 118.8(6) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 121.4(6) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 120.2(6) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 119.7(7) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C17 C22 C21 119.8(6) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C28 119.4(5) . . ? C24 C23 P1 120.7(4) . . ? C28 C23 P1 119.7(4) . . ? C25 C24 C23 119.6(6) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 120.6(6) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.6(6) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C23 120.0(5) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C34 C29 C30 119.7(5) . . ? C34 C29 P1 119.5(4) . . ? C30 C29 P1 120.6(4) . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 119.8(6) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.6(6) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 120.0(6) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C29 C34 C33 119.9(6) . . ? C29 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? _diffrn_measured_fraction_theta_max 0.786 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.786 _refine_diff_density_max 0.685 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.107