# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name S.Brooker _publ_contact_author_name 'Sally Brooker' _publ_contact_author_email Sbrooker@chemistry.otago.ac.nz data_mgc460_0m _database_code_depnum_ccdc_archive 'CCDC 808581' #TrackingRef 'MGC 460 final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H11 Cu N4 O4, B F4, H2 O' _chemical_formula_sum 'C11 H13 B Cu F4 N4 O5' _chemical_formula_weight 431.60 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' O O 0.0106 0.0060 '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' F F 0.0171 0.0103 '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' _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 8.1077(5) _cell_length_b 9.3487(6) _cell_length_c 11.2246(7) _cell_angle_alpha 92.472(4) _cell_angle_beta 92.302(3) _cell_angle_gamma 110.049(3) _cell_volume 797.11(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 4057 _cell_measurement_theta_min 2.323 _cell_measurement_theta_max 26.1555 _exptl_crystal_description 'irregular block' _exptl_crystal_colour blue _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 434 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6761 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SCALE(Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16738 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26.42 _reflns_number_total 3258 _reflns_number_gt 2783 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. {[Cu(C11H7N4O2)(H2O)2](BF4)(H2O)} All non-H ANIS. All H calc and ride except for H's on water whose coordinates were freely refined. H's were involved in numerous hydrogen bonding. Short carbonyl-carbonyl contacts were observed. The suggested H-bond O3-F2 is too long and at a bad angle, therefore was not included. ; _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^)+(0.0259P)^2^+0.8965P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3258 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Cu1 Cu 0.58859(4) 0.74470(4) 0.74504(3) 0.02150(11) Uani 1 1 d . . . O3 O 0.5606(3) 0.8154(2) 0.90723(18) 0.0262(5) Uani 1 1 d . . . H3X H 0.517(4) 0.751(4) 0.964(3) 0.031 Uiso 1 1 d . . . H3Y H 0.646(4) 0.885(4) 0.930(3) 0.031 Uiso 1 1 d . . . O4 O 0.3941(3) 0.5029(2) 0.77683(18) 0.0256(5) Uani 1 1 d . . . H4X H 0.293(4) 0.504(4) 0.790(3) 0.031 Uiso 1 1 d . . . H4Y H 0.390(4) 0.456(4) 0.719(3) 0.031 Uiso 1 1 d . . . N1 N 0.7955(3) 0.6760(3) 0.7774(2) 0.0218(5) Uani 1 1 d . . . C1 C 0.8846(4) 0.6782(3) 0.8802(2) 0.0247(6) Uani 1 1 d . . . H1 H 0.8508 0.7154 0.9519 0.030 Uiso 1 1 calc R . . C2 C 1.0264(4) 0.6269(3) 0.8839(3) 0.0257(6) Uani 1 1 d . . . H2 H 1.0901 0.6332 0.9580 0.031 Uiso 1 1 calc R . . N2 N 1.0762(3) 0.5687(3) 0.7862(2) 0.0259(5) Uani 1 1 d . . . C3 C 0.9836(4) 0.5652(3) 0.6829(2) 0.0240(6) Uani 1 1 d . . . H3 H 1.0134 0.5229 0.6120 0.029 Uiso 1 1 calc R . . C4 C 0.8465(3) 0.6214(3) 0.6772(2) 0.0204(6) Uani 1 1 d . . . C5 C 0.7496(3) 0.6288(3) 0.5620(2) 0.0212(6) Uani 1 1 d . . . O1 O 0.7885(2) 0.5825(2) 0.46741(17) 0.0270(5) Uani 1 1 d . . . N3 N 0.6248(3) 0.6930(2) 0.58140(19) 0.0200(5) Uani 1 1 d . . . C6 C 0.5151(4) 0.7152(3) 0.4946(2) 0.0220(6) Uani 1 1 d . . . O2 O 0.5024(2) 0.6781(2) 0.38763(16) 0.0254(4) Uani 1 1 d . . . C7 C 0.3996(3) 0.7971(3) 0.5453(2) 0.0213(6) Uani 1 1 d . . . C8 C 0.2846(4) 0.8397(3) 0.4737(3) 0.0271(6) Uani 1 1 d . . . H8 H 0.2702 0.8129 0.3904 0.032 Uiso 1 1 calc R . . C9 C 0.1900(4) 0.9227(3) 0.5255(3) 0.0294(7) Uani 1 1 d . . . H9 H 0.1091 0.9528 0.4782 0.035 Uiso 1 1 calc R . . C10 C 0.2156(4) 0.9609(3) 0.6468(3) 0.0281(6) Uani 1 1 d . . . H10 H 0.1548 1.0201 0.6835 0.034 Uiso 1 1 calc R . . C11 C 0.3302(4) 0.9122(3) 0.7141(3) 0.0266(6) Uani 1 1 d . . . H11 H 0.3451 0.9365 0.7978 0.032 Uiso 1 1 calc R . . N4 N 0.4212(3) 0.8314(3) 0.6645(2) 0.0233(5) Uani 1 1 d . . . B1 B 0.8925(4) 0.1318(4) 0.8427(3) 0.0254(7) Uani 1 1 d . . . F1 F 1.0722(2) 0.2007(2) 0.84682(16) 0.0422(5) Uani 1 1 d . . . F2 F 0.8378(2) 0.01348(18) 0.75365(14) 0.0312(4) Uani 1 1 d . . . F3 F 0.8386(2) 0.0719(2) 0.95349(15) 0.0387(5) Uani 1 1 d . . . F4 F 0.8115(3) 0.2384(2) 0.81886(16) 0.0406(5) Uani 1 1 d . . . O21 O 0.4304(3) 0.6399(3) 0.0777(2) 0.0331(5) Uani 1 1 d . . . H21X H 0.493(5) 0.603(4) 0.118(3) 0.040 Uiso 1 1 d . . . H21Y H 0.377(5) 0.675(4) 0.116(3) 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02260(19) 0.0251(2) 0.01606(18) -0.00115(13) -0.00023(13) 0.00767(14) O3 0.0281(11) 0.0263(11) 0.0195(10) -0.0003(9) 0.0025(9) 0.0032(9) O4 0.0218(10) 0.0324(12) 0.0202(10) -0.0037(9) 0.0010(9) 0.0071(9) N1 0.0205(12) 0.0210(12) 0.0204(12) -0.0018(9) -0.0009(9) 0.0031(9) C1 0.0246(15) 0.0281(15) 0.0180(14) -0.0021(11) -0.0018(11) 0.0056(12) C2 0.0226(15) 0.0264(15) 0.0232(15) 0.0024(12) -0.0029(12) 0.0024(12) N2 0.0224(12) 0.0246(13) 0.0271(13) 0.0018(10) -0.0021(10) 0.0042(10) C3 0.0248(15) 0.0225(14) 0.0223(15) -0.0012(11) 0.0023(11) 0.0052(12) C4 0.0191(13) 0.0174(13) 0.0205(14) -0.0008(11) 0.0021(11) 0.0009(11) C5 0.0207(14) 0.0181(13) 0.0203(14) -0.0009(11) 0.0000(11) 0.0011(11) O1 0.0266(11) 0.0353(12) 0.0200(10) -0.0040(9) 0.0017(8) 0.0126(9) N3 0.0202(11) 0.0210(12) 0.0181(11) -0.0011(9) -0.0005(9) 0.0066(9) C6 0.0228(14) 0.0181(13) 0.0214(14) 0.0020(11) 0.0013(11) 0.0022(11) O2 0.0291(11) 0.0270(11) 0.0184(10) -0.0010(8) -0.0012(8) 0.0082(9) C7 0.0214(14) 0.0189(13) 0.0197(14) -0.0001(11) 0.0008(11) 0.0021(11) C8 0.0290(16) 0.0262(15) 0.0232(15) 0.0035(12) -0.0001(12) 0.0058(12) C9 0.0285(16) 0.0308(16) 0.0291(16) 0.0055(13) -0.0020(12) 0.0106(13) C10 0.0271(15) 0.0288(16) 0.0308(16) 0.0037(13) 0.0052(13) 0.0120(13) C11 0.0277(15) 0.0239(15) 0.0256(15) -0.0022(12) 0.0041(12) 0.0057(12) N4 0.0249(12) 0.0217(12) 0.0210(12) 0.0000(10) -0.0001(10) 0.0055(10) B1 0.0278(17) 0.0284(17) 0.0171(15) -0.0009(13) -0.0025(13) 0.0065(14) F1 0.0299(10) 0.0536(12) 0.0326(10) -0.0043(9) -0.0022(8) 0.0020(9) F2 0.0399(10) 0.0260(9) 0.0242(9) -0.0027(7) -0.0025(7) 0.0080(8) F3 0.0466(11) 0.0344(10) 0.0224(9) -0.0002(8) -0.0030(8) -0.0018(8) F4 0.0539(12) 0.0409(11) 0.0346(10) -0.0013(8) 0.0013(9) 0.0265(9) O21 0.0366(13) 0.0403(14) 0.0268(12) 0.0073(10) 0.0052(10) 0.0181(10) _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 Cu1 N3 1.939(2) . ? Cu1 O3 1.958(2) . ? Cu1 N4 2.008(2) . ? Cu1 N1 2.017(2) . ? Cu1 O4 2.323(2) . ? O3 H3X 0.89(3) . ? O3 H3Y 0.79(3) . ? O4 H4X 0.85(3) . ? O4 H4Y 0.76(3) . ? N1 C1 1.332(3) . ? N1 C4 1.352(3) . ? C1 C2 1.389(4) . ? C1 H1 0.9500 . ? C2 N2 1.341(4) . ? C2 H2 0.9500 . ? N2 C3 1.348(4) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.502(4) . ? C5 O1 1.223(3) . ? C5 N3 1.361(3) . ? N3 C6 1.363(4) . ? C6 O2 1.226(3) . ? C6 C7 1.512(4) . ? C7 N4 1.353(3) . ? C7 C8 1.377(4) . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C10 1.382(4) . ? C9 H9 0.9500 . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C11 N4 1.344(4) . ? C11 H11 0.9500 . ? B1 F1 1.374(4) . ? B1 F2 1.397(3) . ? B1 F4 1.398(4) . ? B1 F3 1.410(4) . ? O21 H21X 0.84(4) . ? O21 H21Y 0.76(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 N3 Cu1 O3 175.07(9) . . ? N3 Cu1 N4 82.34(9) . . ? O3 Cu1 N4 95.51(9) . . ? N3 Cu1 N1 81.84(9) . . ? O3 Cu1 N1 99.53(9) . . ? N4 Cu1 N1 161.74(9) . . ? N3 Cu1 O4 94.49(8) . . ? O3 Cu1 O4 90.24(8) . . ? N4 Cu1 O4 99.46(9) . . ? N1 Cu1 O4 90.81(8) . . ? Cu1 O3 H3X 122(2) . . ? Cu1 O3 H3Y 110(2) . . ? H3X O3 H3Y 113(3) . . ? Cu1 O4 H4X 112(2) . . ? Cu1 O4 H4Y 105(3) . . ? H4X O4 H4Y 110(3) . . ? C1 N1 C4 118.0(2) . . ? C1 N1 Cu1 129.49(19) . . ? C4 N1 Cu1 112.51(18) . . ? N1 C1 C2 120.9(3) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? N2 C2 C1 122.0(3) . . ? N2 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 N2 C3 116.5(2) . . ? N2 C3 C4 122.0(3) . . ? N2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? N1 C4 C3 120.5(3) . . ? N1 C4 C5 116.5(2) . . ? C3 C4 C5 122.9(2) . . ? O1 C5 N3 128.6(3) . . ? O1 C5 C4 120.5(3) . . ? N3 C5 C4 110.8(2) . . ? C5 N3 C6 124.8(2) . . ? C5 N3 Cu1 118.02(18) . . ? C6 N3 Cu1 117.05(18) . . ? O2 C6 N3 128.5(3) . . ? O2 C6 C7 120.1(3) . . ? N3 C6 C7 111.3(2) . . ? N4 C7 C8 122.1(3) . . ? N4 C7 C6 115.9(2) . . ? C8 C7 C6 122.0(2) . . ? C7 C8 C9 118.9(3) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 118.9(3) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? N4 C11 C10 121.8(3) . . ? N4 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 N4 C7 118.9(2) . . ? C11 N4 Cu1 128.6(2) . . ? C7 N4 Cu1 112.58(18) . . ? F1 B1 F2 110.3(2) . . ? F1 B1 F4 110.0(3) . . ? F2 B1 F4 109.2(2) . . ? F1 B1 F3 110.2(2) . . ? F2 B1 F3 109.0(2) . . ? F4 B1 F3 108.1(2) . . ? H21X O21 H21Y 113(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N1 C1 175.6(3) . . . . ? O3 Cu1 N1 C1 0.4(3) . . . . ? N4 Cu1 N1 C1 145.4(3) . . . . ? O4 Cu1 N1 C1 -90.0(2) . . . . ? N3 Cu1 N1 C4 -4.09(18) . . . . ? O3 Cu1 N1 C4 -179.29(18) . . . . ? N4 Cu1 N1 C4 -34.2(4) . . . . ? O4 Cu1 N1 C4 90.33(18) . . . . ? C4 N1 C1 C2 0.4(4) . . . . ? Cu1 N1 C1 C2 -179.2(2) . . . . ? N1 C1 C2 N2 -2.2(4) . . . . ? C1 C2 N2 C3 1.3(4) . . . . ? C2 N2 C3 C4 1.2(4) . . . . ? C1 N1 C4 C3 2.1(4) . . . . ? Cu1 N1 C4 C3 -178.2(2) . . . . ? C1 N1 C4 C5 -176.7(2) . . . . ? Cu1 N1 C4 C5 3.0(3) . . . . ? N2 C3 C4 N1 -3.0(4) . . . . ? N2 C3 C4 C5 175.6(2) . . . . ? N1 C4 C5 O1 179.6(2) . . . . ? C3 C4 C5 O1 0.9(4) . . . . ? N1 C4 C5 N3 0.5(3) . . . . ? C3 C4 C5 N3 -178.1(2) . . . . ? O1 C5 N3 C6 1.2(4) . . . . ? C4 C5 N3 C6 -179.8(2) . . . . ? O1 C5 N3 Cu1 176.8(2) . . . . ? C4 C5 N3 Cu1 -4.2(3) . . . . ? O3 Cu1 N3 C5 111.2(10) . . . . ? N4 Cu1 N3 C5 175.6(2) . . . . ? N1 Cu1 N3 C5 4.70(19) . . . . ? O4 Cu1 N3 C5 -85.48(19) . . . . ? O3 Cu1 N3 C6 -72.9(11) . . . . ? N4 Cu1 N3 C6 -8.46(19) . . . . ? N1 Cu1 N3 C6 -179.3(2) . . . . ? O4 Cu1 N3 C6 90.50(19) . . . . ? C5 N3 C6 O2 3.0(4) . . . . ? Cu1 N3 C6 O2 -172.6(2) . . . . ? C5 N3 C6 C7 -176.8(2) . . . . ? Cu1 N3 C6 C7 7.5(3) . . . . ? O2 C6 C7 N4 179.1(2) . . . . ? N3 C6 C7 N4 -1.1(3) . . . . ? O2 C6 C7 C8 -3.5(4) . . . . ? N3 C6 C7 C8 176.3(2) . . . . ? N4 C7 C8 C9 1.1(4) . . . . ? C6 C7 C8 C9 -176.2(2) . . . . ? C7 C8 C9 C10 0.6(4) . . . . ? C8 C9 C10 C11 -1.8(4) . . . . ? C9 C10 C11 N4 1.6(4) . . . . ? C10 C11 N4 C7 0.0(4) . . . . ? C10 C11 N4 Cu1 -178.2(2) . . . . ? C8 C7 N4 C11 -1.4(4) . . . . ? C6 C7 N4 C11 176.1(2) . . . . ? C8 C7 N4 Cu1 177.1(2) . . . . ? C6 C7 N4 Cu1 -5.4(3) . . . . ? N3 Cu1 N4 C11 -174.3(2) . . . . ? O3 Cu1 N4 C11 1.3(2) . . . . ? N1 Cu1 N4 C11 -144.2(3) . . . . ? O4 Cu1 N4 C11 92.4(2) . . . . ? N3 Cu1 N4 C7 7.40(18) . . . . ? O3 Cu1 N4 C7 -177.07(18) . . . . ? N1 Cu1 N4 C7 37.5(4) . . . . ? O4 Cu1 N4 C7 -85.90(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3X O21 0.89(3) 1.70(3) 2.591(3) 176(3) 1_556 O3 H3Y F3 0.79(3) 1.90(3) 2.682(3) 167(3) 1_565 O4 H4X N2 0.85(3) 2.04(3) 2.852(3) 160(3) 1_455 O4 H4Y O2 0.76(3) 2.12(3) 2.794(3) 149(3) 2_666 O4 H4Y O1 0.76(3) 2.43(3) 3.003(3) 133(3) 2_666 O21 H21X O4 0.84(4) 1.96(4) 2.789(3) 171(3) 2_666 O21 H21Y F4 0.76(4) 2.10(4) 2.844(3) 165(4) 2_666 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.583 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.077 data_mgc424 _database_code_depnum_ccdc_archive 'CCDC 808582' #TrackingRef '- mgc424final_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 N8 O4 Co, B F4' _chemical_formula_sum 'C22 H14 B Co F4 N8 O4' _chemical_formula_weight 600.15 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' 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' 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' Co Co 0.3494 0.9721 '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 22.953(7) _cell_length_b 8.540(3) _cell_length_c 23.055(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.000(9) _cell_angle_gamma 90.00 _cell_volume 4403(2) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 2057 _cell_measurement_theta_min 2.2625 _cell_measurement_theta_max 19.5015 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6403 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SCALE(Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(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 APEX II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49902 _diffrn_reflns_av_R_equivalents 0.1746 _diffrn_reflns_av_sigmaI/netI 0.1237 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6313 _reflns_number_gt 3635 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. [Co(pypzca)2BF4]. Two entire complexes in the asym. unit. All non-H atoms are refined anisotropically. All H are calc and ride. One BF4- anion is disordered over two sets of F's (common B) each 0.5 occupancy (restrained using DFIX and SADI). The pyridine/pyrazine CH vs N assignment within each of the two ligands bound to Co1 could not be made so has been modelled as CH:N 0.5:0.5 occupancy in both ends of each of these 2 ligands (EADP and EXYZ used to ensure that C3, N3a share the same site and U, and likewise for N3, C3a). This assignment was able to be made for the 2 ligands bound to Co2, as a Q showed up only on one end of each of these ligands, hence allowing CH to be assigned and leaving the other end as the N. The data is of low quality due to the extremely thin nature of the crystals. Attempts at slowing the evaporation of solvent and/or recrystallisation from water did not yield superior quality crystals. This data set is suitable for connectivity only and not to provide accurate bond lengths and angles. The remaining errors in the checkcif document are a result of this low quality data. ; _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^)+(0.1129P)^2^+114.4031P] 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 6313 _refine_ls_number_parameters 758 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1973 _refine_ls_R_factor_gt 0.1346 _refine_ls_wR_factor_ref 0.3730 _refine_ls_wR_factor_gt 0.3395 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.065 _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 0.88603(10) 0.9504(3) 0.85230(9) 0.0482(7) Uani 1 1 d . B . N1 N 0.9150(8) 0.8668(15) 0.7858(6) 0.055(4) Uani 1 1 d . . . C1 C 0.9711(10) 0.829(2) 0.7872(9) 0.063(5) Uani 1 1 d . B . H1 H 1.0008 0.8379 0.8231 0.076 Uiso 1 1 calc R . . C2 C 0.9866(12) 0.775(2) 0.7350(10) 0.078(7) Uani 1 1 d . . . H2 H 1.0269 0.7477 0.7355 0.094 Uiso 1 1 calc R A 1 C3 C 0.9435(16) 0.760(2) 0.6834(9) 0.107(9) Uani 0.50 1 d P B 1 H3 H 0.9533 0.7219 0.6481 0.128 Uiso 0.50 1 calc PR B 1 N3A N 0.9435(16) 0.760(2) 0.6834(9) 0.107(9) Uani 0.50 1 d P B 2 C4 C 0.8829(18) 0.805(3) 0.6837(11) 0.113(11) Uani 1 1 d . . . H4 H 0.8524 0.8016 0.6482 0.136 Uiso 1 1 calc R B 1 C5 C 0.8703(14) 0.853(2) 0.7351(8) 0.083(8) Uani 1 1 d . B . C6 C 0.8082(11) 0.897(2) 0.7426(9) 0.070(6) Uani 1 1 d . . . O1 O 0.7647(7) 0.8705(17) 0.7011(7) 0.099(5) Uani 1 1 d U B . N2 N 0.8109(8) 0.9509(16) 0.7960(6) 0.053(4) Uani 1 1 d . B . C7 C 0.7643(12) 1.003(2) 0.8131(12) 0.092(8) Uani 1 1 d . . . O2 O 0.7123(5) 1.0206(16) 0.7866(7) 0.092(5) Uani 1 1 d U B . C8 C 0.7776(8) 1.043(2) 0.8779(9) 0.064(6) Uani 1 1 d . B . C9 C 0.7392(8) 1.094(2) 0.9173(14) 0.083(8) Uani 1 1 d . . . H9 H 0.6972 1.0910 0.9018 0.100 Uiso 1 1 calc R B 1 N3 N 0.7571(8) 1.139(2) 0.9693(10) 0.069(5) Uani 0.50 1 d P B 1 C3A C 0.7571(8) 1.139(2) 0.9693(10) 0.069(5) Uani 0.50 1 d P B 2 H3A H 0.7307 1.1818 0.9916 0.082 Uiso 0.50 1 calc PR B 2 C10 C 0.8152(9) 1.126(2) 0.9918(9) 0.065(5) Uani 1 1 d . . . H10 H 0.8297 1.1555 1.0322 0.077 Uiso 1 1 calc R B 1 C11 C 0.8563(8) 1.0723(18) 0.9617(8) 0.047(4) Uani 1 1 d . B . H11 H 0.8974 1.0668 0.9810 0.057 Uiso 1 1 calc R . . N4 N 0.8386(6) 1.0288(17) 0.9059(7) 0.059(4) Uani 1 1 d . . . N21 N 0.8761(6) 0.7459(15) 0.8835(5) 0.044(3) Uani 1 1 d . . . C21 C 0.8299(8) 0.646(2) 0.8693(7) 0.052(5) Uani 1 1 d . B . H21 H 0.7975 0.6741 0.8375 0.063 Uiso 1 1 calc R . . C22 C 0.8264(7) 0.5020(19) 0.8992(8) 0.051(5) Uani 1 1 d . . . H22 H 0.7946 0.4300 0.8862 0.061 Uiso 1 1 calc R B 1 C23 C 0.8711(8) 0.474(2) 0.9470(7) 0.060(5) Uani 0.50 1 d P B 1 H23 H 0.8679 0.3873 0.9720 0.072 Uiso 0.50 1 calc PR B 1 N23A N 0.8711(8) 0.474(2) 0.9470(7) 0.060(5) Uani 0.50 1 d P B 2 C24 C 0.9205(9) 0.565(2) 0.9605(9) 0.069(6) Uani 1 1 d . . . H24 H 0.9533 0.5371 0.9918 0.083 Uiso 1 1 calc R B 1 C25 C 0.9227(7) 0.7010(18) 0.9280(7) 0.043(4) Uani 1 1 d . B . C26 C 0.9741(8) 0.8098(18) 0.9417(7) 0.045(4) Uani 1 1 d . . . O21 O 1.0210(5) 0.7771(15) 0.9768(5) 0.055(3) Uani 1 1 d . B . N22 N 0.9602(6) 0.9453(16) 0.9087(5) 0.047(3) Uani 1 1 d . B . C27 C 0.9977(8) 1.071(2) 0.9113(7) 0.056(5) Uani 1 1 d . . . O22 O 1.0477(5) 1.0842(14) 0.9396(5) 0.057(3) Uani 1 1 d . B . C28 C 0.9676(8) 1.193(2) 0.8710(7) 0.047(4) Uani 1 1 d . B . C29 C 0.9887(7) 1.341(2) 0.8649(7) 0.045(4) Uani 1 1 d . . . H29 H 1.0269 1.3677 0.8886 0.054 Uiso 1 1 calc R B 1 N23 N 0.9589(7) 1.4554(17) 0.8270(7) 0.049(4) Uani 0.50 1 d P B 1 C23A C 0.9589(7) 1.4554(17) 0.8270(7) 0.049(4) Uani 0.50 1 d P B 2 H23A H 0.9753 1.5563 0.8237 0.059 Uiso 0.50 1 calc PR B 2 C30 C 0.9072(8) 1.414(2) 0.7965(7) 0.052(5) Uani 1 1 d . . . H30 H 0.8845 1.4881 0.7700 0.062 Uiso 1 1 calc R B 1 N24 N 0.9133(5) 1.1572(14) 0.8366(5) 0.040(3) Uani 1 1 d . . . C31 C 0.8818(7) 1.2613(18) 0.8003(7) 0.042(4) Uani 1 1 d . B . H31 H 0.8432 1.2360 0.7772 0.050 Uiso 1 1 calc R . . Co2 Co 0.65045(9) 0.9496(2) 0.10905(9) 0.0409(7) Uani 1 1 d . . . N41 N 0.6184(5) 0.7459(13) 0.1207(5) 0.035(3) Uani 1 1 d . . . C41 C 0.6340(7) 0.6514(16) 0.1695(7) 0.046(4) Uani 1 1 d . . . H41 H 0.6677 0.6739 0.2007 0.055 Uiso 1 1 calc R . . C42 C 0.5979(8) 0.5195(17) 0.1717(7) 0.050(5) Uani 1 1 d . . . H42 H 0.6054 0.4586 0.2070 0.060 Uiso 1 1 calc R . . C43 C 0.5555(8) 0.4772(18) 0.1282(8) 0.056(5) Uani 1 1 d . . . H43 H 0.5356 0.3802 0.1297 0.067 Uiso 1 1 calc R . . C44 C 0.5393(8) 0.5730(18) 0.0799(7) 0.049(4) Uani 1 1 d . . . H44 H 0.5047 0.5501 0.0498 0.059 Uiso 1 1 calc R . . C45 C 0.5728(7) 0.7012(18) 0.0751(8) 0.044(4) Uani 1 1 d . . . C46 C 0.5573(7) 0.810(2) 0.0227(7) 0.048(4) Uani 1 1 d . . . O41 O 0.5220(5) 0.7778(13) -0.0211(4) 0.050(3) Uani 1 1 d . . . N42 N 0.5918(5) 0.9455(13) 0.0369(5) 0.032(3) Uani 1 1 d . . . C47 C 0.5880(7) 1.0718(17) -0.0010(7) 0.041(4) Uani 1 1 d . . . O42 O 0.5602(5) 1.0887(12) -0.0498(4) 0.048(3) Uani 1 1 d . . . C48 C 0.6315(7) 1.197(2) 0.0287(8) 0.051(5) Uani 1 1 d . . . C49 C 0.6353(8) 1.3399(17) 0.0071(8) 0.047(4) Uani 1 1 d . . . H49 H 0.6103 1.3655 -0.0304 0.056 Uiso 1 1 calc R . . N43 N 0.6738(6) 1.4534(17) 0.0365(7) 0.062(4) Uani 1 1 d . . . C50 C 0.7069(8) 1.403(2) 0.0892(9) 0.060(5) Uani 1 1 d . . . H50 H 0.7366 1.4717 0.1106 0.072 Uiso 1 1 calc R . . C51 C 0.7014(7) 1.2677(18) 0.1127(7) 0.048(4) Uani 1 1 d . . . H51 H 0.7237 1.2460 0.1519 0.057 Uiso 1 1 calc R . . N44 N 0.6648(5) 1.1574(15) 0.0829(6) 0.043(3) Uani 1 1 d . . . N61 N 0.7138(5) 0.8616(15) 0.0765(7) 0.048(4) Uani 1 1 d . . . C61 C 0.7089(8) 0.811(2) 0.0221(10) 0.058(5) Uani 1 1 d . . . H61 H 0.6712 0.8129 -0.0054 0.070 Uiso 1 1 calc R . . C62 C 0.7609(9) 0.752(2) 0.0039(11) 0.073(6) Uani 1 1 d . . . H62 H 0.7575 0.7140 -0.0354 0.087 Uiso 1 1 calc R . . C63 C 0.8149(9) 0.752(2) 0.0431(13) 0.070(6) Uani 1 1 d . . . H63 H 0.8496 0.7129 0.0321 0.084 Uiso 1 1 calc R . . C64 C 0.8173(10) 0.805(3) 0.0932(14) 0.089(8) Uani 1 1 d . . . H64 H 0.8557 0.8076 0.1193 0.107 Uiso 1 1 calc R . . C65 C 0.7682(7) 0.8618(17) 0.1167(9) 0.050(5) Uani 1 1 d . . . C66 C 0.7666(9) 0.908(2) 0.1757(10) 0.071(6) Uani 1 1 d . . . O61 O 0.8133(6) 0.9135(16) 0.2159(8) 0.100(6) Uani 1 1 d . . . N62 N 0.7115(6) 0.9546(15) 0.1804(7) 0.049(4) Uani 1 1 d . . . C67 C 0.6971(9) 1.020(2) 0.2285(10) 0.065(6) Uani 1 1 d . . . C68 C 0.6325(8) 1.060(2) 0.2151(7) 0.054(5) Uani 1 1 d . . . O62 O 0.7293(6) 1.0469(17) 0.2788(5) 0.081(5) Uani 1 1 d . . . C69 C 0.6019(12) 1.123(3) 0.2566(11) 0.086(7) Uani 1 1 d . . . H69 H 0.6236 1.1406 0.2963 0.103 Uiso 1 1 calc R . . N63 N 0.5457(9) 1.158(2) 0.2429(7) 0.074(5) Uani 1 1 d . . . C70 C 0.5149(8) 1.135(2) 0.1854(7) 0.051(4) Uani 1 1 d . . . H70 H 0.4738 1.1627 0.1739 0.061 Uiso 1 1 calc R . . C71 C 0.5434(8) 1.0716(18) 0.1439(8) 0.052(5) Uani 1 1 d . . . H71 H 0.5209 1.0514 0.1047 0.062 Uiso 1 1 calc R . . N64 N 0.6021(5) 1.0376(12) 0.1578(4) 0.028(3) Uani 1 1 d . . . B1 B 0.6412(8) 0.6969(17) -0.1355(7) 0.079(7) Uani 1 1 d D . . F11 F 0.5999(6) 0.6602(14) -0.1862(5) 0.086(4) Uani 1 1 d D . . F12 F 0.6401(11) 0.5854(14) -0.0939(5) 0.189(11) Uani 1 1 d D . . F13 F 0.6944(7) 0.694(2) -0.1515(9) 0.157(7) Uani 1 1 d D . . F14 F 0.6301(5) 0.8370(11) -0.1126(5) 0.079(3) Uani 1 1 d D . . B2 B 0.8709(7) 0.289(2) 0.1464(7) 0.147(19) Uani 1 1 d D . . F21 F 0.8542(19) 0.285(4) 0.1990(12) 0.25(4) Uani 0.50 1 d PDU C 1 F22 F 0.9154(9) 0.394(3) 0.1489(14) 0.105(10) Uani 0.50 1 d PD C 1 F23 F 0.8897(10) 0.145(2) 0.1337(15) 0.17(2) Uani 0.50 1 d PD C 1 F24 F 0.8242(11) 0.335(4) 0.1030(12) 0.23(3) Uani 0.50 1 d PD C 1 F26 F 0.8828(17) 0.292(3) 0.2065(7) 0.142(17) Uani 0.50 1 d PD C 2 F27 F 0.9172(10) 0.224(5) 0.1279(11) 0.18(2) Uani 0.50 1 d PD C 2 F28 F 0.8609(19) 0.434(2) 0.1235(12) 0.20(3) Uani 0.50 1 d PD C 2 F29 F 0.8222(10) 0.198(3) 0.1262(13) 0.110(11) Uani 0.50 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0578(15) 0.0322(13) 0.0410(13) -0.0009(10) -0.0178(11) -0.0002(11) N1 0.086(12) 0.030(8) 0.042(9) -0.008(6) -0.001(8) 0.003(8) C1 0.081(15) 0.042(11) 0.068(13) -0.006(10) 0.021(11) -0.003(10) C2 0.13(2) 0.033(11) 0.083(16) 0.000(11) 0.051(16) -0.022(12) C3 0.23(3) 0.048(13) 0.048(13) -0.012(10) 0.045(19) -0.001(17) N3A 0.23(3) 0.048(13) 0.048(13) -0.012(10) 0.045(19) -0.001(17) C4 0.23(4) 0.034(13) 0.067(17) -0.010(12) 0.01(2) -0.016(18) C5 0.19(3) 0.024(10) 0.026(10) -0.005(8) 0.006(13) -0.035(13) C6 0.090(15) 0.030(10) 0.068(15) 0.001(9) -0.029(13) 0.003(10) O1 0.111(10) 0.066(9) 0.087(9) 0.000(8) -0.051(9) -0.005(8) N2 0.077(11) 0.036(8) 0.032(8) -0.006(7) -0.021(8) 0.000(8) C7 0.091(18) 0.041(12) 0.12(2) 0.000(13) -0.032(18) -0.025(12) O2 0.045(7) 0.073(9) 0.123(11) 0.013(8) -0.058(8) 0.004(6) C8 0.045(11) 0.044(11) 0.089(15) 0.023(11) -0.018(11) -0.005(9) C9 0.029(10) 0.051(13) 0.18(3) 0.040(15) 0.036(15) 0.007(9) N3 0.051(12) 0.072(13) 0.082(14) -0.008(11) 0.013(11) -0.010(10) C3A 0.051(12) 0.072(13) 0.082(14) -0.008(11) 0.013(11) -0.010(10) C10 0.057(13) 0.056(12) 0.074(13) 0.011(11) 0.000(11) 0.004(10) C11 0.044(10) 0.035(9) 0.055(11) 0.010(8) -0.006(9) 0.004(8) N4 0.049(9) 0.053(9) 0.068(11) 0.040(8) -0.004(8) 0.004(7) N21 0.054(8) 0.032(7) 0.039(7) 0.004(6) -0.005(7) 0.009(7) C21 0.049(10) 0.050(11) 0.047(10) -0.006(9) -0.010(8) 0.008(9) C22 0.046(10) 0.038(10) 0.062(11) 0.025(8) -0.003(9) -0.010(8) C23 0.072(12) 0.060(11) 0.047(10) 0.010(8) 0.011(9) 0.017(10) N23A 0.072(12) 0.060(11) 0.047(10) 0.010(8) 0.011(9) 0.017(10) C24 0.065(13) 0.046(12) 0.087(15) 0.019(11) -0.001(11) 0.013(10) C25 0.040(9) 0.033(9) 0.046(9) -0.002(8) -0.009(8) 0.003(7) C26 0.060(11) 0.038(10) 0.031(9) -0.008(7) 0.000(9) 0.012(8) O21 0.039(6) 0.078(9) 0.041(6) -0.006(6) -0.007(6) 0.020(6) N22 0.041(7) 0.049(9) 0.039(7) -0.003(7) -0.016(6) 0.004(7) C27 0.063(12) 0.054(12) 0.039(10) -0.017(9) -0.016(9) 0.017(10) O22 0.043(7) 0.069(9) 0.048(7) -0.002(6) -0.011(6) 0.003(6) C28 0.057(11) 0.048(11) 0.031(9) -0.001(8) 0.003(8) -0.006(9) C29 0.033(9) 0.064(12) 0.039(9) 0.009(9) 0.010(7) 0.012(8) N23 0.058(10) 0.042(9) 0.049(9) -0.001(8) 0.013(8) -0.010(8) C23A 0.058(10) 0.042(9) 0.049(9) -0.001(8) 0.013(8) -0.010(8) C30 0.062(12) 0.068(13) 0.023(8) -0.001(8) 0.004(8) 0.015(10) N24 0.041(7) 0.031(7) 0.038(7) -0.001(6) -0.009(6) 0.001(6) C31 0.039(9) 0.041(10) 0.038(9) -0.005(8) -0.008(7) -0.002(8) Co2 0.0395(12) 0.0283(12) 0.0455(13) 0.0059(10) -0.0101(10) -0.0027(9) N41 0.034(7) 0.023(7) 0.042(7) 0.003(6) -0.006(6) 0.006(5) C41 0.052(10) 0.019(8) 0.054(10) 0.009(8) -0.014(8) 0.006(7) C42 0.083(13) 0.017(8) 0.043(10) 0.005(7) 0.000(10) -0.010(8) C43 0.080(13) 0.020(9) 0.059(11) -0.004(8) -0.005(10) -0.014(9) C44 0.071(12) 0.034(9) 0.045(10) -0.010(8) 0.017(9) -0.018(9) C45 0.034(9) 0.033(9) 0.066(11) 0.000(8) 0.013(9) 0.006(7) C46 0.042(10) 0.057(11) 0.038(10) -0.021(9) -0.007(9) -0.003(8) O41 0.052(7) 0.051(7) 0.036(6) -0.012(5) -0.010(6) -0.004(6) N42 0.025(6) 0.031(7) 0.033(7) -0.003(6) -0.007(5) 0.007(5) C47 0.057(10) 0.024(8) 0.034(9) -0.011(7) -0.007(8) -0.003(7) O42 0.052(7) 0.050(7) 0.033(6) -0.002(5) -0.012(6) 0.003(5) C48 0.029(9) 0.065(12) 0.062(12) 0.020(10) 0.013(8) 0.011(8) C49 0.066(11) 0.022(8) 0.056(10) 0.017(8) 0.020(9) 0.008(8) N43 0.051(9) 0.052(9) 0.072(10) 0.026(8) -0.009(8) -0.002(8) C50 0.055(11) 0.050(12) 0.076(13) 0.018(10) 0.015(10) -0.016(9) C51 0.058(10) 0.030(9) 0.042(9) -0.014(8) -0.017(8) -0.018(8) N44 0.030(7) 0.044(8) 0.046(8) 0.012(7) -0.010(6) -0.001(6) N61 0.033(8) 0.026(7) 0.078(11) 0.016(7) 0.000(8) 0.002(6) C61 0.046(11) 0.045(11) 0.084(15) 0.023(11) 0.013(11) 0.003(9) C62 0.076(15) 0.042(11) 0.116(18) 0.025(11) 0.055(14) 0.018(10) C63 0.045(13) 0.046(13) 0.12(2) 0.015(13) 0.030(14) 0.015(10) C64 0.065(16) 0.046(14) 0.15(3) 0.033(15) 0.001(17) -0.002(12) C65 0.026(9) 0.017(8) 0.098(15) 0.015(9) -0.004(9) 0.002(7) C66 0.062(13) 0.041(11) 0.083(15) 0.003(10) -0.040(12) -0.006(9) O61 0.064(9) 0.067(10) 0.135(13) 0.014(9) -0.051(9) 0.001(7) N62 0.052(9) 0.022(7) 0.068(10) 0.013(7) -0.002(8) -0.002(7) C67 0.059(12) 0.051(12) 0.070(14) 0.019(11) -0.019(12) -0.022(10) C68 0.069(12) 0.050(11) 0.033(9) -0.003(8) -0.012(9) -0.020(10) O62 0.079(9) 0.089(10) 0.052(7) 0.017(7) -0.035(7) -0.037(8) C69 0.097(19) 0.069(15) 0.077(16) 0.007(13) -0.013(15) -0.036(14) N63 0.083(13) 0.068(12) 0.067(11) -0.009(9) 0.010(10) -0.023(10) C70 0.056(11) 0.049(11) 0.046(10) -0.020(9) 0.010(9) -0.022(9) C71 0.061(12) 0.032(9) 0.054(11) 0.000(8) -0.004(10) -0.007(8) N64 0.045(7) 0.018(6) 0.017(6) 0.001(5) -0.005(5) -0.009(5) B1 0.09(2) 0.069(18) 0.09(2) 0.007(15) 0.033(17) 0.008(15) F11 0.123(10) 0.072(8) 0.060(7) 0.004(6) 0.016(7) 0.026(7) F12 0.44(3) 0.044(8) 0.056(8) 0.027(7) -0.002(13) 0.009(13) F13 0.109(12) 0.158(16) 0.213(19) 0.018(14) 0.059(13) 0.076(12) F14 0.097(8) 0.040(6) 0.104(9) -0.022(6) 0.028(7) 0.006(6) B2 0.08(2) 0.21(5) 0.14(4) -0.10(4) -0.01(3) -0.04(3) F21 0.34(6) 0.25(6) 0.22(5) -0.11(4) 0.20(5) 0.05(5) F22 0.070(18) 0.12(3) 0.13(3) -0.01(2) 0.040(18) 0.029(18) F23 0.09(2) 0.17(3) 0.29(5) -0.20(4) 0.12(3) -0.09(2) F24 0.08(2) 0.26(6) 0.32(7) -0.26(6) 0.00(3) 0.01(3) F26 0.25(5) 0.050(18) 0.12(3) 0.004(19) 0.03(3) 0.02(2) F27 0.11(3) 0.38(8) 0.052(17) 0.00(3) 0.003(18) 0.10(4) F28 0.41(9) 0.07(2) 0.11(3) -0.01(2) -0.01(4) 0.02(4) F29 0.11(2) 0.056(16) 0.17(3) -0.017(19) 0.05(2) -0.005(16) _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 N22 1.896(12) . ? Co1 N2 1.911(14) . ? Co1 N21 1.921(13) . ? Co1 N24 1.935(12) . ? Co1 N1 1.939(15) . ? Co1 N4 1.941(17) . ? N1 C1 1.32(2) . ? N1 C5 1.38(2) . ? C1 C2 1.41(3) . ? C1 H1 0.9500 . ? C2 C3 1.37(3) . ? C2 H2 0.9500 . ? C3 C4 1.45(4) . ? C3 H3 0.9500 . ? C4 C5 1.34(3) . ? C4 H4 0.9500 . ? C5 C6 1.52(3) . ? C6 O1 1.24(2) . ? C6 N2 1.30(2) . ? N2 C7 1.30(3) . ? C7 O2 1.22(3) . ? C7 C8 1.50(3) . ? C8 N4 1.41(2) . ? C8 C9 1.47(3) . ? C9 N3 1.24(3) . ? C9 H9 0.9500 . ? N3 C10 1.32(2) . ? C10 C11 1.37(2) . ? C10 H10 0.9500 . ? C11 N4 1.31(2) . ? C11 H11 0.9500 . ? N21 C21 1.34(2) . ? N21 C25 1.360(18) . ? C21 C22 1.42(2) . ? C21 H21 0.9500 . ? C22 C23 1.35(2) . ? C22 H22 0.9500 . ? C23 C24 1.36(2) . ? C23 H23 0.9500 . ? C24 C25 1.39(2) . ? C24 H24 0.9500 . ? C25 C26 1.48(2) . ? C26 O21 1.225(17) . ? C26 N22 1.38(2) . ? N22 C27 1.37(2) . ? C27 O22 1.190(19) . ? C27 C28 1.46(2) . ? C28 N24 1.352(19) . ? C28 C29 1.37(2) . ? C29 N23 1.38(2) . ? C29 H29 0.9500 . ? N23 C30 1.29(2) . ? C30 C31 1.44(2) . ? C30 H30 0.9500 . ? N24 C31 1.320(18) . ? C31 H31 0.9500 . ? Co2 N42 1.890(10) . ? Co2 N64 1.903(12) . ? Co2 N62 1.905(14) . ? Co2 N44 1.926(13) . ? Co2 N41 1.931(12) . ? Co2 N61 1.932(15) . ? N41 C45 1.359(19) . ? N41 C41 1.366(18) . ? C41 C42 1.40(2) . ? C41 H41 0.9500 . ? C42 C43 1.28(2) . ? C42 H42 0.9500 . ? C43 C44 1.36(2) . ? C43 H43 0.9500 . ? C44 C45 1.36(2) . ? C44 H44 0.9500 . ? C45 C46 1.51(2) . ? C46 O41 1.176(16) . ? C46 N42 1.396(19) . ? N42 C47 1.377(19) . ? C47 O42 1.172(17) . ? C47 C48 1.52(2) . ? C48 C49 1.33(2) . ? C48 N44 1.354(19) . ? C49 N43 1.38(2) . ? C49 H49 0.9500 . ? N43 C50 1.35(2) . ? C50 C51 1.29(2) . ? C50 H50 0.9500 . ? C51 N44 1.343(18) . ? C51 H51 0.9500 . ? N61 C61 1.31(2) . ? N61 C65 1.38(2) . ? C61 C62 1.44(3) . ? C61 H61 0.9500 . ? C62 C63 1.36(3) . ? C62 H62 0.9500 . ? C63 C64 1.23(3) . ? C63 H63 0.9500 . ? C64 C65 1.44(3) . ? C64 H64 0.9500 . ? C65 C66 1.42(3) . ? C66 O61 1.25(2) . ? C66 N62 1.35(2) . ? N62 C67 1.35(2) . ? C67 O62 1.25(2) . ? C67 C68 1.48(3) . ? C68 N64 1.360(18) . ? C68 C69 1.42(3) . ? C69 N63 1.29(3) . ? C69 H69 0.9500 . ? N63 C70 1.37(2) . ? C70 C71 1.38(2) . ? C70 H70 0.9500 . ? C71 N64 1.35(2) . ? C71 H71 0.9500 . ? B1 F13 1.353(13) . ? B1 F14 1.355(13) . ? B1 F12 1.356(13) . ? B1 F11 1.366(13) . ? B2 F27 1.348(13) . ? B2 F22 1.348(13) . ? B2 F28 1.348(13) . ? B2 F26 1.351(13) . ? B2 F24 1.351(13) . ? B2 F23 1.353(13) . ? B2 F21 1.354(13) . ? B2 F29 1.356(13) . ? 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 N22 Co1 N2 178.7(6) . . ? N22 Co1 N21 83.5(6) . . ? N2 Co1 N21 95.3(6) . . ? N22 Co1 N24 82.5(6) . . ? N2 Co1 N24 98.7(5) . . ? N21 Co1 N24 165.9(5) . . ? N22 Co1 N1 96.8(6) . . ? N2 Co1 N1 83.1(7) . . ? N21 Co1 N1 92.9(6) . . ? N24 Co1 N1 90.3(6) . . ? N22 Co1 N4 96.7(6) . . ? N2 Co1 N4 83.2(7) . . ? N21 Co1 N4 86.8(6) . . ? N24 Co1 N4 93.2(6) . . ? N1 Co1 N4 166.3(6) . . ? C1 N1 C5 122.4(19) . . ? C1 N1 Co1 125.2(13) . . ? C5 N1 Co1 112.4(16) . . ? N1 C1 C2 119(2) . . ? N1 C1 H1 120.3 . . ? C2 C1 H1 120.3 . . ? C3 C2 C1 120(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119(2) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 N1 121(3) . . ? C4 C5 C6 125(3) . . ? N1 C5 C6 114.9(17) . . ? O1 C6 N2 131(2) . . ? O1 C6 C5 119(2) . . ? N2 C6 C5 110.3(17) . . ? C7 N2 C6 122.7(19) . . ? C7 N2 Co1 118.2(14) . . ? C6 N2 Co1 119.0(16) . . ? O2 C7 N2 132(3) . . ? O2 C7 C8 115(3) . . ? N2 C7 C8 112.6(19) . . ? N4 C8 C9 114.5(18) . . ? N4 C8 C7 113(2) . . ? C9 C8 C7 132(2) . . ? N3 C9 C8 125.2(19) . . ? N3 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? C9 N3 C10 116(2) . . ? N3 C10 C11 125.4(19) . . ? N3 C10 H10 117.3 . . ? C11 C10 H10 117.3 . . ? N4 C11 C10 119.6(16) . . ? N4 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 N4 C8 118.8(17) . . ? C11 N4 Co1 128.8(12) . . ? C8 N4 Co1 112.3(14) . . ? C21 N21 C25 116.7(14) . . ? C21 N21 Co1 129.7(11) . . ? C25 N21 Co1 113.6(10) . . ? N21 C21 C22 124.0(14) . . ? N21 C21 H21 118.0 . . ? C22 C21 H21 118.0 . . ? C23 C22 C21 115.8(15) . . ? C23 C22 H22 122.1 . . ? C21 C22 H22 122.1 . . ? C22 C23 C24 121.9(17) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C25 119.3(17) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? N21 C25 C24 121.7(15) . . ? N21 C25 C26 116.0(14) . . ? C24 C25 C26 122.2(15) . . ? O21 C26 N22 127.9(16) . . ? O21 C26 C25 122.6(15) . . ? N22 C26 C25 109.5(13) . . ? C27 N22 C26 124.5(13) . . ? C27 N22 Co1 118.1(11) . . ? C26 N22 Co1 117.2(11) . . ? O22 C27 N22 128.1(16) . . ? O22 C27 C28 122.7(18) . . ? N22 C27 C28 109.2(14) . . ? N24 C28 C29 116.7(14) . . ? N24 C28 C27 116.8(15) . . ? C29 C28 C27 126.5(15) . . ? C28 C29 N23 125.3(15) . . ? C28 C29 H29 117.4 . . ? N23 C29 H29 117.4 . . ? C30 N23 C29 114.6(15) . . ? N23 C30 C31 123.6(16) . . ? N23 C30 H30 118.2 . . ? C31 C30 H30 118.2 . . ? C31 N24 C28 121.3(14) . . ? C31 N24 Co1 125.4(10) . . ? C28 N24 Co1 113.1(10) . . ? N24 C31 C30 118.5(14) . . ? N24 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? N42 Co2 N64 97.7(5) . . ? N42 Co2 N62 178.1(6) . . ? N64 Co2 N62 83.9(6) . . ? N42 Co2 N44 83.1(5) . . ? N64 Co2 N44 89.1(5) . . ? N62 Co2 N44 96.0(5) . . ? N42 Co2 N41 83.6(5) . . ? N64 Co2 N41 89.0(5) . . ? N62 Co2 N41 97.4(5) . . ? N44 Co2 N41 166.2(5) . . ? N42 Co2 N61 95.7(6) . . ? N64 Co2 N61 166.6(5) . . ? N62 Co2 N61 82.7(7) . . ? N44 Co2 N61 92.3(5) . . ? N41 Co2 N61 92.7(5) . . ? C45 N41 C41 119.0(13) . . ? C45 N41 Co2 113.3(10) . . ? C41 N41 Co2 127.6(10) . . ? N41 C41 C42 117.1(14) . . ? N41 C41 H41 121.5 . . ? C42 C41 H41 121.5 . . ? C43 C42 C41 123.3(15) . . ? C43 C42 H42 118.3 . . ? C41 C42 H42 118.3 . . ? C42 C43 C44 119.2(16) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 119.7(17) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 N41 121.0(15) . . ? C44 C45 C46 122.0(15) . . ? N41 C45 C46 116.7(13) . . ? O41 C46 N42 130.0(16) . . ? O41 C46 C45 122.3(16) . . ? N42 C46 C45 107.7(12) . . ? C47 N42 C46 123.1(12) . . ? C47 N42 Co2 118.3(9) . . ? C46 N42 Co2 118.4(10) . . ? O42 C47 N42 130.5(14) . . ? O42 C47 C48 120.5(14) . . ? N42 C47 C48 108.9(12) . . ? C49 C48 N44 120.2(17) . . ? C49 C48 C47 124.8(15) . . ? N44 C48 C47 114.8(14) . . ? C48 C49 N43 123.3(16) . . ? C48 C49 H49 118.3 . . ? N43 C49 H49 118.3 . . ? C50 N43 C49 112.7(14) . . ? C51 C50 N43 125.0(17) . . ? C51 C50 H50 117.5 . . ? N43 C50 H50 117.5 . . ? C50 C51 N44 121.3(16) . . ? C50 C51 H51 119.3 . . ? N44 C51 H51 119.3 . . ? C51 N44 C48 117.1(14) . . ? C51 N44 Co2 128.1(11) . . ? C48 N44 Co2 114.7(11) . . ? C61 N61 C65 121.0(16) . . ? C61 N61 Co2 126.3(12) . . ? C65 N61 Co2 112.6(13) . . ? N61 C61 C62 119.8(19) . . ? N61 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C63 C62 C61 120(2) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C64 C63 C62 118(2) . . ? C64 C63 H63 121.1 . . ? C62 C63 H63 121.1 . . ? C63 C64 C65 127(2) . . ? C63 C64 H64 116.4 . . ? C65 C64 H64 116.4 . . ? N61 C65 C66 115.4(16) . . ? N61 C65 C64 114.4(19) . . ? C66 C65 C64 130.0(19) . . ? O61 C66 N62 126(2) . . ? O61 C66 C65 121(2) . . ? N62 C66 C65 112.5(15) . . ? C67 N62 C66 126.4(17) . . ? C67 N62 Co2 116.8(12) . . ? C66 N62 Co2 116.4(14) . . ? O62 C67 N62 130(2) . . ? O62 C67 C68 121(2) . . ? N62 C67 C68 109.9(16) . . ? N64 C68 C69 119.1(17) . . ? N64 C68 C67 116.1(18) . . ? C69 C68 C67 124.8(17) . . ? N63 C69 C68 123(2) . . ? N63 C69 H69 118.5 . . ? C68 C69 H69 118.5 . . ? C69 N63 C70 118.1(19) . . ? N63 C70 C71 120.3(17) . . ? N63 C70 H70 119.8 . . ? C71 C70 H70 119.8 . . ? N64 C71 C70 121.6(15) . . ? N64 C71 H71 119.2 . . ? C70 C71 H71 119.2 . . ? C71 N64 C68 117.9(15) . . ? C71 N64 Co2 129.1(10) . . ? C68 N64 Co2 112.9(12) . . ? F13 B1 F14 112.5(14) . . ? F13 B1 F12 110.0(18) . . ? F14 B1 F12 108.1(13) . . ? F13 B1 F11 104.9(14) . . ? F14 B1 F11 112.4(13) . . ? F12 B1 F11 108.9(14) . . ? F27 B2 F22 69.2(19) . . ? F27 B2 F28 109.4(16) . . ? F22 B2 F28 57.8(18) . . ? F27 B2 F26 110.0(15) . . ? F22 B2 F26 88(2) . . ? F28 B2 F26 110.9(14) . . ? F27 B2 F24 115.9(19) . . ? F22 B2 F24 107.7(14) . . ? F28 B2 F24 53.4(17) . . ? F26 B2 F24 134(2) . . ? F27 B2 F23 41.3(18) . . ? F22 B2 F23 109.7(13) . . ? F28 B2 F23 142(2) . . ? F26 B2 F23 104(2) . . ? F24 B2 F23 110.1(14) . . ? F27 B2 F21 133(2) . . ? F22 B2 F21 110.0(16) . . ? F28 B2 F21 108(2) . . ? F26 B2 F21 27(2) . . ? F24 B2 F21 109.4(16) . . ? F23 B2 F21 109.9(15) . . ? F27 B2 F29 107.7(15) . . ? F22 B2 F29 162.4(19) . . ? F28 B2 F29 109.7(15) . . ? F26 B2 F29 108.9(15) . . ? F24 B2 F29 57.1(17) . . ? F23 B2 F29 71.6(15) . . ? F21 B2 F29 85(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22 Co1 N1 C1 -1.6(15) . . . . ? N2 Co1 N1 C1 179.7(15) . . . . ? N21 Co1 N1 C1 -85.4(15) . . . . ? N24 Co1 N1 C1 80.9(15) . . . . ? N4 Co1 N1 C1 -174(2) . . . . ? N22 Co1 N1 C5 179.4(11) . . . . ? N2 Co1 N1 C5 0.7(11) . . . . ? N21 Co1 N1 C5 95.6(12) . . . . ? N24 Co1 N1 C5 -98.1(11) . . . . ? N4 Co1 N1 C5 7(3) . . . . ? C5 N1 C1 C2 1(3) . . . . ? Co1 N1 C1 C2 -177.7(12) . . . . ? N1 C1 C2 C3 0(3) . . . . ? C1 C2 C3 C4 1(3) . . . . ? C2 C3 C4 C5 -3(3) . . . . ? C3 C4 C5 N1 4(3) . . . . ? C3 C4 C5 C6 -177.2(19) . . . . ? C1 N1 C5 C4 -3(3) . . . . ? Co1 N1 C5 C4 176.1(15) . . . . ? C1 N1 C5 C6 177.9(16) . . . . ? Co1 N1 C5 C6 -3.1(18) . . . . ? C4 C5 C6 O1 9(3) . . . . ? N1 C5 C6 O1 -172.0(16) . . . . ? C4 C5 C6 N2 -174.3(18) . . . . ? N1 C5 C6 N2 5(2) . . . . ? O1 C6 N2 C7 -7(3) . . . . ? C5 C6 N2 C7 176.9(17) . . . . ? O1 C6 N2 Co1 171.9(17) . . . . ? C5 C6 N2 Co1 -4(2) . . . . ? N22 Co1 N2 C7 92(32) . . . . ? N21 Co1 N2 C7 88.8(15) . . . . ? N24 Co1 N2 C7 -89.6(15) . . . . ? N1 Co1 N2 C7 -178.9(16) . . . . ? N4 Co1 N2 C7 2.6(15) . . . . ? N22 Co1 N2 C6 -87(32) . . . . ? N21 Co1 N2 C6 -90.0(14) . . . . ? N24 Co1 N2 C6 91.6(14) . . . . ? N1 Co1 N2 C6 2.3(14) . . . . ? N4 Co1 N2 C6 -176.2(14) . . . . ? C6 N2 C7 O2 -3(4) . . . . ? Co1 N2 C7 O2 177.8(19) . . . . ? C6 N2 C7 C8 173.9(16) . . . . ? Co1 N2 C7 C8 -5(2) . . . . ? O2 C7 C8 N4 -177.1(16) . . . . ? N2 C7 C8 N4 5(2) . . . . ? O2 C7 C8 C9 3(3) . . . . ? N2 C7 C8 C9 -174.6(18) . . . . ? N4 C8 C9 N3 9(3) . . . . ? C7 C8 C9 N3 -172(2) . . . . ? C8 C9 N3 C10 -7(3) . . . . ? C9 N3 C10 C11 3(3) . . . . ? N3 C10 C11 N4 -1(3) . . . . ? C10 C11 N4 C8 2(2) . . . . ? C10 C11 N4 Co1 179.5(12) . . . . ? C9 C8 N4 C11 -5(2) . . . . ? C7 C8 N4 C11 174.8(15) . . . . ? C9 C8 N4 Co1 176.7(12) . . . . ? C7 C8 N4 Co1 -3.0(18) . . . . ? N22 Co1 N4 C11 4.2(15) . . . . ? N2 Co1 N4 C11 -177.1(15) . . . . ? N21 Co1 N4 C11 87.2(14) . . . . ? N24 Co1 N4 C11 -78.7(14) . . . . ? N1 Co1 N4 C11 177(2) . . . . ? N22 Co1 N4 C8 -178.2(11) . . . . ? N2 Co1 N4 C8 0.5(11) . . . . ? N21 Co1 N4 C8 -95.2(11) . . . . ? N24 Co1 N4 C8 98.9(11) . . . . ? N1 Co1 N4 C8 -6(3) . . . . ? N22 Co1 N21 C21 178.3(15) . . . . ? N2 Co1 N21 C21 -1.8(16) . . . . ? N24 Co1 N21 C21 172(2) . . . . ? N1 Co1 N21 C21 -85.2(15) . . . . ? N4 Co1 N21 C21 81.1(15) . . . . ? N22 Co1 N21 C25 1.1(11) . . . . ? N2 Co1 N21 C25 -179.0(12) . . . . ? N24 Co1 N21 C25 -5(3) . . . . ? N1 Co1 N21 C25 97.7(12) . . . . ? N4 Co1 N21 C25 -96.1(12) . . . . ? C25 N21 C21 C22 2(2) . . . . ? Co1 N21 C21 C22 -175.1(13) . . . . ? N21 C21 C22 C23 5(3) . . . . ? C21 C22 C23 C24 -9(3) . . . . ? C22 C23 C24 C25 7(3) . . . . ? C21 N21 C25 C24 -5(2) . . . . ? Co1 N21 C25 C24 172.5(14) . . . . ? C21 N21 C25 C26 178.2(14) . . . . ? Co1 N21 C25 C26 -4.3(18) . . . . ? C23 C24 C25 N21 1(3) . . . . ? C23 C24 C25 C26 177.5(16) . . . . ? N21 C25 C26 O21 -173.1(14) . . . . ? C24 C25 C26 O21 10(3) . . . . ? N21 C25 C26 N22 6(2) . . . . ? C24 C25 C26 N22 -170.7(16) . . . . ? O21 C26 N22 C27 -2(3) . . . . ? C25 C26 N22 C27 179.2(15) . . . . ? O21 C26 N22 Co1 173.9(13) . . . . ? C25 C26 N22 Co1 -5.1(17) . . . . ? N2 Co1 N22 C27 176(100) . . . . ? N21 Co1 N22 C27 178.5(13) . . . . ? N24 Co1 N22 C27 -3.1(12) . . . . ? N1 Co1 N22 C27 86.3(13) . . . . ? N4 Co1 N22 C27 -95.5(13) . . . . ? N2 Co1 N22 C26 0(32) . . . . ? N21 Co1 N22 C26 2.5(12) . . . . ? N24 Co1 N22 C26 -179.1(12) . . . . ? N1 Co1 N22 C26 -89.7(12) . . . . ? N4 Co1 N22 C26 88.5(12) . . . . ? C26 N22 C27 O22 3(3) . . . . ? Co1 N22 C27 O22 -172.9(15) . . . . ? C26 N22 C27 C28 -179.1(14) . . . . ? Co1 N22 C27 C28 5.2(18) . . . . ? O22 C27 C28 N24 173.0(16) . . . . ? N22 C27 C28 N24 -5(2) . . . . ? O22 C27 C28 C29 -8(3) . . . . ? N22 C27 C28 C29 174.3(16) . . . . ? N24 C28 C29 N23 0(2) . . . . ? C27 C28 C29 N23 -179.1(16) . . . . ? C28 C29 N23 C30 1(2) . . . . ? C29 N23 C30 C31 -1(2) . . . . ? C29 C28 N24 C31 -2(2) . . . . ? C27 C28 N24 C31 177.8(15) . . . . ? C29 C28 N24 Co1 -176.6(12) . . . . ? C27 C28 N24 Co1 3.0(18) . . . . ? N22 Co1 N24 C31 -174.6(14) . . . . ? N2 Co1 N24 C31 5.4(14) . . . . ? N21 Co1 N24 C31 -168(2) . . . . ? N1 Co1 N24 C31 88.5(13) . . . . ? N4 Co1 N24 C31 -78.2(13) . . . . ? N22 Co1 N24 C28 0.0(11) . . . . ? N2 Co1 N24 C28 180.0(12) . . . . ? N21 Co1 N24 C28 7(3) . . . . ? N1 Co1 N24 C28 -96.9(12) . . . . ? N4 Co1 N24 C28 96.3(11) . . . . ? C28 N24 C31 C30 2(2) . . . . ? Co1 N24 C31 C30 176.0(11) . . . . ? N23 C30 C31 N24 -1(3) . . . . ? N42 Co2 N41 C45 -0.1(10) . . . . ? N64 Co2 N41 C45 97.8(11) . . . . ? N62 Co2 N41 C45 -178.5(11) . . . . ? N44 Co2 N41 C45 15(3) . . . . ? N61 Co2 N41 C45 -95.5(11) . . . . ? N42 Co2 N41 C41 -175.8(14) . . . . ? N64 Co2 N41 C41 -78.0(13) . . . . ? N62 Co2 N41 C41 5.8(14) . . . . ? N44 Co2 N41 C41 -160(2) . . . . ? N61 Co2 N41 C41 88.7(14) . . . . ? C45 N41 C41 C42 -5(2) . . . . ? Co2 N41 C41 C42 170.1(12) . . . . ? N41 C41 C42 C43 7(3) . . . . ? C41 C42 C43 C44 -8(3) . . . . ? C42 C43 C44 C45 8(3) . . . . ? C43 C44 C45 N41 -7(2) . . . . ? C43 C44 C45 C46 179.6(16) . . . . ? C41 N41 C45 C44 6(2) . . . . ? Co2 N41 C45 C44 -169.9(12) . . . . ? C41 N41 C45 C46 179.5(14) . . . . ? Co2 N41 C45 C46 3.3(17) . . . . ? C44 C45 C46 O41 -13(3) . . . . ? N41 C45 C46 O41 173.8(15) . . . . ? C44 C45 C46 N42 167.4(15) . . . . ? N41 C45 C46 N42 -5.8(19) . . . . ? O41 C46 N42 C47 2(3) . . . . ? C45 C46 N42 C47 -178.7(13) . . . . ? O41 C46 N42 Co2 -173.7(15) . . . . ? C45 C46 N42 Co2 5.8(16) . . . . ? N64 Co2 N42 C47 92.6(11) . . . . ? N62 Co2 N42 C47 -56(17) . . . . ? N44 Co2 N42 C47 4.4(11) . . . . ? N41 Co2 N42 C47 -179.2(11) . . . . ? N61 Co2 N42 C47 -87.2(11) . . . . ? N64 Co2 N42 C46 -91.7(11) . . . . ? N62 Co2 N42 C46 119(16) . . . . ? N44 Co2 N42 C46 -179.9(12) . . . . ? N41 Co2 N42 C46 -3.6(11) . . . . ? N61 Co2 N42 C46 88.5(11) . . . . ? C46 N42 C47 O42 -4(3) . . . . ? Co2 N42 C47 O42 171.1(15) . . . . ? C46 N42 C47 C48 179.9(13) . . . . ? Co2 N42 C47 C48 -4.6(16) . . . . ? O42 C47 C48 C49 11(3) . . . . ? N42 C47 C48 C49 -173.1(16) . . . . ? O42 C47 C48 N44 -174.2(15) . . . . ? N42 C47 C48 N44 2.0(19) . . . . ? N44 C48 C49 N43 2(3) . . . . ? C47 C48 C49 N43 177.2(16) . . . . ? C48 C49 N43 C50 0(3) . . . . ? C49 N43 C50 C51 -5(3) . . . . ? N43 C50 C51 N44 7(3) . . . . ? C50 C51 N44 C48 -4(3) . . . . ? C50 C51 N44 Co2 179.5(14) . . . . ? C49 C48 N44 C51 -1(2) . . . . ? C47 C48 N44 C51 -176.0(14) . . . . ? C49 C48 N44 Co2 176.7(13) . . . . ? C47 C48 N44 Co2 1.3(18) . . . . ? N42 Co2 N44 C51 173.9(15) . . . . ? N64 Co2 N44 C51 76.1(15) . . . . ? N62 Co2 N44 C51 -7.7(15) . . . . ? N41 Co2 N44 C51 158(2) . . . . ? N61 Co2 N44 C51 -90.6(15) . . . . ? N42 Co2 N44 C48 -3.0(11) . . . . ? N64 Co2 N44 C48 -100.8(11) . . . . ? N62 Co2 N44 C48 175.4(12) . . . . ? N41 Co2 N44 C48 -18(3) . . . . ? N61 Co2 N44 C48 92.5(12) . . . . ? N42 Co2 N61 C61 -4.2(14) . . . . ? N64 Co2 N61 C61 176.7(18) . . . . ? N62 Co2 N61 C61 176.8(14) . . . . ? N44 Co2 N61 C61 -87.5(14) . . . . ? N41 Co2 N61 C61 79.6(14) . . . . ? N42 Co2 N61 C65 173.3(10) . . . . ? N64 Co2 N61 C65 -6(3) . . . . ? N62 Co2 N61 C65 -5.7(10) . . . . ? N44 Co2 N61 C65 90.0(10) . . . . ? N41 Co2 N61 C65 -102.9(10) . . . . ? C65 N61 C61 C62 1(2) . . . . ? Co2 N61 C61 C62 178.2(11) . . . . ? N61 C61 C62 C63 -1(3) . . . . ? C61 C62 C63 C64 -1(3) . . . . ? C62 C63 C64 C65 3(4) . . . . ? C61 N61 C65 C66 -175.3(15) . . . . ? Co2 N61 C65 C66 7.0(17) . . . . ? C61 N61 C65 C64 1(2) . . . . ? Co2 N61 C65 C64 -176.9(12) . . . . ? C63 C64 C65 N61 -3(3) . . . . ? C63 C64 C65 C66 173(2) . . . . ? N61 C65 C66 O61 -179.8(15) . . . . ? C64 C65 C66 O61 5(3) . . . . ? N61 C65 C66 N62 -4(2) . . . . ? C64 C65 C66 N62 -179.5(16) . . . . ? O61 C66 N62 C67 3(3) . . . . ? C65 C66 N62 C67 -172.5(15) . . . . ? O61 C66 N62 Co2 174.6(15) . . . . ? C65 C66 N62 Co2 -0.7(19) . . . . ? N42 Co2 N62 C67 145(16) . . . . ? N64 Co2 N62 C67 -3.8(12) . . . . ? N44 Co2 N62 C67 84.7(12) . . . . ? N41 Co2 N62 C67 -92.0(12) . . . . ? N61 Co2 N62 C67 176.2(12) . . . . ? N42 Co2 N62 C66 -27(17) . . . . ? N64 Co2 N62 C66 -176.4(12) . . . . ? N44 Co2 N62 C66 -88.0(12) . . . . ? N41 Co2 N62 C66 95.3(12) . . . . ? N61 Co2 N62 C66 3.6(12) . . . . ? C66 N62 C67 O62 -3(3) . . . . ? Co2 N62 C67 O62 -175.1(15) . . . . ? C66 N62 C67 C68 177.7(15) . . . . ? Co2 N62 C67 C68 5.9(18) . . . . ? O62 C67 C68 N64 175.3(15) . . . . ? N62 C67 C68 N64 -6(2) . . . . ? O62 C67 C68 C69 -2(3) . . . . ? N62 C67 C68 C69 176.6(17) . . . . ? N64 C68 C69 N63 1(3) . . . . ? C67 C68 C69 N63 179.0(18) . . . . ? C68 C69 N63 C70 -1(3) . . . . ? C69 N63 C70 C71 2(3) . . . . ? N63 C70 C71 N64 -3(2) . . . . ? C70 C71 N64 C68 3(2) . . . . ? C70 C71 N64 Co2 179.6(11) . . . . ? C69 C68 N64 C71 -2(2) . . . . ? C67 C68 N64 C71 179.7(14) . . . . ? C69 C68 N64 Co2 -179.3(14) . . . . ? C67 C68 N64 Co2 2.9(17) . . . . ? N42 Co2 N64 C71 4.9(13) . . . . ? N62 Co2 N64 C71 -176.1(13) . . . . ? N44 Co2 N64 C71 87.8(12) . . . . ? N41 Co2 N64 C71 -78.5(12) . . . . ? N61 Co2 N64 C71 -176.0(19) . . . . ? N42 Co2 N64 C68 -178.7(10) . . . . ? N62 Co2 N64 C68 0.3(10) . . . . ? N44 Co2 N64 C68 -95.8(10) . . . . ? N41 Co2 N64 C68 97.9(10) . . . . ? N61 Co2 N64 C68 0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.756 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.149 # Attachment 'mgc444final.cif' data_mgc444 _database_code_depnum_ccdc_archive 'CCDC 808583' #TrackingRef 'mgc444final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 N, Mn Cl2 C11 H7 N4 O2' _chemical_formula_sum 'C17 H23 Cl2 Mn N5 O2' _chemical_formula_weight 455.24 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' 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' Mn Mn 0.3368 0.7283 '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 7.9477(8) _cell_length_b 18.030(2) _cell_length_c 14.8985(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.695(6) _cell_angle_gamma 90.00 _cell_volume 2104.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3426 _cell_measurement_theta_min 2.259 _cell_measurement_theta_max 21.79 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8401 _exptl_absorpt_correction_T_max 0.9648 _exptl_absorpt_process_details 'SCALE(Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35200 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 24.71 _reflns_number_total 3586 _reflns_number_gt 2904 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. [Mn(pypzca)Cl2]HNEt3. Whole molecule in asym unit. All non-H atoms with occupancy greater than 0.25 were anis. All non-H atoms with occupancy 0.25 were isotropically refined. NHEt3 was modelled as a twirl disorder in two parts of 0.75 and 0.25. SADI was used to constrain the geometry of HNEt3. All atoms with occupancy >0.25 were anis. A alerts remain as a result of this disorder. The acidic proton was found from the map and fixed in position. All hydrogen atoms were calc and ride except H21 which was found from the map and fixed in position with AFIX 1. ; _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^+18.3188P] 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 3586 _refine_ls_number_parameters 274 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0972 _refine_ls_wR_factor_ref 0.2040 _refine_ls_wR_factor_gt 0.1974 _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_restrained_S_all 1.303 _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 Mn1 Mn 0.21141(15) 0.49087(7) 0.75350(9) 0.0356(4) Uani 1 1 d . . . Cl2 Cl 0.2729(3) 0.48482(13) 0.60319(15) 0.0451(6) Uani 1 1 d . . . Cl1 Cl 0.1248(3) 0.37465(12) 0.80277(16) 0.0455(6) Uani 1 1 d . . . N1 N 0.4749(8) 0.5038(4) 0.8373(5) 0.0381(16) Uani 1 1 d . . . C1 C 0.6089(10) 0.4593(5) 0.8322(6) 0.041(2) Uani 1 1 d . . . H1 H 0.5973 0.4207 0.7882 0.049 Uiso 1 1 calc R . . C2 C 0.7645(11) 0.4685(5) 0.8903(7) 0.048(2) Uani 1 1 d . . . H2 H 0.8578 0.4367 0.8855 0.057 Uiso 1 1 calc R . . C3 C 0.7821(11) 0.5237(5) 0.9543(6) 0.047(2) Uani 1 1 d . . . H3 H 0.8873 0.5305 0.9944 0.057 Uiso 1 1 calc R . . C4 C 0.6447(11) 0.5692(5) 0.9599(6) 0.045(2) Uani 1 1 d . . . H4 H 0.6536 0.6074 1.0043 0.054 Uiso 1 1 calc R . . C5 C 0.4921(11) 0.5583(5) 0.8993(6) 0.039(2) Uani 1 1 d . . . C6 C 0.3406(11) 0.6071(5) 0.9033(6) 0.042(2) Uani 1 1 d . . . O1 O 0.3566(9) 0.6607(4) 0.9549(5) 0.0557(18) Uani 1 1 d . . . N2 N 0.1996(9) 0.5859(4) 0.8432(5) 0.0428(18) Uani 1 1 d . . . C7 C 0.0508(12) 0.6233(5) 0.8408(7) 0.052(2) Uani 1 1 d . . . O2 O 0.0142(9) 0.6733(4) 0.8900(6) 0.083(3) Uani 1 1 d . . . C8 C -0.0850(11) 0.5999(5) 0.7623(6) 0.043(2) Uani 1 1 d . . . C9 C -0.2432(11) 0.6356(5) 0.7454(7) 0.049(2) Uani 1 1 d . . . H9 H -0.2652 0.6747 0.7846 0.059 Uiso 1 1 calc R . . N3 N -0.3658(9) 0.6165(5) 0.6751(6) 0.055(2) Uani 1 1 d . . . C10 C -0.3232(11) 0.5613(5) 0.6209(6) 0.043(2) Uani 1 1 d . . . H10 H -0.4043 0.5456 0.5702 0.052 Uiso 1 1 calc R . . C11 C -0.1661(10) 0.5279(5) 0.6377(6) 0.039(2) Uani 1 1 d . . . H11 H -0.1412 0.4905 0.5969 0.047 Uiso 1 1 calc R . . N4 N -0.0475(9) 0.5453(4) 0.7079(5) 0.0401(17) Uani 1 1 d . . . N21 N 0.1487(10) 0.7842(4) 1.0041(5) 0.051(2) Uani 1 1 d D . . H21 H 0.1483 0.7395 0.9790 0.061 Uiso 1 1 d . . . C21 C 0.3119(13) 0.8270(6) 0.9888(7) 0.037(3) Uani 0.75 1 d PD A 1 H21A H 0.3106 0.8770 1.0159 0.044 Uiso 0.75 1 calc PR A 1 H21B H 0.4138 0.8006 1.0209 0.044 Uiso 0.75 1 calc PR A 1 C22 C 0.3269(19) 0.8346(8) 0.8891(8) 0.042(3) Uani 0.75 1 d PD A 1 H22A H 0.3450 0.7856 0.8640 0.063 Uiso 0.75 1 calc PR A 1 H22B H 0.4236 0.8669 0.8833 0.063 Uiso 0.75 1 calc PR A 1 H22C H 0.2216 0.8563 0.8557 0.063 Uiso 0.75 1 calc PR A 1 C23 C -0.0043(14) 0.8288(6) 0.9760(9) 0.046(3) Uani 0.75 1 d PD A 1 H23A H -0.0164 0.8397 0.9101 0.055 Uiso 0.75 1 calc PR A 1 H23B H 0.0079 0.8766 1.0092 0.055 Uiso 0.75 1 calc PR A 1 C24 C -0.161(3) 0.7902(16) 0.994(2) 0.086(10) Uani 0.75 1 d PD A 1 H24A H -0.1698 0.7415 0.9646 0.130 Uiso 0.75 1 calc PR A 1 H24B H -0.2618 0.8199 0.9703 0.130 Uiso 0.75 1 calc PR A 1 H24C H -0.1545 0.7837 1.0601 0.130 Uiso 0.75 1 calc PR A 1 C25 C 0.181(2) 0.7483(10) 1.0946(10) 0.089(6) Uani 0.75 1 d PD A 1 H25A H 0.0883 0.7125 1.0983 0.106 Uiso 0.75 1 calc PR A 1 H25B H 0.2891 0.7197 1.0999 0.106 Uiso 0.75 1 calc PR A 1 C26 C 0.194(3) 0.7964(10) 1.1683(14) 0.113(7) Uani 0.75 1 d PD A 1 H26A H 0.3136 0.8103 1.1881 0.170 Uiso 0.75 1 calc PR A 1 H26B H 0.1505 0.7719 1.2185 0.170 Uiso 0.75 1 calc PR A 1 H26C H 0.1262 0.8411 1.1502 0.170 Uiso 0.75 1 calc PR A 1 C31 C 0.275(5) 0.803(2) 1.085(2) 0.073(13) Uiso 0.25 1 d PD A 2 H31A H 0.2349 0.8475 1.1148 0.088 Uiso 0.25 1 calc PR A 2 H31B H 0.3845 0.8167 1.0654 0.088 Uiso 0.25 1 calc PR A 2 C32 C 0.307(3) 0.7408(14) 1.1533(18) 0.017(5) Uiso 0.25 1 d PD A 2 H32A H 0.2235 0.7438 1.1949 0.025 Uiso 0.25 1 calc PR A 2 H32B H 0.4223 0.7448 1.1881 0.025 Uiso 0.25 1 calc PR A 2 H32C H 0.2939 0.6932 1.1212 0.025 Uiso 0.25 1 calc PR A 2 C33 C 0.099(4) 0.8410(18) 0.9328(19) 0.050(10) Uiso 0.25 1 d PD A 2 H33A H 0.0789 0.8897 0.9597 0.060 Uiso 0.25 1 calc PR A 2 H33B H -0.0041 0.8260 0.8899 0.060 Uiso 0.25 1 calc PR A 2 C34 C 0.255(4) 0.843(3) 0.886(3) 0.035(12) Uiso 0.25 1 d PD A 2 H34A H 0.3551 0.8582 0.9302 0.053 Uiso 0.25 1 calc PR A 2 H34B H 0.2359 0.8790 0.8360 0.053 Uiso 0.25 1 calc PR A 2 H34C H 0.2744 0.7939 0.8622 0.053 Uiso 0.25 1 calc PR A 2 C35 C -0.026(4) 0.775(4) 1.048(3) 0.12(2) Uiso 0.25 1 d PD A 2 H35A H -0.0237 0.7238 1.0732 0.148 Uiso 0.25 1 calc PR A 2 H35B H -0.0169 0.8092 1.0998 0.148 Uiso 0.25 1 calc PR A 2 C36 C -0.198(7) 0.785(5) 0.993(5) 0.049(17) Uiso 0.25 1 d PD A 2 H36A H -0.2048 0.8342 0.9643 0.073 Uiso 0.25 1 calc PR A 2 H36B H -0.2842 0.7818 1.0331 0.073 Uiso 0.25 1 calc PR A 2 H36C H -0.2198 0.7468 0.9462 0.073 Uiso 0.25 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0283(7) 0.0328(7) 0.0436(8) -0.0034(6) 0.0000(5) 0.0003(5) Cl2 0.0337(11) 0.0554(14) 0.0464(13) -0.0018(11) 0.0069(9) -0.0058(10) Cl1 0.0409(12) 0.0407(12) 0.0541(14) 0.0036(11) 0.0054(10) -0.0034(9) N1 0.035(4) 0.040(4) 0.038(4) 0.000(3) 0.001(3) -0.003(3) C1 0.035(5) 0.038(5) 0.051(6) 0.000(4) 0.008(4) -0.001(4) C2 0.035(5) 0.047(6) 0.062(6) 0.013(5) 0.007(4) 0.002(4) C3 0.038(5) 0.052(6) 0.046(6) 0.007(5) -0.007(4) -0.012(4) C4 0.042(5) 0.053(6) 0.036(5) 0.009(4) -0.001(4) -0.017(4) C5 0.037(5) 0.039(5) 0.039(5) -0.001(4) 0.004(4) -0.005(4) C6 0.046(5) 0.039(5) 0.041(5) 0.004(4) 0.009(4) -0.004(4) O1 0.063(4) 0.044(4) 0.057(4) -0.018(3) 0.003(3) -0.005(3) N2 0.037(4) 0.036(4) 0.051(5) -0.008(4) -0.004(3) 0.000(3) C7 0.050(6) 0.042(6) 0.064(7) -0.010(5) 0.010(5) 0.004(4) O2 0.055(5) 0.069(5) 0.117(7) -0.050(5) -0.008(5) 0.015(4) C8 0.035(5) 0.034(5) 0.057(6) -0.009(4) 0.004(4) 0.000(4) C9 0.040(5) 0.044(5) 0.066(7) -0.004(5) 0.017(5) 0.002(4) N3 0.036(4) 0.061(5) 0.064(6) 0.009(5) 0.002(4) -0.003(4) C10 0.035(5) 0.054(6) 0.041(5) 0.001(4) 0.008(4) -0.008(4) C11 0.036(5) 0.040(5) 0.040(5) 0.001(4) 0.005(4) -0.004(4) N4 0.036(4) 0.039(4) 0.045(4) 0.005(4) 0.004(3) -0.002(3) N21 0.070(6) 0.037(4) 0.044(5) 0.006(4) 0.005(4) -0.003(4) C21 0.038(6) 0.047(7) 0.025(6) -0.002(5) 0.005(5) -0.007(5) C22 0.039(9) 0.054(9) 0.033(7) 0.009(6) 0.006(6) 0.000(7) C23 0.040(7) 0.030(6) 0.072(10) -0.010(6) 0.019(6) -0.001(5) C24 0.078(16) 0.053(12) 0.15(2) -0.017(11) 0.082(16) 0.007(12) C25 0.110(15) 0.103(14) 0.064(11) 0.023(11) 0.046(11) -0.019(12) C26 0.17(2) 0.075(13) 0.104(17) 0.007(12) 0.038(15) -0.015(14) _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 Mn1 N2 2.184(7) . ? Mn1 N1 2.262(7) . ? Mn1 N4 2.278(7) . ? Mn1 Cl1 2.361(3) . ? Mn1 Cl2 2.374(3) . ? N1 C5 1.339(10) . ? N1 C1 1.347(11) . ? C1 C2 1.394(12) . ? C2 C3 1.369(13) . ? C3 C4 1.379(13) . ? C4 C5 1.398(11) . ? C5 C6 1.501(12) . ? C6 O1 1.227(10) . ? C6 N2 1.367(11) . ? N2 C7 1.356(11) . ? C7 O2 1.227(11) . ? C7 C8 1.512(13) . ? C8 N4 1.340(11) . ? C8 C9 1.398(12) . ? C9 N3 1.349(12) . ? N3 C10 1.360(12) . ? C10 C11 1.372(12) . ? C11 N4 1.323(10) . ? N21 C23 1.459(12) . ? N21 C31 1.48(2) . ? N21 C33 1.48(2) . ? N21 C25 1.480(14) . ? N21 C21 1.558(12) . ? N21 C35 1.64(3) . ? C21 C22 1.515(15) . ? C23 C24 1.49(2) . ? C25 C26 1.39(2) . ? C31 C32 1.51(3) . ? C33 C34 1.52(3) . ? C35 C36 1.48(3) . ? 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 N2 Mn1 N1 73.3(3) . . ? N2 Mn1 N4 73.4(3) . . ? N1 Mn1 N4 145.7(3) . . ? N2 Mn1 Cl1 117.5(2) . . ? N1 Mn1 Cl1 102.19(19) . . ? N4 Mn1 Cl1 100.32(19) . . ? N2 Mn1 Cl2 130.5(2) . . ? N1 Mn1 Cl2 101.94(19) . . ? N4 Mn1 Cl2 93.3(2) . . ? Cl1 Mn1 Cl2 111.70(10) . . ? C5 N1 C1 119.1(7) . . ? C5 N1 Mn1 115.7(5) . . ? C1 N1 Mn1 125.1(6) . . ? N1 C1 C2 121.4(8) . . ? C3 C2 C1 119.7(9) . . ? C2 C3 C4 119.0(8) . . ? C3 C4 C5 119.2(9) . . ? N1 C5 C4 121.6(8) . . ? N1 C5 C6 117.9(7) . . ? C4 C5 C6 120.4(8) . . ? O1 C6 N2 128.2(9) . . ? O1 C6 C5 119.2(8) . . ? N2 C6 C5 112.6(8) . . ? C7 N2 C6 119.5(8) . . ? C7 N2 Mn1 120.1(6) . . ? C6 N2 Mn1 120.4(6) . . ? O2 C7 N2 130.0(9) . . ? O2 C7 C8 117.1(9) . . ? N2 C7 C8 112.8(8) . . ? N4 C8 C9 121.0(8) . . ? N4 C8 C7 118.1(8) . . ? C9 C8 C7 121.0(8) . . ? N3 C9 C8 122.2(9) . . ? C9 N3 C10 115.4(8) . . ? N3 C10 C11 121.5(8) . . ? N4 C11 C10 123.1(9) . . ? C11 N4 C8 116.8(8) . . ? C11 N4 Mn1 128.4(6) . . ? C8 N4 Mn1 114.7(6) . . ? C23 N21 C31 121.7(19) . . ? C23 N21 C33 46.0(12) . . ? C31 N21 C33 119.1(18) . . ? C23 N21 C25 120.8(10) . . ? C31 N21 C25 50.7(15) . . ? C33 N21 C25 160.4(17) . . ? C23 N21 C21 111.1(8) . . ? C31 N21 C21 62.2(15) . . ? C33 N21 C21 71.3(13) . . ? C25 N21 C21 109.1(9) . . ? C23 N21 C35 56.7(19) . . ? C31 N21 C35 102.1(19) . . ? C33 N21 C35 102.6(18) . . ? C25 N21 C35 67.9(17) . . ? C21 N21 C35 153(3) . . ? C22 C21 N21 113.1(9) . . ? N21 C23 C24 111.8(13) . . ? C26 C25 N21 115.1(16) . . ? N21 C31 C32 113(2) . . ? N21 C33 C34 102(3) . . ? C36 C35 N21 122(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Mn1 N1 C5 2.2(6) . . . . ? N4 Mn1 N1 C5 16.8(8) . . . . ? Cl1 Mn1 N1 C5 -113.1(6) . . . . ? Cl2 Mn1 N1 C5 131.3(6) . . . . ? N2 Mn1 N1 C1 178.7(7) . . . . ? N4 Mn1 N1 C1 -166.8(6) . . . . ? Cl1 Mn1 N1 C1 63.3(7) . . . . ? Cl2 Mn1 N1 C1 -52.3(7) . . . . ? C5 N1 C1 C2 0.2(13) . . . . ? Mn1 N1 C1 C2 -176.1(6) . . . . ? N1 C1 C2 C3 0.4(14) . . . . ? C1 C2 C3 C4 -0.1(14) . . . . ? C2 C3 C4 C5 -0.8(13) . . . . ? C1 N1 C5 C4 -1.1(12) . . . . ? Mn1 N1 C5 C4 175.6(6) . . . . ? C1 N1 C5 C6 179.9(8) . . . . ? Mn1 N1 C5 C6 -3.4(10) . . . . ? C3 C4 C5 N1 1.4(13) . . . . ? C3 C4 C5 C6 -179.7(8) . . . . ? N1 C5 C6 O1 -174.8(8) . . . . ? C4 C5 C6 O1 6.3(13) . . . . ? N1 C5 C6 N2 2.8(11) . . . . ? C4 C5 C6 N2 -176.2(8) . . . . ? O1 C6 N2 C7 -4.8(15) . . . . ? C5 C6 N2 C7 177.9(8) . . . . ? O1 C6 N2 Mn1 176.5(7) . . . . ? C5 C6 N2 Mn1 -0.7(10) . . . . ? N1 Mn1 N2 C7 -179.3(8) . . . . ? N4 Mn1 N2 C7 9.2(7) . . . . ? Cl1 Mn1 N2 C7 -84.0(7) . . . . ? Cl2 Mn1 N2 C7 89.1(8) . . . . ? N1 Mn1 N2 C6 -0.7(6) . . . . ? N4 Mn1 N2 C6 -172.2(7) . . . . ? Cl1 Mn1 N2 C6 94.6(7) . . . . ? Cl2 Mn1 N2 C6 -92.3(7) . . . . ? C6 N2 C7 O2 -5.4(17) . . . . ? Mn1 N2 C7 O2 173.2(10) . . . . ? C6 N2 C7 C8 172.0(8) . . . . ? Mn1 N2 C7 C8 -9.4(11) . . . . ? O2 C7 C8 N4 -179.9(9) . . . . ? N2 C7 C8 N4 2.3(13) . . . . ? O2 C7 C8 C9 1.9(15) . . . . ? N2 C7 C8 C9 -175.9(9) . . . . ? N4 C8 C9 N3 1.0(15) . . . . ? C7 C8 C9 N3 179.1(9) . . . . ? C8 C9 N3 C10 -1.4(13) . . . . ? C9 N3 C10 C11 0.2(13) . . . . ? N3 C10 C11 N4 1.6(14) . . . . ? C10 C11 N4 C8 -2.0(13) . . . . ? C10 C11 N4 Mn1 174.9(6) . . . . ? C9 C8 N4 C11 0.7(13) . . . . ? C7 C8 N4 C11 -177.4(8) . . . . ? C9 C8 N4 Mn1 -176.6(7) . . . . ? C7 C8 N4 Mn1 5.2(11) . . . . ? N2 Mn1 N4 C11 175.7(8) . . . . ? N1 Mn1 N4 C11 161.1(6) . . . . ? Cl1 Mn1 N4 C11 -68.6(7) . . . . ? Cl2 Mn1 N4 C11 44.2(7) . . . . ? N2 Mn1 N4 C8 -7.3(6) . . . . ? N1 Mn1 N4 C8 -21.9(9) . . . . ? Cl1 Mn1 N4 C8 108.5(6) . . . . ? Cl2 Mn1 N4 C8 -138.8(6) . . . . ? C23 N21 C21 C22 -71.4(12) . . . . ? C31 N21 C21 C22 173(2) . . . . ? C33 N21 C21 C22 -47.8(17) . . . . ? C25 N21 C21 C22 152.9(12) . . . . ? C35 N21 C21 C22 -129(4) . . . . ? C31 N21 C23 C24 -108(2) . . . . ? C33 N21 C23 C24 151(3) . . . . ? C25 N21 C23 C24 -47.6(19) . . . . ? C21 N21 C23 C24 -177.3(15) . . . . ? C35 N21 C23 C24 -24(3) . . . . ? C23 N21 C25 C26 -60(2) . . . . ? C31 N21 C25 C26 48(3) . . . . ? C33 N21 C25 C26 -17(5) . . . . ? C21 N21 C25 C26 70.7(18) . . . . ? C35 N21 C25 C26 -81(3) . . . . ? C23 N21 C31 C32 124(3) . . . . ? C33 N21 C31 C32 177(3) . . . . ? C25 N21 C31 C32 18(2) . . . . ? C21 N21 C31 C32 -138(4) . . . . ? C35 N21 C31 C32 66(4) . . . . ? C23 N21 C33 C34 -178(4) . . . . ? C31 N21 C33 C34 74(4) . . . . ? C25 N21 C33 C34 128(4) . . . . ? C21 N21 C33 C34 33(2) . . . . ? C35 N21 C33 C34 -174(3) . . . . ? C23 N21 C35 C36 34(5) . . . . ? C31 N21 C35 C36 154(6) . . . . ? C33 N21 C35 C36 31(7) . . . . ? C25 N21 C35 C36 -167(7) . . . . ? C21 N21 C35 C36 104(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.548 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.098 # Attachment 'mgc447 Final.cif' data_mgc447 _database_code_depnum_ccdc_archive 'CCDC 808584' #TrackingRef 'mgc447 Final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H14 N8 O4 Cu, O0.75 H1.5' _chemical_formula_sum 'C22 H15.50 Cu N8 O4.75' _chemical_formula_weight 531.46 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' O O 0.0106 0.0060 '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' _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 9.3128(4) _cell_length_b 8.5744(3) _cell_length_c 28.3561(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.046(2) _cell_angle_gamma 90.00 _cell_volume 2247.18(16) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8190 _cell_measurement_theta_min 4.2335 _cell_measurement_theta_max 25.873 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1082 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7487 _exptl_absorpt_correction_T_max 0.9045 _exptl_absorpt_process_details 'SCALE(Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38121 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4588 _reflns_number_gt 3751 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. [Cu(C11H7N4O2)2].0.75H2O. Entire complex in asym unit. For main residue all non-H anis and all H calc and ride. SQUEEZE was used to show that there was approx one, badly disordered, water of crystallisation, but please note that SQUEEZE was not applied to the present dataset. Rather, this water was modelled in two parts of 0.50 (O41) and 0.25 (O51). Despite Q1 and Q2 occurring in the same region of space as O41 and O51, attempts to insert a further 0.25 occupancy water were unsuccessful, as this tended to upset O41(ANIS) and O51 (isotropic). As a result there is B Alert for the ratio of remaining electron density (Q1 1.80; Q2 1.21, 0.75 and 0.49 A from O51, resp; Q3 is 0.76 and min is -0.34). Hydrogen atoms on O41 and O51 were found from the map and HIMP'd, then fixed in position with AFIX 01, whilst U(H)=1.2U(O). ; _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^)+(0.0782P)^2^+4.4435P] 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 4588 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Cu1 Cu 0.05298(4) 0.53931(4) 0.133828(13) 0.01984(15) Uani 1 1 d . . . N1 N -0.0328(3) 0.3143(3) 0.12690(10) 0.0233(6) Uani 1 1 d . . . C1 C -0.0142(4) 0.1929(4) 0.15677(13) 0.0282(8) Uani 1 1 d . . . H1 H 0.0498 0.2028 0.1854 0.034 Uiso 1 1 calc R . . C2 C -0.0862(4) 0.0539(4) 0.14671(14) 0.0304(8) Uani 1 1 d . . . H2 H -0.0707 -0.0297 0.1687 0.036 Uiso 1 1 calc R . . N2 N -0.1774(4) 0.0333(4) 0.10676(13) 0.0383(8) Uani 1 1 d . . . C3 C -0.1947(4) 0.1567(5) 0.07583(14) 0.0331(8) Uani 1 1 d . . . H3 H -0.2574 0.1466 0.0469 0.040 Uiso 1 1 calc R . . C4 C -0.1218(4) 0.2962(4) 0.08622(12) 0.0246(7) Uani 1 1 d . . . C5 C -0.1375(4) 0.4336(4) 0.05266(12) 0.0261(7) Uani 1 1 d . . . N3 N -0.0472(3) 0.5535(3) 0.06905(10) 0.0236(6) Uani 1 1 d . . . C6 C -0.0278(4) 0.6835(4) 0.04293(12) 0.0251(7) Uani 1 1 d . . . O1 O -0.2238(3) 0.4280(4) 0.01676(9) 0.0395(7) Uani 1 1 d . . . O2 O -0.0860(3) 0.7182(3) 0.00327(9) 0.0398(7) Uani 1 1 d . . . C7 C 0.0824(4) 0.7921(4) 0.06911(12) 0.0243(7) Uani 1 1 d . . . C8 C 0.1343(4) 0.9205(5) 0.04700(14) 0.0335(9) Uani 1 1 d . . . H8 H 0.1022 0.9410 0.0145 0.040 Uiso 1 1 calc R . . C9 C 0.2331(5) 1.0192(4) 0.07235(14) 0.0339(9) Uani 1 1 d . . . H9 H 0.2701 1.1078 0.0577 0.041 Uiso 1 1 calc R . . C10 C 0.2757(4) 0.9855(4) 0.11888(14) 0.0325(9) Uani 1 1 d . . . H10 H 0.3427 1.0515 0.1373 0.039 Uiso 1 1 calc R . . C11 C 0.2213(4) 0.8547(4) 0.13942(12) 0.0269(7) Uani 1 1 d . . . H11 H 0.2516 0.8332 0.1720 0.032 Uiso 1 1 calc R . . N4 N 0.1275(3) 0.7581(3) 0.11482(9) 0.0222(6) Uani 1 1 d . . . N21 N 0.2794(3) 0.4475(3) 0.12782(10) 0.0224(6) Uani 1 1 d . . . C21 C 0.3478(4) 0.4109(4) 0.09070(12) 0.0281(8) Uani 1 1 d . . . H21 H 0.2978 0.4194 0.0595 0.034 Uiso 1 1 calc R . . C22 C 0.4901(4) 0.3608(5) 0.09669(14) 0.0342(9) Uani 1 1 d . . . H22 H 0.5354 0.3357 0.0694 0.041 Uiso 1 1 calc R . . N22 N 0.5663(4) 0.3466(4) 0.14007(12) 0.0393(8) Uani 1 1 d . . . C23 C 0.4967(4) 0.3858(4) 0.17729(13) 0.0292(8) Uani 1 1 d . . . H23 H 0.5467 0.3787 0.2085 0.035 Uiso 1 1 calc R . . C24 C 0.3547(4) 0.4359(4) 0.17128(12) 0.0226(7) Uani 1 1 d . . . C25 C 0.2794(4) 0.4796(4) 0.21379(12) 0.0253(7) Uani 1 1 d . . . O21 O 0.3495(3) 0.4772(4) 0.25337(9) 0.0414(7) Uani 1 1 d . . . N23 N 0.1373(3) 0.5218(3) 0.20201(10) 0.0219(6) Uani 1 1 d . . . C26 C 0.0484(4) 0.5426(4) 0.23702(12) 0.0256(7) Uani 1 1 d . . . O22 O 0.0747(3) 0.5135(4) 0.27940(9) 0.0418(7) Uani 1 1 d . . . C27 C -0.0998(4) 0.6068(4) 0.21873(12) 0.0239(7) Uani 1 1 d . . . C28 C -0.1992(4) 0.6392(4) 0.25042(13) 0.0299(8) Uani 1 1 d . . . H28 H -0.1777 0.6147 0.2832 0.036 Uiso 1 1 calc R . . C29 C -0.3287(4) 0.7070(4) 0.23343(15) 0.0340(9) Uani 1 1 d . . . H29 H -0.3972 0.7326 0.2544 0.041 Uiso 1 1 calc R . . C30 C -0.3579(4) 0.7373(5) 0.18564(16) 0.0380(9) Uani 1 1 d . . . H30 H -0.4459 0.7862 0.1731 0.046 Uiso 1 1 calc R . . C31 C -0.2564(4) 0.6953(4) 0.15602(14) 0.0330(9) Uani 1 1 d . . . H31 H -0.2785 0.7123 0.1228 0.040 Uiso 1 1 calc R . . N24 N -0.1286(3) 0.6318(3) 0.17222(10) 0.0252(6) Uani 1 1 d . . . O41 O -0.4620(8) 0.7612(10) 0.0362(2) 0.065(2) Uani 0.50 1 d P A 1 H41X H -0.4187 0.7640 0.0117 0.078 Uiso 0.50 1 d P B 1 H41Y H -0.5568 0.7564 0.0203 0.078 Uiso 0.50 1 d P C 1 O51 O -0.4667(12) 0.8714(13) -0.0042(4) 0.038(3) Uiso 0.25 1 d P D 2 H51X H -0.4068 0.9368 0.0069 0.046 Uiso 0.25 1 d P E 2 H51Y H -0.4598 0.8012 0.0187 0.046 Uiso 0.25 1 d P F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0244(2) 0.0186(2) 0.0152(2) 0.00135(15) -0.00263(16) 0.00019(15) N1 0.0226(15) 0.0233(14) 0.0229(14) -0.0009(11) -0.0018(11) 0.0018(11) C1 0.0293(19) 0.0286(18) 0.0261(18) 0.0036(14) 0.0005(15) 0.0020(15) C2 0.035(2) 0.0259(18) 0.031(2) 0.0040(15) 0.0033(16) 0.0001(15) N2 0.0385(19) 0.0286(17) 0.048(2) -0.0054(15) 0.0056(16) -0.0032(14) C3 0.030(2) 0.034(2) 0.034(2) -0.0115(16) 0.0003(16) -0.0045(16) C4 0.0220(17) 0.0273(17) 0.0241(17) -0.0050(14) 0.0010(13) 0.0006(14) C5 0.0250(18) 0.0333(19) 0.0188(16) -0.0035(14) -0.0020(14) 0.0028(14) N3 0.0269(15) 0.0267(15) 0.0162(13) 0.0016(11) -0.0013(11) 0.0023(12) C6 0.0251(18) 0.0313(18) 0.0184(16) 0.0047(14) 0.0003(13) 0.0059(14) O1 0.0380(16) 0.0507(17) 0.0255(14) 0.0016(12) -0.0134(12) -0.0057(13) O2 0.0411(16) 0.0509(17) 0.0239(13) 0.0150(12) -0.0103(12) -0.0017(13) C7 0.0286(18) 0.0244(17) 0.0195(16) 0.0036(13) 0.0021(14) 0.0078(14) C8 0.042(2) 0.0327(19) 0.0255(18) 0.0117(16) 0.0010(16) 0.0034(17) C9 0.046(2) 0.0256(18) 0.030(2) 0.0094(15) 0.0034(17) -0.0046(16) C10 0.039(2) 0.0258(18) 0.029(2) -0.0022(15) -0.0074(16) -0.0015(16) C11 0.0298(19) 0.0285(18) 0.0214(17) -0.0004(14) -0.0015(14) 0.0046(15) N4 0.0261(15) 0.0216(13) 0.0186(14) 0.0026(11) 0.0018(11) 0.0044(11) N21 0.0254(15) 0.0209(13) 0.0196(14) 0.0018(11) -0.0031(11) -0.0014(11) C21 0.035(2) 0.0289(18) 0.0198(17) -0.0009(14) 0.0003(14) -0.0005(15) C22 0.035(2) 0.039(2) 0.0289(19) -0.0035(16) 0.0035(16) 0.0008(17) N22 0.0354(19) 0.0431(19) 0.0388(19) -0.0049(16) 0.0014(15) 0.0039(15) C23 0.0292(19) 0.0282(18) 0.0279(18) -0.0004(15) -0.0059(15) 0.0008(15) C24 0.0270(18) 0.0186(15) 0.0205(16) 0.0027(12) -0.0037(13) -0.0033(13) C25 0.0277(18) 0.0274(17) 0.0191(17) 0.0021(13) -0.0037(14) -0.0013(14) O21 0.0330(15) 0.069(2) 0.0203(13) 0.0001(13) -0.0062(11) 0.0031(14) N23 0.0262(15) 0.0215(13) 0.0172(13) 0.0015(11) -0.0001(11) -0.0009(11) C26 0.0299(19) 0.0248(17) 0.0211(17) 0.0003(13) -0.0009(14) -0.0021(14) O22 0.0406(17) 0.067(2) 0.0180(13) 0.0103(13) 0.0031(12) 0.0067(14) C27 0.0311(18) 0.0188(15) 0.0214(16) 0.0005(13) 0.0018(14) -0.0040(14) C28 0.034(2) 0.0299(18) 0.0262(18) -0.0016(15) 0.0061(15) -0.0047(16) C29 0.031(2) 0.0316(19) 0.042(2) -0.0020(17) 0.0130(17) -0.0005(16) C30 0.0254(19) 0.0297(19) 0.058(3) 0.0066(18) 0.0002(18) 0.0015(16) C31 0.033(2) 0.0293(18) 0.034(2) 0.0075(16) -0.0045(16) -0.0024(16) N24 0.0298(16) 0.0225(14) 0.0222(14) 0.0019(11) -0.0014(12) -0.0015(12) O41 0.057(4) 0.098(6) 0.032(3) -0.001(4) -0.026(3) 0.014(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 Cu1 N3 1.959(3) . ? Cu1 N23 2.001(3) . ? Cu1 N1 2.088(3) . ? Cu1 N4 2.094(3) . ? Cu1 N24 2.264(3) . ? Cu1 N21 2.276(3) . ? N1 C1 1.339(4) . ? N1 C4 1.344(4) . ? C1 C2 1.381(5) . ? C1 H1 0.9500 . ? C2 N2 1.341(5) . ? C2 H2 0.9500 . ? N2 C3 1.371(5) . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C5 1.510(5) . ? C5 O1 1.218(4) . ? C5 N3 1.372(5) . ? N3 C6 1.362(4) . ? C6 O2 1.224(4) . ? C6 C7 1.512(5) . ? C7 N4 1.344(4) . ? C7 C8 1.383(5) . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 C10 1.361(5) . ? C9 H9 0.9500 . ? C10 C11 1.388(5) . ? C10 H10 0.9500 . ? C11 N4 1.337(4) . ? C11 H11 0.9500 . ? N21 C21 1.333(5) . ? N21 C24 1.345(4) . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 N22 1.348(5) . ? C22 H22 0.9500 . ? N22 C23 1.347(5) . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.514(5) . ? C25 O21 1.228(4) . ? C25 N23 1.373(5) . ? N23 C26 1.380(5) . ? C26 O22 1.222(4) . ? C26 C27 1.517(5) . ? C27 N24 1.331(4) . ? C27 C28 1.395(5) . ? C28 C29 1.372(5) . ? C28 H28 0.9500 . ? C29 C30 1.374(6) . ? C29 H29 0.9500 . ? C30 C31 1.387(6) . ? C30 H30 0.9500 . ? C31 N24 1.338(5) . ? C31 H31 0.9500 . ? O41 H41X 0.8450 . ? O41 H41Y 0.9421 . ? O41 H51Y 0.6055 . ? O51 H41X 1.0962 . ? O51 H51X 0.8251 . ? O51 H51Y 0.8820 . ? 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 N3 Cu1 N23 174.67(12) . . ? N3 Cu1 N1 80.59(11) . . ? N23 Cu1 N1 96.99(11) . . ? N3 Cu1 N4 80.66(11) . . ? N23 Cu1 N4 102.30(11) . . ? N1 Cu1 N4 159.84(11) . . ? N3 Cu1 N24 97.53(11) . . ? N23 Cu1 N24 77.84(11) . . ? N1 Cu1 N24 93.99(11) . . ? N4 Cu1 N24 95.75(11) . . ? N3 Cu1 N21 106.88(11) . . ? N23 Cu1 N21 77.83(11) . . ? N1 Cu1 N21 91.18(10) . . ? N4 Cu1 N21 87.21(10) . . ? N24 Cu1 N21 155.56(10) . . ? C1 N1 C4 118.1(3) . . ? C1 N1 Cu1 129.8(2) . . ? C4 N1 Cu1 112.1(2) . . ? N1 C1 C2 121.2(3) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? N2 C2 C1 122.0(3) . . ? N2 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 N2 C3 116.8(3) . . ? N2 C3 C4 120.8(3) . . ? N2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? N1 C4 C3 121.0(3) . . ? N1 C4 C5 116.9(3) . . ? C3 C4 C5 122.1(3) . . ? O1 C5 N3 128.8(3) . . ? O1 C5 C4 119.9(3) . . ? N3 C5 C4 111.3(3) . . ? C6 N3 C5 123.0(3) . . ? C6 N3 Cu1 118.7(2) . . ? C5 N3 Cu1 118.2(2) . . ? O2 C6 N3 128.7(3) . . ? O2 C6 C7 119.9(3) . . ? N3 C6 C7 111.4(3) . . ? N4 C7 C8 121.6(3) . . ? N4 C7 C6 116.9(3) . . ? C8 C7 C6 121.5(3) . . ? C7 C8 C9 119.9(3) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 118.0(4) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? N4 C11 C10 122.0(3) . . ? N4 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 N4 C7 118.4(3) . . ? C11 N4 Cu1 129.6(2) . . ? C7 N4 Cu1 111.6(2) . . ? C21 N21 C24 117.4(3) . . ? C21 N21 Cu1 132.6(2) . . ? C24 N21 Cu1 109.9(2) . . ? N21 C21 C22 121.3(3) . . ? N21 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? N22 C22 C21 122.0(4) . . ? N22 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C23 N22 C22 116.3(3) . . ? N22 C23 C24 121.8(3) . . ? N22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? N21 C24 C23 121.3(3) . . ? N21 C24 C25 118.1(3) . . ? C23 C24 C25 120.6(3) . . ? O21 C25 N23 128.0(3) . . ? O21 C25 C24 118.5(3) . . ? N23 C25 C24 113.5(3) . . ? C25 N23 C26 120.3(3) . . ? C25 N23 Cu1 120.5(2) . . ? C26 N23 Cu1 119.1(2) . . ? O22 C26 N23 128.0(3) . . ? O22 C26 C27 118.3(3) . . ? N23 C26 C27 113.7(3) . . ? N24 C27 C28 122.5(3) . . ? N24 C27 C26 117.5(3) . . ? C28 C27 C26 120.0(3) . . ? C29 C28 C27 118.9(3) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 119.1(4) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 118.8(4) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N24 C31 C30 122.8(4) . . ? N24 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C27 N24 C31 118.0(3) . . ? C27 N24 Cu1 110.4(2) . . ? C31 N24 Cu1 131.5(3) . . ? H41X O41 H41Y 97.0 . . ? H41X O41 H51Y 40.8 . . ? H41Y O41 H51Y 75.9 . . ? H41X O51 H51X 101.1 . . ? H41X O51 H51Y 30.1 . . ? H51X O51 H51Y 101.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.803 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.104