Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global loop_ _publ_author_name 'Delgado, Rita' 'Branco, Luis' 'Costa, Judite ' 'Drew, Michael G.B.' 'Felix, Vitor ' 'Goodfellow, Brian J.' _publ_requested_journal 'Dalton Transactions' _journal_coden_Cambridge 186 ; _publ_contact_author_phone '[351]234 370 729' _publ_contact_author_email vfelix@dq.ua.pt _publ_contact_author_name 'Prof. V. Felix' _publ_contact_author_adress ; Departamento de Quimica Universidade de Aveiro 3810-193 Aveiro Portugal ; #------------------------- data section of block--------------------------- #==BEGIN data_compound [Ni([18]py2N4](ClO4)2.CH3CN 1 _database_code_CSD 185052 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 Cl2 N8 Ni O8' _chemical_formula_weight 666.17 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' 'Ni' 'Ni' 0.3393 1.1124 '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 C2/c 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 20.023(27) _cell_length_b 15.041(18) _cell_length_c 11.869(14) _cell_angle_alpha 90.00 _cell_angle_beta 123.33(1) _cell_angle_gamma 90.00 _cell_volume 2987(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _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 4417 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.17 _reflns_number_total 2686 _reflns_number_gt 1554 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1961P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2686 _refine_ls_number_parameters 182 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1461 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2981 _refine_ls_wR_factor_gt 0.2609 _refine_ls_goodness_of_fit_ref 1.055 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.77400(7) 0.7500 0.0536(5) Uani 1 d S . . N1 N 0.4368(4) 0.7427(4) 0.5384(6) 0.0719(17) Uani 1 d . . . H1 H 0.3995 0.7851 0.4887 0.086 Uiso 1 calc R . . C2 C 0.3989(5) 0.6552(5) 0.5137(8) 0.074(2) Uani 1 d . . . H2A H 0.3927 0.6286 0.4340 0.088 Uiso 1 calc R . . H2B H 0.3463 0.6613 0.4985 0.088 Uiso 1 calc R . . C3 C 0.4510(4) 0.5962(4) 0.6356(7) 0.0604(17) Uani 1 d . . . N4 N 0.5000 0.6388(5) 0.7500 0.0577(19) Uani 1 d S . . N13 N 0.5000 0.9085(5) 0.7500 0.0511(17) Uani 1 d S . . C14 C 0.5622(3) 0.9527(4) 0.7621(7) 0.0546(16) Uani 1 d . . . C15 C 0.6274(4) 0.8933(5) 0.7779(9) 0.068(2) Uani 1 d . . . H15A H 0.6501 0.9194 0.7314 0.082 Uiso 1 calc R . . H15B H 0.6695 0.8881 0.8726 0.082 Uiso 1 calc R . . N16 N 0.5956(3) 0.8044(4) 0.7220(6) 0.0662(16) Uani 1 d . . . H16 H 0.6347 0.7623 0.7606 0.079 Uiso 1 calc R . . C17 C 0.5585(6) 0.8103(9) 0.5721(12) 0.105(3) Uani 1 d . . . H17A H 0.5326 0.8676 0.5390 0.126 Uiso 1 calc R . . H17B H 0.5996 0.8049 0.5531 0.126 Uiso 1 calc R . . C18 C 0.5010(6) 0.7408(8) 0.5056(9) 0.092(3) Uani 1 d . . . H18A H 0.5282 0.6839 0.5327 0.111 Uiso 1 calc R . . H18B H 0.4755 0.7466 0.4089 0.111 Uiso 1 calc R . . C21 C 0.4507(5) 0.5040(5) 0.6314(10) 0.084(3) Uani 1 d . . . H21 H 0.4180 0.4740 0.5504 0.101 Uiso 1 calc R . . C22 C 0.5000 0.4572(7) 0.7500 0.083(4) Uani 1 d S . . H22 H 0.5000 0.3954 0.7500 0.100 Uiso 1 calc SR . . C31 C 0.5631(4) 1.0448(5) 0.7619(8) 0.0670(19) Uani 1 d . . . H31 H 0.6059 1.0753 0.7697 0.080 Uiso 1 calc R . . C32 C 0.5000 1.0905(7) 0.7500 0.073(3) Uani 1 d S . . H32 H 0.5000 1.1523 0.7500 0.087 Uiso 1 calc SR . . N100 N 0.1231(5) 0.7719(5) 0.8626(10) 0.102(3) Uani 1 d . . . C101 C 0.1714(5) 0.8207(5) 0.8847(9) 0.078(2) Uani 1 d . . . C102 C 0.2327(6) 0.8829(7) 0.9111(13) 0.106(4) Uani 1 d . . . H10A H 0.2840 0.8594 0.9793 0.127 Uiso 1 calc R . . H10B H 0.2239 0.9381 0.9416 0.127 Uiso 1 calc R . . H10C H 0.2313 0.8929 0.8299 0.127 Uiso 1 calc R . . Cl1 Cl 0.25328(10) 0.61984(12) 0.7083(2) 0.0695(6) Uani 1 d D . . O11 O 0.1745(7) 0.5865(10) 0.6034(13) 0.122(3) Uiso 0.613(15) d PD . . O21 O 0.2440(8) 0.7114(7) 0.7254(15) 0.122(3) Uiso 0.613(15) d PD . . O31 O 0.3033(7) 0.6131(9) 0.6595(14) 0.122(3) Uiso 0.613(15) d PD . . O41 O 0.2770(8) 0.5648(8) 0.8189(11) 0.122(3) Uiso 0.613(15) d PD . . O12 O 0.1848(11) 0.5693(15) 0.633(2) 0.148(7) Uiso 0.387(15) d PD . . O22 O 0.2468(14) 0.6834(15) 0.790(2) 0.148(7) Uiso 0.387(15) d PD . . O32 O 0.2613(14) 0.6749(15) 0.612(2) 0.148(7) Uiso 0.387(15) d PD . . O42 O 0.3247(10) 0.5719(14) 0.776(2) 0.148(7) Uiso 0.387(15) d PD . . 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 Ni1 0.0486(7) 0.0494(7) 0.0559(8) 0.000 0.0243(5) 0.000 N1 0.064(3) 0.076(4) 0.054(3) 0.010(3) 0.019(3) 0.002(3) C2 0.070(4) 0.078(5) 0.059(4) 0.001(4) 0.027(3) -0.010(4) C3 0.056(3) 0.051(3) 0.063(4) -0.007(3) 0.025(3) -0.003(3) N4 0.056(4) 0.056(4) 0.051(4) 0.000 0.023(3) 0.000 N13 0.049(4) 0.048(4) 0.060(5) 0.000 0.032(3) 0.000 C14 0.052(3) 0.056(4) 0.058(4) 0.001(3) 0.031(3) -0.002(3) C15 0.054(3) 0.075(5) 0.091(6) 0.005(4) 0.050(4) 0.001(3) N16 0.051(3) 0.075(4) 0.067(4) -0.003(3) 0.030(3) 0.012(3) C17 0.106(7) 0.134(8) 0.110(8) -0.014(7) 0.082(6) -0.001(6) C18 0.085(6) 0.128(8) 0.056(5) -0.002(5) 0.034(4) -0.021(5) C21 0.069(4) 0.066(5) 0.093(6) -0.016(4) 0.030(4) -0.006(3) C22 0.069(6) 0.052(5) 0.128(11) 0.000 0.053(7) 0.000 C31 0.073(4) 0.057(4) 0.070(5) 0.006(3) 0.039(4) -0.008(3) C32 0.080(7) 0.052(5) 0.094(8) 0.000 0.052(6) 0.000 N100 0.101(6) 0.085(5) 0.113(7) -0.009(4) 0.053(5) -0.019(4) C101 0.078(5) 0.067(5) 0.078(5) 0.002(4) 0.036(4) 0.002(4) C102 0.086(6) 0.087(6) 0.120(9) 0.019(6) 0.041(6) -0.009(4) Cl1 0.0621(10) 0.0685(11) 0.0786(13) -0.0001(9) 0.0390(9) 0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N13 2.024(7) . ? Ni1 N4 2.034(8) . ? Ni1 N1 2.153(7) . ? Ni1 N1 2.153(7) 6_657 ? Ni1 N16 2.164(7) . ? Ni1 N16 2.164(7) 6_657 ? N1 C2 1.466(10) . ? N1 C18 1.537(13) . ? C2 C3 1.520(10) . ? C3 N4 1.324(8) . ? C3 C21 1.388(10) . ? N4 C3 1.324(8) 6_657 ? N13 C14 1.348(7) . ? N13 C14 1.348(7) 6_657 ? C14 C31 1.386(10) . ? C14 C15 1.506(9) . ? C15 N16 1.472(10) . ? N16 C17 1.507(13) . ? C17 C18 1.428(15) . ? C21 C22 1.387(11) . ? C22 C21 1.387(11) 6_657 ? C31 C32 1.376(9) . ? C32 C31 1.376(9) 6_657 ? N100 C101 1.124(11) . ? C101 C102 1.435(13) . ? Cl1 O12 1.381(14) . ? Cl1 O41 1.396(11) . ? Cl1 O42 1.396(15) . ? Cl1 O31 1.410(11) . ? Cl1 O22 1.415(15) . ? Cl1 O21 1.420(11) . ? Cl1 O11 1.460(11) . ? Cl1 O32 1.489(16) . ? O21 O22 0.85(2) . ? O21 O32 1.66(2) . ? O31 O32 1.17(2) . ? O31 O42 1.35(2) . ? O41 O42 1.31(2) . ? 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 N13 Ni1 N4 180.000(2) . . ? N13 Ni1 N1 102.64(18) . . ? N4 Ni1 N1 77.36(18) . . ? N13 Ni1 N1 102.64(18) . 6_657 ? N4 Ni1 N1 77.36(18) . 6_657 ? N1 Ni1 N1 154.7(4) . 6_657 ? N13 Ni1 N16 77.81(17) . . ? N4 Ni1 N16 102.19(17) . . ? N1 Ni1 N16 82.5(3) . . ? N1 Ni1 N16 102.8(3) 6_657 . ? N13 Ni1 N16 77.81(17) . 6_657 ? N4 Ni1 N16 102.19(17) . 6_657 ? N1 Ni1 N16 102.8(3) . 6_657 ? N1 Ni1 N16 82.5(3) 6_657 6_657 ? N16 Ni1 N16 155.6(3) . 6_657 ? C2 N1 C18 110.2(7) . . ? C2 N1 Ni1 109.8(5) . . ? C18 N1 Ni1 105.2(4) . . ? N1 C2 C3 108.9(6) . . ? N4 C3 C21 120.4(7) . . ? N4 C3 C2 115.4(6) . . ? C21 C3 C2 124.2(7) . . ? C3 N4 C3 122.1(8) . 6_657 ? C3 N4 Ni1 118.9(4) . . ? C3 N4 Ni1 118.9(4) 6_657 . ? C14 N13 C14 121.0(8) . 6_657 ? C14 N13 Ni1 119.5(4) . . ? C14 N13 Ni1 119.5(4) 6_657 . ? N13 C14 C31 120.3(6) . . ? N13 C14 C15 114.1(6) . . ? C31 C14 C15 125.6(6) . . ? N16 C15 C14 110.6(5) . . ? C15 N16 C17 106.8(7) . . ? C15 N16 Ni1 108.8(4) . . ? C17 N16 Ni1 106.8(5) . . ? C18 C17 N16 109.5(9) . . ? C17 C18 N1 112.2(8) . . ? C22 C21 C3 119.0(8) . . ? C21 C22 C21 119.0(10) 6_657 . ? C32 C31 C14 119.2(7) . . ? C31 C32 C31 120.1(9) 6_657 . ? N100 C101 C102 179.2(11) . . ? O12 Cl1 O41 89.2(12) . . ? O12 Cl1 O42 115.2(12) . . ? O41 Cl1 O42 56.1(11) . . ? O12 Cl1 O31 111.9(14) . . ? O41 Cl1 O31 113.1(7) . . ? O42 Cl1 O31 57.5(10) . . ? O12 Cl1 O22 112.4(13) . . ? O41 Cl1 O22 82.5(12) . . ? O42 Cl1 O22 114.1(12) . . ? O31 Cl1 O22 133.0(11) . . ? O12 Cl1 O21 117.7(13) . . ? O41 Cl1 O21 116.4(8) . . ? O42 Cl1 O21 126.4(11) . . ? O31 Cl1 O21 107.9(8) . . ? O22 Cl1 O21 34.8(10) . . ? O12 Cl1 O11 15.6(13) . . ? O41 Cl1 O11 104.4(7) . . ? O42 Cl1 O11 126.7(12) . . ? O31 Cl1 O11 107.7(8) . . ? O22 Cl1 O11 110.6(13) . . ? O21 Cl1 O11 106.9(7) . . ? O12 Cl1 O32 107.3(12) . . ? O41 Cl1 O32 157.9(10) . . ? O42 Cl1 O32 102.6(11) . . ? O31 Cl1 O32 47.5(9) . . ? O22 Cl1 O32 103.7(11) . . ? O21 Cl1 O32 69.3(10) . . ? O11 Cl1 O32 93.4(11) . . ? O22 O21 Cl1 72.3(13) . . ? O22 O21 O32 128.9(16) . . ? Cl1 O21 O32 57.3(7) . . ? O32 O31 O42 126.6(15) . . ? O32 O31 Cl1 69.8(9) . . ? O42 O31 Cl1 60.7(8) . . ? O42 O41 Cl1 61.9(8) . . ? O21 O22 Cl1 72.9(13) . . ? O31 O32 Cl1 62.7(9) . . ? O31 O32 O21 106.9(12) . . ? Cl1 O32 O21 53.4(7) . . ? O41 O42 O31 123.1(12) . . ? O41 O42 Cl1 61.9(8) . . ? O31 O42 Cl1 61.8(8) . . ? _diffrn_measured_fraction_theta_max 0.449 _diffrn_reflns_theta_full 26.17 _diffrn_measured_fraction_theta_full 0.449 _refine_diff_density_max 1.291 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.108 #==END data_compound [Cu([18]py2N4](ClO4)2.CH3CN 2 _database_code_CSD 185053 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H32 Cl2 Cu N8 O8' _chemical_formula_weight 671.00 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' '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 C2/c 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 19.990(26) _cell_length_b 15.012(16) _cell_length_c 11.921(14) _cell_angle_alpha 90.00 _cell_angle_beta 123.57(1) _cell_angle_gamma 90.00 _cell_volume 2981(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _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 3161 _diffrn_reflns_av_R_equivalents 0.1740 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.92 _reflns_number_total 1899 _reflns_number_gt 1263 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1899 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1600 _refine_ls_R_factor_gt 0.1134 _refine_ls_wR_factor_ref 0.3096 _refine_ls_wR_factor_gt 0.2791 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.5000 0.77496(8) 0.7500 0.0434(7) Uani 1 d S . . N1 N 0.5643(5) 0.7399(6) 0.9711(10) 0.066(3) Uani 1 d . . . H1 H 0.6013 0.7821 1.0235 0.080 Uiso 1 calc R . . C2 C 0.6014(6) 0.6554(6) 0.9884(10) 0.060(3) Uani 1 d . . . H2A H 0.6105 0.6267 1.0686 0.072 Uiso 1 calc R . . H2B H 0.6530 0.6635 0.9999 0.072 Uiso 1 calc R . . C3 C 0.5481(6) 0.5967(6) 0.8663(11) 0.051(2) Uani 1 d . . . N4 N 0.5000 0.6420(6) 0.7500 0.041(2) Uani 1 d S . . N13 N 0.5000 0.9062(6) 0.7500 0.040(2) Uani 1 d S . . C14 C 0.4377(4) 0.9505(5) 0.7366(10) 0.045(2) Uani 1 d . . . C15 C 0.3709(5) 0.8922(5) 0.7166(12) 0.056(3) Uani 1 d . . . H15A H 0.3444 0.9204 0.7551 0.067 Uiso 1 calc R . . H15B H 0.3316 0.8832 0.6212 0.067 Uiso 1 calc R . . N16 N 0.4051(5) 0.8054(5) 0.7834(10) 0.053(2) Uani 1 d . . . H16 H 0.3667 0.7623 0.7470 0.064 Uiso 1 calc R . . C17 C 0.5570(8) 0.8108(8) 0.5717(17) 0.082(4) Uani 1 d . . . H17A H 0.5982 0.8109 0.5522 0.098 Uiso 1 calc R . . H17B H 0.5274 0.8662 0.5384 0.098 Uiso 1 calc R . . C18 C 0.5011(8) 0.7341(8) 0.5005(14) 0.070(3) Uani 1 d . . . H18A H 0.5298 0.6781 0.5336 0.084 Uiso 1 calc R . . H18B H 0.4777 0.7376 0.4044 0.084 Uiso 1 calc R . . C21 C 0.5488(7) 0.5041(6) 0.8680(16) 0.077(4) Uani 1 d . . . H21 H 0.5820 0.4736 0.9483 0.092 Uiso 1 calc R . . C22 C 0.5000 0.4581(9) 0.7500 0.085(7) Uani 1 d S . . H22 H 0.5000 0.3962 0.7500 0.101 Uiso 1 calc SR . . C31 C 0.4369(5) 1.0427(6) 0.7378(13) 0.059(3) Uani 1 d . . . H31 H 0.3939 1.0729 0.7304 0.071 Uiso 1 calc R . . C32 C 0.5000 1.0900(8) 0.7500 0.058(4) Uani 1 d S . . H32 H 0.5000 1.1519 0.7500 0.070 Uiso 1 calc SR . . Cl Cl 0.75447(14) 0.88221(15) 1.2100(3) 0.0609(8) Uani 1 d . . . O11 O 0.7891(13) 0.9368(15) 1.308(2) 0.271(18) Uani 1 d . . . O12 O 0.8028(14) 0.8847(14) 1.167(3) 0.238(14) Uani 1 d . . . O13 O 0.6795(6) 0.9198(7) 1.1141(13) 0.112(4) Uani 1 d . . . O14 O 0.7454(11) 0.7944(8) 1.230(2) 0.196(10) Uani 1 d . . . C101 C 0.7677(9) 0.8817(8) 1.591(2) 0.091(4) Uiso 1 d . . . H10A H 0.7570 0.8749 1.6595 0.110 Uiso 1 calc R . . H10B H 0.7198 0.8689 1.5044 0.110 Uiso 1 calc R . . H10C H 0.7845 0.9417 1.5914 0.110 Uiso 1 calc R . . C102 C 0.8313(7) 0.8200(7) 1.6163(13) 0.074(4) Uani 1 d . . . N103 N 0.8787(8) 0.7728(6) 1.6391(16) 0.095(4) Uani 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 Cu 0.0431(9) 0.0440(9) 0.0442(11) 0.000 0.0249(7) 0.000 N1 0.057(5) 0.077(5) 0.048(6) -0.010(4) 0.018(4) -0.006(3) C2 0.050(5) 0.089(7) 0.024(6) -0.003(4) 0.010(4) 0.005(4) C3 0.054(5) 0.058(5) 0.048(7) 0.006(4) 0.033(5) 0.006(3) N4 0.034(5) 0.054(5) 0.034(6) 0.000 0.018(4) 0.000 N13 0.041(5) 0.055(5) 0.025(6) 0.000 0.019(4) 0.000 C14 0.040(4) 0.055(4) 0.040(6) 0.003(3) 0.021(4) -0.001(3) C15 0.046(5) 0.066(5) 0.065(8) 0.002(4) 0.036(5) 0.002(3) N16 0.052(4) 0.077(5) 0.048(6) 0.006(3) 0.038(4) -0.007(3) C17 0.112(9) 0.079(7) 0.090(11) 0.005(6) 0.078(9) -0.006(6) C18 0.088(8) 0.095(8) 0.040(7) 0.000(5) 0.042(6) 0.000(5) C21 0.065(6) 0.049(5) 0.095(10) 0.013(5) 0.031(6) 0.008(4) C22 0.050(8) 0.056(7) 0.116(17) 0.000 0.026(9) 0.000 C31 0.067(6) 0.055(5) 0.066(8) 0.001(4) 0.044(5) 0.015(4) C32 0.074(9) 0.052(7) 0.048(9) 0.000 0.034(7) 0.000 Cl 0.0588(15) 0.0679(15) 0.0620(19) 0.0004(10) 0.0372(14) -0.0007(9) O11 0.23(2) 0.23(2) 0.15(2) -0.065(15) -0.023(17) -0.086(16) O12 0.26(2) 0.25(2) 0.37(4) 0.16(2) 0.28(3) 0.139(17) O13 0.092(7) 0.150(9) 0.085(9) -0.005(6) 0.042(6) 0.042(5) O14 0.185(14) 0.087(7) 0.27(3) 0.038(9) 0.101(15) -0.020(7) C102 0.071(7) 0.067(6) 0.067(9) -0.006(5) 0.028(6) -0.009(5) N103 0.107(8) 0.076(6) 0.117(12) 0.013(6) 0.070(9) 0.022(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 Cu N13 1.970(9) . ? Cu N4 1.996(9) . ? Cu N16 2.190(9) 6_657 ? Cu N16 2.190(9) . ? Cu N1 2.265(11) 6_657 ? Cu N1 2.265(11) . ? N1 C2 1.425(13) . ? N1 C18 1.524(17) 6_657 ? C2 C3 1.521(14) . ? C3 N4 1.355(11) . ? C3 C21 1.390(12) . ? N4 C3 1.355(11) 6_657 ? N13 C14 1.341(9) 6_657 ? N13 C14 1.341(9) . ? C14 C31 1.385(12) . ? C14 C15 1.501(12) . ? C15 N16 1.482(12) . ? N16 C17 1.456(19) 6_657 ? C17 N16 1.456(19) 6_657 ? C17 C18 1.500(18) . ? C18 N1 1.524(17) 6_657 ? C21 C22 1.375(15) . ? C22 C21 1.375(15) 6_657 ? C31 C32 1.384(11) . ? C32 C31 1.384(11) 6_657 ? Cl O11 1.272(17) . ? Cl O12 1.318(18) . ? Cl O14 1.369(11) . ? Cl O13 1.407(10) . ? C101 C102 1.462(17) . ? C102 N103 1.092(15) . ? 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 N13 Cu N4 180.000(3) . . ? N13 Cu N16 77.96(19) . 6_657 ? N4 Cu N16 102.04(19) . 6_657 ? N13 Cu N16 77.96(19) . . ? N4 Cu N16 102.04(19) . . ? N16 Cu N16 155.9(4) 6_657 . ? N13 Cu N1 103.5(2) . 6_657 ? N4 Cu N1 76.5(2) . 6_657 ? N16 Cu N1 80.1(4) 6_657 6_657 ? N16 Cu N1 105.6(4) . 6_657 ? N13 Cu N1 103.5(2) . . ? N4 Cu N1 76.5(2) . . ? N16 Cu N1 105.6(4) 6_657 . ? N16 Cu N1 80.1(4) . . ? N1 Cu N1 153.1(4) 6_657 . ? C2 N1 C18 111.0(9) . 6_657 ? C2 N1 Cu 106.9(7) . . ? C18 N1 Cu 105.5(6) 6_657 . ? N1 C2 C3 110.1(7) . . ? N4 C3 C21 120.8(9) . . ? N4 C3 C2 114.4(8) . . ? C21 C3 C2 124.7(9) . . ? C3 N4 C3 119.7(10) 6_657 . ? C3 N4 Cu 120.1(5) 6_657 . ? C3 N4 Cu 120.1(5) . . ? C14 N13 C14 120.5(9) 6_657 . ? C14 N13 Cu 119.7(5) 6_657 . ? C14 N13 Cu 119.7(5) . . ? N13 C14 C31 120.7(7) . . ? N13 C14 C15 114.5(7) . . ? C31 C14 C15 124.7(7) . . ? N16 C15 C14 108.8(7) . . ? C17 N16 C15 111.8(9) 6_657 . ? C17 N16 Cu 107.1(7) 6_657 . ? C15 N16 Cu 105.9(6) . . ? N16 C17 C18 111.3(10) 6_657 . ? C17 C18 N1 107.1(10) . 6_657 ? C22 C21 C3 119.5(11) . . ? C21 C22 C21 119.7(13) . 6_657 ? C32 C31 C14 119.8(8) . . ? C31 C32 C31 118.3(11) . 6_657 ? O11 Cl O12 101.1(17) . . ? O11 Cl O14 121.2(17) . . ? O12 Cl O14 106.9(13) . . ? O11 Cl O13 106.4(13) . . ? O12 Cl O13 110.7(13) . . ? O14 Cl O13 110.1(9) . . ? N103 C102 C101 177.5(17) . . ? _diffrn_measured_fraction_theta_max 0.326 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.326 _refine_diff_density_max 0.525 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.119 #==END data_compound [Co([20]py2N4]0.5[Co(H2O)6](SO4)2.CH3OH 3 _database_code_CSD 185054 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H48 Co1.50 N6 O16 S2' _chemical_formula_weight 793.17 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.089(27) _cell_length_b 16.349(20) _cell_length_c 9.766(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3207(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _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 7735 _diffrn_reflns_av_R_equivalents 0.1158 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3001 _reflns_number_gt 1817 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 3001 _refine_ls_number_parameters 466 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.1870 _refine_ls_wR_factor_gt 0.1646 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.089 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.72147(7) 0.46152(9) 0.9559(5) 0.0430(4) Uani 1 d . . . N1 N 0.6627(5) 0.4320(7) 0.8021(12) 0.051(3) Uani 1 d . . . H1 H 0.6918 0.4180 0.7346 0.061 Uiso 1 calc R . . C2 C 0.6261(7) 0.5027(8) 0.7425(17) 0.060(4) Uani 1 d . . . H2A H 0.6372 0.5086 0.6464 0.072 Uiso 1 calc R . . H2B H 0.5785 0.4937 0.7499 0.072 Uiso 1 calc R . . C3 C 0.6449(6) 0.5777(9) 0.8179(13) 0.051(3) Uani 1 d . . . N4 N 0.6879(5) 0.5655(6) 0.9247(11) 0.053(3) Uani 1 d . . . C5 C 0.7116(5) 0.6269(8) 1.0019(15) 0.057(4) Uani 1 d . . . C6 C 0.7563(7) 0.6044(11) 1.1135(16) 0.070(4) Uani 1 d . . . H6A H 0.7353 0.6171 1.2005 0.084 Uiso 1 calc R . . H6B H 0.7970 0.6360 1.1068 0.084 Uiso 1 calc R . . N7 N 0.7729(5) 0.5130(8) 1.1081(12) 0.059(3) Uani 1 d . . . H7 H 0.7572 0.4907 1.1872 0.071 Uiso 1 calc R . . C8 C 0.8459(6) 0.4992(10) 1.1076(15) 0.059(4) Uani 1 d . . . H8A H 0.8539 0.4407 1.1082 0.071 Uiso 1 calc R . . H8B H 0.8641 0.5212 1.1918 0.071 Uiso 1 calc R . . C9 C 0.8838(6) 0.5359(9) 0.9887(13) 0.060(4) Uani 1 d . . . H9A H 0.9227 0.5025 0.9706 0.072 Uiso 1 calc R . . H9B H 0.8992 0.5900 1.0147 0.072 Uiso 1 calc R . . C10 C 0.8423(7) 0.5431(9) 0.8552(14) 0.055(4) Uani 1 d . . . H10A H 0.8158 0.5926 0.8597 0.065 Uiso 1 calc R . . H10B H 0.8726 0.5486 0.7783 0.065 Uiso 1 calc R . . N11 N 0.7974(5) 0.4727(8) 0.8292(11) 0.055(3) Uani 1 d . . . H11 H 0.7785 0.4837 0.7465 0.066 Uiso 1 calc R . . C12 C 0.8327(6) 0.3942(8) 0.8087(14) 0.053(3) Uani 1 d . . . H12A H 0.8796 0.4012 0.8290 0.064 Uiso 1 calc R . . H12B H 0.8286 0.3772 0.7139 0.064 Uiso 1 calc R . . C13 C 0.8041(6) 0.3301(9) 0.8998(12) 0.052(3) Uani 1 d . . . N14 N 0.7541(4) 0.3554(6) 0.9808(11) 0.043(2) Uani 1 d . . . C15 C 0.7212(6) 0.3054(9) 1.0661(13) 0.048(3) Uani 1 d . . . C16 C 0.6694(8) 0.3473(10) 1.1522(14) 0.069(4) Uani 1 d . . . H16A H 0.6299 0.3132 1.1578 0.083 Uiso 1 calc R . . H16B H 0.6863 0.3552 1.2442 0.083 Uiso 1 calc R . . N17 N 0.6520(5) 0.4269(7) 1.0919(13) 0.055(3) Uani 1 d . . . H17 H 0.6538 0.4638 1.1615 0.067 Uiso 1 calc R . . C18 C 0.5805(6) 0.4294(10) 1.0376(16) 0.066(4) Uani 1 d . . . H18A H 0.5716 0.4829 0.9988 0.079 Uiso 1 calc R . . H18B H 0.5497 0.4209 1.1128 0.079 Uiso 1 calc R . . C19 C 0.5688(7) 0.3633(11) 0.9274(17) 0.081(5) Uani 1 d . . . H19A H 0.5659 0.3107 0.9729 0.097 Uiso 1 calc R . . H19B H 0.5260 0.3737 0.8848 0.097 Uiso 1 calc R . . C20 C 0.6201(6) 0.3569(9) 0.8165(13) 0.057(3) Uani 1 d . . . H20A H 0.5977 0.3468 0.7301 0.069 Uiso 1 calc R . . H20B H 0.6485 0.3103 0.8354 0.069 Uiso 1 calc R . . C21 C 0.6255(8) 0.6556(11) 0.7867(17) 0.075(4) Uani 1 d . . . H21 H 0.5968 0.6641 0.7134 0.090 Uiso 1 calc R . . C22 C 0.6474(8) 0.7217(11) 0.862(2) 0.094(6) Uani 1 d . . . H22 H 0.6335 0.7743 0.8395 0.112 Uiso 1 calc R . . C23 C 0.6903(7) 0.7091(8) 0.969(2) 0.072(4) Uani 1 d . . . H23 H 0.7054 0.7531 1.0212 0.086 Uiso 1 calc R . . C31 C 0.8206(7) 0.2490(9) 0.8989(16) 0.067(4) Uani 1 d . . . H31 H 0.8548 0.2303 0.8429 0.081 Uiso 1 calc R . . C32 C 0.7858(7) 0.1940(8) 0.9826(17) 0.071(4) Uani 1 d . . . H32 H 0.7952 0.1383 0.9807 0.085 Uiso 1 calc R . . C33 C 0.7373(8) 0.2250(11) 1.0680(15) 0.070(4) Uani 1 d . . . H33 H 0.7152 0.1900 1.1278 0.084 Uiso 1 calc R . . Co2 Co 1.0000 0.5000 0.4776(5) 0.0476(6) Uani 1 d SD . . O21 O 0.9165(4) 0.5777(5) 0.4811(9) 0.056(2) Uani 1 d D . . H21A H 0.909(2) 0.616(4) 0.557(6) 0.067 Uiso 1 d D . . H21B H 0.8719(9) 0.559(4) 0.456(9) 0.067 Uiso 1 d D . . O22 O 1.0000 0.5000 0.2694(13) 0.062(4) Uani 1 d SD . . H22A H 1.002(8) 0.547(2) 0.206(4) 0.075 Uiso 1 d D . . O23 O 0.9397(4) 0.3939(5) 0.4759(10) 0.060(2) Uani 1 d D . . H23A H 0.941(2) 0.357(4) 0.555(5) 0.072 Uiso 1 d D . . H23B H 0.8926(10) 0.397(3) 0.451(8) 0.072 Uiso 1 d D . . O24 O 1.0000 0.5000 0.6911(14) 0.072(4) Uani 1 d SD . . H24A H 1.006(8) 0.451(2) 0.747(4) 0.087 Uiso 1 d D . . S1 S 0.74206(13) -0.04683(18) 0.9657(6) 0.0470(7) Uani 1 d . . . O11 O 0.7737(4) -0.1098(6) 1.0538(9) 0.058(2) Uani 1 d . . . O12 O 0.7157(5) 0.0175(6) 1.0547(10) 0.061(3) Uani 1 d . . . O13 O 0.6883(5) -0.0862(7) 0.8833(11) 0.072(3) Uani 1 d . . . O14 O 0.7917(5) -0.0120(6) 0.8718(11) 0.067(3) Uani 1 d . . . S3 S 0.98943(18) 0.7132(2) 0.7541(5) 0.0535(9) Uani 1 d . . . O31 O 1.0050(5) 0.6413(6) 0.8409(11) 0.065(3) Uani 1 d . . . O32 O 0.9738(5) 0.7836(6) 0.8412(11) 0.070(3) Uani 1 d . . . O33 O 0.9320(5) 0.6951(6) 0.6702(11) 0.071(3) Uani 1 d . . . O34 O 1.0476(5) 0.7312(6) 0.6675(10) 0.070(3) Uani 1 d . . . C100 C 1.0116(8) 0.2991(10) 1.1911(18) 0.068(5) Uani 1 d . . . H10C H 1.0127 0.3129 1.2866 0.082 Uiso 1 calc R . . H10D H 1.0563 0.2958 1.1567 0.082 Uiso 1 calc R . . H10E H 0.9899 0.2472 1.1794 0.082 Uiso 1 calc R . . O101 O 0.9767(6) 0.3590(7) 1.1194(12) 0.078(3) Uani 1 d . . . H101 H 0.9577 0.3892 1.1737 0.094 Uiso 1 calc R . . O200 O 0.8486(5) 0.7494(6) 0.9809(15) 0.102(4) Uani 1 d D . . H201 H 0.8941(19) 0.765(6) 0.955(13) 0.123 Uiso 1 d D . . H202 H 0.829(6) 0.800(5) 1.017(17) 0.123 Uiso 1 d D . . O300 O 0.5878(6) 0.6019(8) 1.1810(12) 0.105(4) Uani 1 d D . . H301 H 0.576(4) 0.585(9) 1.274(5) 0.127 Uiso 1 d D . . H302 H 0.615(8) 0.651(7) 1.193(13) 0.127 Uiso 1 d D . . O400 O 1.0138(11) 0.8958(13) 1.037(2) 0.184(8) Uani 1 d D . . H401 H 1.0534(18) 0.892(14) 0.979(7) 0.220 Uiso 1 d D . . H402 H 0.991(10) 0.945(11) 1.01(3) 0.220 Uiso 1 d D . . O500 O 0.9247(10) 0.9782(16) 0.899(2) 0.225(13) Uani 1 d D . . H501 H 0.899(16) 0.936(16) 0.95(4) 0.270 Uiso 1 d D . . H502 H 0.947(17) 0.931(14) 0.86(4) 0.270 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0371(8) 0.0453(9) 0.0465(8) -0.0032(9) 0.0059(8) -0.0040(6) N1 0.037(6) 0.054(7) 0.062(6) -0.002(6) -0.005(5) -0.003(5) C2 0.054(8) 0.043(8) 0.083(10) 0.006(8) -0.009(7) 0.007(7) C3 0.048(7) 0.055(10) 0.050(7) 0.009(6) 0.001(6) 0.016(6) N4 0.052(6) 0.042(7) 0.065(8) -0.013(5) 0.015(5) -0.009(5) C5 0.023(6) 0.055(9) 0.094(11) -0.009(8) 0.006(6) -0.008(5) C6 0.062(9) 0.085(13) 0.062(9) -0.007(8) 0.007(7) -0.010(8) N7 0.049(7) 0.085(11) 0.044(6) -0.008(6) 0.000(5) -0.015(6) C8 0.040(8) 0.083(11) 0.053(7) -0.016(7) -0.004(6) 0.002(7) C9 0.042(6) 0.081(9) 0.057(9) -0.030(7) 0.003(6) -0.015(6) C10 0.052(8) 0.054(10) 0.059(8) 0.006(6) 0.019(6) 0.001(7) N11 0.037(6) 0.091(11) 0.037(5) -0.001(5) 0.007(4) -0.005(6) C12 0.041(7) 0.055(9) 0.063(7) -0.001(7) 0.007(6) 0.010(6) C13 0.050(7) 0.061(10) 0.045(6) -0.001(6) 0.004(6) -0.008(7) N14 0.047(5) 0.036(5) 0.046(6) 0.001(5) -0.001(5) -0.006(4) C15 0.053(8) 0.046(9) 0.044(7) 0.001(6) -0.008(5) -0.009(6) C16 0.081(11) 0.071(12) 0.054(8) 0.010(8) 0.006(7) -0.027(8) N17 0.059(7) 0.044(8) 0.064(6) -0.022(6) 0.024(6) -0.027(6) C18 0.045(8) 0.076(12) 0.078(9) 0.009(8) 0.011(7) 0.003(7) C19 0.063(9) 0.077(11) 0.102(14) -0.002(9) -0.011(8) -0.008(8) C20 0.054(8) 0.071(10) 0.047(7) -0.003(7) -0.004(6) 0.002(7) C21 0.077(11) 0.074(13) 0.075(9) 0.014(9) 0.009(8) 0.013(9) C22 0.063(11) 0.065(13) 0.153(18) -0.021(12) -0.001(11) 0.007(9) C23 0.061(8) 0.043(9) 0.111(11) -0.019(10) 0.016(11) -0.001(6) C31 0.071(10) 0.040(10) 0.091(10) 0.003(8) -0.006(8) 0.000(7) C32 0.088(10) 0.036(8) 0.088(11) -0.002(9) -0.006(10) 0.005(7) C33 0.082(11) 0.068(12) 0.061(9) 0.013(8) -0.009(7) -0.019(9) Co2 0.0418(12) 0.0524(15) 0.0487(14) 0.000 0.000 -0.0016(10) O21 0.044(4) 0.072(6) 0.051(5) -0.004(5) 0.006(4) 0.007(4) O22 0.078(10) 0.059(10) 0.050(7) 0.000 0.000 -0.006(8) O23 0.053(5) 0.056(6) 0.072(5) 0.005(6) -0.006(5) -0.018(4) O24 0.093(12) 0.063(11) 0.061(8) 0.000 0.000 0.012(10) S1 0.0454(15) 0.0549(19) 0.0406(14) -0.0007(18) 0.0046(17) -0.0002(13) O11 0.058(5) 0.066(7) 0.052(5) -0.002(4) -0.010(4) 0.008(5) O12 0.081(7) 0.056(6) 0.045(5) 0.002(4) 0.018(4) 0.019(5) O13 0.059(6) 0.082(8) 0.073(6) -0.007(6) -0.012(5) -0.005(5) O14 0.061(6) 0.084(8) 0.055(5) -0.006(5) 0.015(5) -0.012(5) S3 0.061(2) 0.049(2) 0.0506(19) -0.0017(16) 0.0019(16) 0.0029(18) O31 0.078(7) 0.046(7) 0.071(6) 0.012(5) 0.001(5) 0.005(5) O32 0.069(6) 0.066(7) 0.077(7) -0.011(5) 0.001(5) -0.005(5) O33 0.067(6) 0.062(6) 0.083(6) -0.008(5) -0.015(5) 0.005(5) O34 0.074(7) 0.074(7) 0.061(6) -0.008(5) 0.011(5) -0.012(5) C100 0.060(10) 0.063(12) 0.081(10) -0.005(9) 0.010(8) -0.009(8) O101 0.090(8) 0.070(9) 0.076(7) -0.009(6) 0.005(6) 0.027(6) O200 0.071(7) 0.084(8) 0.152(11) 0.035(9) 0.047(8) 0.017(5) O300 0.093(9) 0.089(9) 0.134(10) -0.034(8) 0.046(8) -0.010(7) O400 0.22(2) 0.19(2) 0.141(16) -0.008(13) -0.049(14) -0.018(16) O500 0.108(14) 0.43(4) 0.137(17) -0.07(2) 0.039(12) -0.058(19) _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 N4 1.854(11) . ? Co1 N14 1.871(10) . ? Co1 N1 1.970(11) . ? Co1 N11 1.973(10) . ? Co1 N7 1.996(11) . ? Co1 N17 2.008(10) . ? N1 C2 1.489(17) . ? N1 C20 1.504(17) . ? C2 C3 1.48(2) . ? C3 C21 1.37(2) . ? C3 N4 1.369(15) . ? N4 C5 1.343(15) . ? C5 C23 1.446(19) . ? C5 C6 1.46(2) . ? C6 N7 1.53(2) . ? N7 C8 1.485(16) . ? C8 C9 1.512(19) . ? C9 C10 1.552(18) . ? C10 N11 1.485(18) . ? N11 C12 1.480(16) . ? C12 C13 1.490(18) . ? C13 N14 1.344(14) . ? C13 C31 1.37(2) . ? N14 C15 1.341(15) . ? C15 C33 1.354(19) . ? C15 C16 1.504(19) . ? C16 N17 1.471(18) . ? N17 C18 1.532(18) . ? C18 C19 1.54(2) . ? C19 C20 1.498(19) . ? C21 C22 1.38(2) . ? C22 C23 1.38(2) . ? C31 C32 1.40(2) . ? C32 C33 1.38(2) . ? Co2 O22 2.033(13) . ? Co2 O24 2.085(15) . ? Co2 O21 2.104(8) . ? Co2 O21 2.104(8) 2_765 ? Co2 O23 2.115(8) 2_765 ? Co2 O23 2.115(8) . ? S1 O12 1.464(9) . ? S1 O14 1.470(10) . ? S1 O11 1.485(9) . ? S1 O13 1.492(10) . ? S3 O33 1.446(10) . ? S3 O32 1.465(10) . ? S3 O34 1.472(10) . ? S3 O31 1.483(10) . ? C100 O101 1.394(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N14 177.8(4) . . ? N4 Co1 N1 83.2(5) . . ? N14 Co1 N1 94.7(5) . . ? N4 Co1 N11 95.4(5) . . ? N14 Co1 N11 84.0(5) . . ? N1 Co1 N11 90.4(5) . . ? N4 Co1 N7 85.7(5) . . ? N14 Co1 N7 96.5(5) . . ? N1 Co1 N7 168.8(5) . . ? N11 Co1 N7 91.6(4) . . ? N4 Co1 N17 96.5(5) . . ? N14 Co1 N17 84.0(5) . . ? N1 Co1 N17 91.1(5) . . ? N11 Co1 N17 168.1(5) . . ? N7 Co1 N17 89.2(5) . . ? C2 N1 C20 112.8(10) . . ? C2 N1 Co1 113.8(9) . . ? C20 N1 Co1 118.0(8) . . ? C3 C2 N1 108.8(11) . . ? C21 C3 N4 119.1(14) . . ? C21 C3 C2 126.1(13) . . ? N4 C3 C2 114.8(11) . . ? C5 N4 C3 122.9(11) . . ? C5 N4 Co1 117.6(9) . . ? C3 N4 Co1 119.2(9) . . ? N4 C5 C23 117.8(13) . . ? N4 C5 C6 116.7(13) . . ? C23 C5 C6 125.5(14) . . ? C5 C6 N7 110.7(12) . . ? C8 N7 C6 111.3(11) . . ? C8 N7 Co1 116.4(9) . . ? C6 N7 Co1 108.9(8) . . ? N7 C8 C9 116.1(12) . . ? C8 C9 C10 113.9(10) . . ? N11 C10 C9 114.3(11) . . ? C12 N11 C10 113.8(10) . . ? C12 N11 Co1 112.1(8) . . ? C10 N11 Co1 115.7(8) . . ? N11 C12 C13 110.2(10) . . ? N14 C13 C31 118.9(12) . . ? N14 C13 C12 115.0(12) . . ? C31 C13 C12 125.9(12) . . ? C15 N14 C13 123.1(11) . . ? C15 N14 Co1 118.2(9) . . ? C13 N14 Co1 118.1(8) . . ? N14 C15 C33 118.9(12) . . ? N14 C15 C16 114.3(12) . . ? C33 C15 C16 126.9(12) . . ? N17 C16 C15 110.1(10) . . ? C16 N17 C18 112.6(11) . . ? C16 N17 Co1 110.4(8) . . ? C18 N17 Co1 114.5(9) . . ? N17 C18 C19 111.4(11) . . ? C20 C19 C18 116.7(12) . . ? C19 C20 N1 113.7(12) . . ? C3 C21 C22 121.4(16) . . ? C23 C22 C21 119.3(17) . . ? C22 C23 C5 119.5(14) . . ? C13 C31 C32 119.9(14) . . ? C33 C32 C31 118.1(14) . . ? C15 C33 C32 121.1(14) . . ? O22 Co2 O24 180.000(4) . . ? O22 Co2 O21 90.9(3) . . ? O24 Co2 O21 89.1(3) . . ? O22 Co2 O21 90.9(3) . 2_765 ? O24 Co2 O21 89.1(3) . 2_765 ? O21 Co2 O21 178.2(5) . 2_765 ? O22 Co2 O23 89.5(3) . 2_765 ? O24 Co2 O23 90.5(3) . 2_765 ? O21 Co2 O23 87.8(3) . 2_765 ? O21 Co2 O23 92.2(3) 2_765 2_765 ? O22 Co2 O23 89.5(3) . . ? O24 Co2 O23 90.5(3) . . ? O21 Co2 O23 92.2(3) . . ? O21 Co2 O23 87.8(3) 2_765 . ? O23 Co2 O23 179.1(6) 2_765 . ? O12 S1 O14 109.8(6) . . ? O12 S1 O11 108.1(5) . . ? O14 S1 O11 109.8(6) . . ? O12 S1 O13 111.6(6) . . ? O14 S1 O13 108.7(6) . . ? O11 S1 O13 108.9(6) . . ? O33 S3 O32 108.6(6) . . ? O33 S3 O34 110.4(6) . . ? O32 S3 O34 110.3(6) . . ? O33 S3 O31 109.3(6) . . ? O32 S3 O31 109.7(6) . . ? O34 S3 O31 108.6(6) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.660 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.104 #==END data_compound [Ni([20]py2N4](ClO4)2 4 _database_code_CSD 185055 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Cl2 N6 Ni O8' _chemical_formula_weight 612.11 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.140(17) _cell_length_b 13.478(18) _cell_length_c 17.277(23) _cell_angle_alpha 90.00 _cell_angle_beta 110.58(1) _cell_angle_gamma 90.00 _cell_volume 2647(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _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 8505 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.1222 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.90 _reflns_number_total 4578 _reflns_number_gt 2294 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1432P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4578 _refine_ls_number_parameters 333 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1826 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2463 _refine_ls_wR_factor_gt 0.2094 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.994 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.81453(8) 0.77118(6) 0.56111(5) 0.0502(4) Uani 1 d . . . N1 N 0.7360(8) 0.6265(5) 0.5248(4) 0.091(3) Uani 1 d . . . H1 H 0.7356 0.6126 0.4732 0.109 Uiso 1 calc R . . C2 C 0.6140(10) 0.6310(7) 0.5222(6) 0.104(4) Uani 1 d . . . H2A H 0.5903 0.5661 0.5347 0.125 Uiso 1 calc R . . H2B H 0.5628 0.6491 0.4669 0.125 Uiso 1 calc R . . C3 C 0.6000(8) 0.7074(8) 0.5846(6) 0.085(3) Uani 1 d . . . N4 N 0.6870(5) 0.7761(5) 0.6085(3) 0.0589(16) Uani 1 d . . . C5 C 0.6828(8) 0.8541(6) 0.6583(4) 0.070(2) Uani 1 d . . . C6 C 0.7884(9) 0.9166(6) 0.6845(5) 0.081(3) Uani 1 d . . . H6A H 0.8401 0.8950 0.7386 0.097 Uiso 1 calc R . . H6B H 0.7656 0.9846 0.6896 0.097 Uiso 1 calc R . . N7 N 0.8542(6) 0.9138(4) 0.6264(3) 0.0647(17) Uani 1 d . . . H7 H 0.9319 0.9121 0.6583 0.078 Uiso 1 calc R . . C8 C 0.8366(9) 1.0052(6) 0.5770(6) 0.090(3) Uani 1 d . . . H8A H 0.9032 1.0139 0.5590 0.108 Uiso 1 calc R . . H8B H 0.8352 1.0612 0.6118 0.108 Uiso 1 calc R . . C9 C 0.7235(10) 1.0061(6) 0.5008(6) 0.105(4) Uani 1 d . . . H9A H 0.6594 0.9850 0.5182 0.126 Uiso 1 calc R . . H9B H 0.7078 1.0742 0.4821 0.126 Uiso 1 calc R . . C10 C 0.7203(9) 0.9461(6) 0.4309(6) 0.086(3) Uani 1 d . . . H10A H 0.7900 0.9608 0.4178 0.103 Uiso 1 calc R . . H10B H 0.6526 0.9663 0.3838 0.103 Uiso 1 calc R . . N11 N 0.7141(5) 0.8361(4) 0.4408(3) 0.0533(15) Uani 1 d . . . H11 H 0.6372 0.8190 0.4280 0.064 Uiso 1 calc R . . C12 C 0.7585(6) 0.7876(5) 0.3799(4) 0.0587(19) Uani 1 d . . . H12A H 0.7432 0.8300 0.3319 0.070 Uiso 1 calc R . . H12B H 0.7175 0.7253 0.3618 0.070 Uiso 1 calc R . . C13 C 0.8882(7) 0.7687(5) 0.4186(4) 0.0528(17) Uani 1 d . . . N14 N 0.9280(5) 0.7625(4) 0.5005(3) 0.0520(14) Uani 1 d . . . C15 C 1.0441(7) 0.7435(5) 0.5419(5) 0.066(2) Uani 1 d . . . C16 C 1.0762(8) 0.7456(7) 0.6337(6) 0.088(3) Uani 1 d . . . H16A H 1.1437 0.7030 0.6592 0.106 Uiso 1 calc R . . H16B H 1.0978 0.8127 0.6537 0.106 Uiso 1 calc R . . N17 N 0.9760(7) 0.7116(5) 0.6576(4) 0.083(2) Uani 1 d . . . H17 H 0.9828 0.7442 0.7052 0.100 Uiso 1 calc R . . C18 C 0.9865(12) 0.6060(8) 0.6781(7) 0.114(4) Uani 1 d . . . H18A H 1.0694 0.5888 0.7000 0.137 Uiso 1 calc R . . H18B H 0.9547 0.5946 0.7216 0.137 Uiso 1 calc R . . C19 C 0.9320(11) 0.5446(7) 0.6147(7) 0.115(4) Uani 1 d . . . H19A H 0.9635 0.4785 0.6304 0.138 Uiso 1 calc R . . H19B H 0.9536 0.5648 0.5681 0.138 Uiso 1 calc R . . C20 C 0.7999(11) 0.5376(7) 0.5854(12) 0.159(6) Uani 1 d . . . H20A H 0.7751 0.5381 0.6330 0.191 Uiso 1 calc R . . H20B H 0.7753 0.4750 0.5568 0.191 Uiso 1 calc R . . C21 C 0.5073(12) 0.7113(12) 0.6087(8) 0.129(5) Uani 1 d . . . H21 H 0.4492 0.6627 0.5926 0.155 Uiso 1 calc R . . C22 C 0.4998(12) 0.7883(15) 0.6575(9) 0.138(6) Uani 1 d . . . H22 H 0.4351 0.7908 0.6744 0.166 Uiso 1 calc R . . C23 C 0.5850(12) 0.8653(11) 0.6841(6) 0.116(4) Uani 1 d . . . H23 H 0.5771 0.9187 0.7159 0.139 Uiso 1 calc R . . C31 C 0.9671(9) 0.7574(6) 0.3770(6) 0.076(2) Uani 1 d . . . H31 H 0.9400 0.7653 0.3199 0.091 Uiso 1 calc R . . C32 C 1.0796(8) 0.7359(6) 0.4163(7) 0.078(2) Uani 1 d . . . H32 H 1.1295 0.7254 0.3867 0.094 Uiso 1 calc R . . C33 C 1.1219(8) 0.7291(6) 0.5009(7) 0.084(3) Uani 1 d . . . H33 H 1.2007 0.7151 0.5298 0.100 Uiso 1 calc R . . Cl1 Cl 0.88069(17) 0.71062(16) 0.85919(12) 0.0716(6) Uani 1 d . . . O11 O 0.8380(8) 0.7868(9) 0.8970(7) 0.176(5) Uani 1 d . . . O12 O 0.9664(5) 0.7530(5) 0.8299(4) 0.0868(18) Uani 1 d . . . O13 O 0.7864(6) 0.6690(5) 0.7937(4) 0.108(2) Uani 1 d . . . O14 O 0.9387(7) 0.6386(7) 0.9173(6) 0.168(5) Uani 1 d . . . Cl2 Cl 1.1762(2) 0.99603(15) 0.79429(14) 0.0853(8) Uani 0.461(14) d PD A 1 O21 O 1.2528(16) 0.9497(14) 0.7481(12) 0.165(9) Uiso 0.461(14) d PD A 1 O22 O 1.1612(13) 1.0920(9) 0.7684(11) 0.106(6) Uiso 0.461(14) d PD A 1 O23 O 1.0938(11) 0.9251(10) 0.7857(9) 0.102(5) Uiso 0.461(14) d PD A 1 O24 O 1.2678(11) 0.9882(10) 0.8773(7) 0.096(5) Uiso 0.461(14) d PD A 1 Cl2' Cl 1.1762(2) 0.99603(15) 0.79429(14) 0.0853(8) Uani 0.539(14) d PD A 2 O21' O 1.1208(14) 0.9919(11) 0.7067(8) 0.149(7) Uiso 0.539(14) d PD A 2 O22' O 1.1836(11) 1.1021(7) 0.8153(8) 0.091(4) Uiso 0.539(14) d PD A 2 O23' O 1.0920(15) 0.9611(14) 0.8308(12) 0.172(8) Uiso 0.539(14) d PD A 2 O24' O 1.2841(13) 0.9506(13) 0.8250(12) 0.168(8) Uiso 0.539(14) d PD 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 Ni1 0.0561(6) 0.0466(6) 0.0467(5) 0.0009(4) 0.0167(4) 0.0084(4) N1 0.140(8) 0.063(5) 0.069(4) -0.007(3) 0.035(5) -0.030(5) C2 0.104(8) 0.076(6) 0.094(7) -0.005(5) -0.015(6) -0.024(5) C3 0.060(5) 0.113(8) 0.074(6) 0.029(5) 0.013(5) -0.010(5) N4 0.054(4) 0.069(4) 0.053(3) 0.017(3) 0.016(3) -0.002(3) C5 0.076(6) 0.085(6) 0.047(4) 0.003(4) 0.020(4) 0.027(5) C6 0.113(8) 0.066(5) 0.066(5) -0.012(4) 0.035(5) 0.019(5) N7 0.063(4) 0.063(4) 0.059(4) -0.005(3) 0.009(3) 0.002(3) C8 0.130(9) 0.053(5) 0.092(6) 0.002(4) 0.045(6) -0.009(5) C9 0.137(9) 0.051(5) 0.113(7) 0.016(5) 0.027(7) 0.026(5) C10 0.105(7) 0.049(5) 0.100(6) 0.014(4) 0.030(6) 0.029(4) N11 0.051(3) 0.056(4) 0.050(3) 0.008(2) 0.013(3) 0.004(3) C12 0.058(4) 0.072(5) 0.044(4) -0.001(3) 0.015(3) 0.003(4) C13 0.063(5) 0.043(4) 0.057(4) 0.004(3) 0.027(4) -0.003(3) N14 0.054(4) 0.052(3) 0.047(3) -0.005(2) 0.014(3) 0.004(3) C15 0.053(5) 0.056(5) 0.073(5) -0.006(3) 0.002(4) 0.007(3) C16 0.065(6) 0.103(7) 0.081(6) -0.011(5) 0.006(5) 0.012(5) N17 0.108(6) 0.086(5) 0.046(3) 0.009(3) 0.017(4) 0.048(4) C18 0.150(11) 0.094(8) 0.104(8) 0.020(6) 0.052(8) 0.046(7) C19 0.138(11) 0.064(6) 0.120(8) 0.012(6) 0.018(8) 0.030(6) C20 0.097(9) 0.037(5) 0.36(2) 0.013(8) 0.095(11) -0.006(5) C21 0.096(10) 0.210(16) 0.092(8) 0.041(9) 0.047(8) -0.001(9) C22 0.080(8) 0.26(2) 0.095(9) 0.074(11) 0.057(7) 0.033(11) C23 0.116(10) 0.170(12) 0.077(7) 0.010(7) 0.053(7) 0.045(9) C31 0.089(7) 0.071(6) 0.086(6) 0.002(4) 0.054(5) 0.007(4) C32 0.072(6) 0.066(5) 0.119(8) -0.006(5) 0.062(6) 0.001(4) C33 0.050(5) 0.066(5) 0.137(9) -0.019(5) 0.035(5) 0.004(4) Cl1 0.0538(12) 0.0941(16) 0.0653(12) 0.0120(10) 0.0189(10) -0.0105(10) O11 0.110(7) 0.230(11) 0.211(10) -0.109(8) 0.086(7) -0.022(7) O12 0.068(4) 0.119(5) 0.083(4) 0.007(3) 0.038(3) -0.020(3) O13 0.083(4) 0.124(6) 0.092(4) 0.000(4) 0.001(4) -0.044(4) O14 0.101(6) 0.198(9) 0.166(7) 0.118(7) -0.003(5) -0.029(6) Cl2 0.0845(16) 0.0683(13) 0.0862(15) 0.0196(10) 0.0089(12) -0.0266(11) Cl2 0.0845(16) 0.0683(13) 0.0862(15) 0.0196(10) 0.0089(12) -0.0266(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 1.991(7) . ? Ni1 N14 2.006(6) . ? Ni1 N1 2.164(7) . ? Ni1 N11 2.189(5) . ? Ni1 N7 2.195(6) . ? Ni1 N17 2.229(6) . ? N1 C2 1.466(14) . ? N1 C20 1.601(15) . ? C2 C3 1.543(15) . ? C3 C21 1.331(16) . ? C3 N4 1.356(11) . ? N4 C5 1.371(10) . ? C5 C23 1.415(14) . ? C5 C6 1.467(13) . ? C6 N7 1.486(11) . ? N7 C8 1.471(10) . ? C8 C9 1.531(13) . ? C9 C10 1.442(13) . ? C10 N11 1.498(9) . ? N11 C12 1.491(9) . ? C12 C13 1.501(10) . ? C13 N14 1.327(9) . ? C13 C31 1.394(11) . ? N14 C15 1.362(10) . ? C15 C33 1.378(13) . ? C15 C16 1.494(12) . ? C16 N17 1.488(12) . ? N17 C18 1.461(12) . ? C18 C19 1.345(14) . ? C19 C20 1.506(15) . ? C21 C22 1.36(2) . ? C22 C23 1.42(2) . ? C31 C32 1.326(12) . ? C32 C33 1.373(14) . ? Cl1 O14 1.396(7) . ? Cl1 O11 1.409(9) . ? Cl1 O13 1.413(6) . ? Cl1 O12 1.427(6) . ? Cl2 O23 1.354(11) . ? Cl2 O22 1.360(11) . ? Cl2 O24 1.477(11) . ? Cl2 O21 1.553(14) . ? Cl2 O24 1.372(13) . ? Cl2 O21 1.425(12) . ? Cl2 O23 1.455(13) . ? Cl2 O22 1.470(10) . ? 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 N4 Ni1 N14 173.2(2) . . ? N4 Ni1 N1 79.7(3) . . ? N14 Ni1 N1 96.3(3) . . ? N4 Ni1 N11 97.1(2) . . ? N14 Ni1 N11 77.5(2) . . ? N1 Ni1 N11 92.5(2) . . ? N4 Ni1 N7 79.7(3) . . ? N14 Ni1 N7 104.7(2) . . ? N1 Ni1 N7 158.8(3) . . ? N11 Ni1 N7 94.9(2) . . ? N4 Ni1 N17 108.1(3) . . ? N14 Ni1 N17 77.5(3) . . ? N1 Ni1 N17 94.2(3) . . ? N11 Ni1 N17 154.7(3) . . ? N7 Ni1 N17 87.4(2) . . ? C2 N1 C20 107.7(8) . . ? C2 N1 Ni1 108.0(6) . . ? C20 N1 Ni1 115.0(6) . . ? N1 C2 C3 111.4(7) . . ? C21 C3 N4 122.1(11) . . ? C21 C3 C2 124.0(11) . . ? N4 C3 C2 113.7(9) . . ? C3 N4 C5 121.2(8) . . ? C3 N4 Ni1 119.2(7) . . ? C5 N4 Ni1 119.4(6) . . ? N4 C5 C23 120.1(10) . . ? N4 C5 C6 114.4(8) . . ? C23 C5 C6 125.5(9) . . ? C5 C6 N7 113.3(6) . . ? C8 N7 C6 111.6(6) . . ? C8 N7 Ni1 118.3(5) . . ? C6 N7 Ni1 107.2(5) . . ? N7 C8 C9 114.1(7) . . ? C10 C9 C8 117.8(9) . . ? C9 C10 N11 116.6(8) . . ? C12 N11 C10 108.0(6) . . ? C12 N11 Ni1 106.0(4) . . ? C10 N11 Ni1 118.1(4) . . ? N11 C12 C13 110.1(5) . . ? N14 C13 C31 119.0(7) . . ? N14 C13 C12 114.7(6) . . ? C31 C13 C12 126.3(7) . . ? C13 N14 C15 119.6(7) . . ? C13 N14 Ni1 119.6(5) . . ? C15 N14 Ni1 120.7(5) . . ? N14 C15 C33 121.7(8) . . ? N14 C15 C16 112.9(8) . . ? C33 C15 C16 125.3(8) . . ? N17 C16 C15 110.8(7) . . ? C18 N17 C16 111.0(8) . . ? C18 N17 Ni1 120.7(7) . . ? C16 N17 Ni1 105.8(5) . . ? C19 C18 N17 115.2(9) . . ? C18 C19 C20 118.3(12) . . ? C19 C20 N1 112.8(9) . . ? C3 C21 C22 118.2(14) . . ? C21 C22 C23 123.9(13) . . ? C5 C23 C22 114.5(11) . . ? C32 C31 C13 122.0(9) . . ? C31 C32 C33 119.5(9) . . ? C32 C33 C15 118.1(8) . . ? O14 Cl1 O11 110.4(8) . . ? O14 Cl1 O13 111.2(5) . . ? O11 Cl1 O13 109.5(5) . . ? O14 Cl1 O12 106.6(5) . . ? O11 Cl1 O12 107.8(6) . . ? O13 Cl1 O12 111.2(4) . . ? O23 Cl2 O22 128.8(9) . . ? O23 Cl2 O24 109.3(8) . . ? O22 Cl2 O24 110.8(8) . . ? O23 Cl2 O21 102.3(9) . . ? O22 Cl2 O21 104.4(9) . . ? O24 Cl2 O21 95.0(8) . . ? O24 Cl2 O21 115.1(10) . . ? O24 Cl2 O23 114.1(10) . . ? O21 Cl2 O23 107.8(9) . . ? O24 Cl2 O22 111.8(9) . . ? O21 Cl2 O22 105.4(7) . . ? O23 Cl2 O22 101.5(9) . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 0.520 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.092 #==END data_compound [Cu([20]py2N4](ClO4)2 5 _database_code_CSD 185056 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Cl2 Cu N6 O8' _chemical_formula_weight 616.94 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' '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 P21/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 12.121(17) _cell_length_b 13.534(18) _cell_length_c 17.046(24) _cell_angle_alpha 90.00 _cell_angle_beta 110.46(10) _cell_angle_gamma 90.00 _cell_volume 2620(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _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 8132 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.08 _reflns_number_total 4922 _reflns_number_gt 3453 _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1257P)^2^+1.5731P] 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 SHELXL _refine_ls_extinction_coef 0.0061(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4922 _refine_ls_number_parameters 334 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1962 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.133 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.81154(5) 0.27239(4) 0.56358(4) 0.0469(3) Uani 1 d . . . N1 N 0.7369(5) 0.1292(3) 0.5308(3) 0.0730(14) Uani 1 d . . . H1 H 0.7397 0.1125 0.4798 0.088 Uiso 1 calc R . . C2 C 0.6140(6) 0.1367(5) 0.5243(4) 0.087(2) Uani 1 d . . . H2A H 0.5870 0.0729 0.5362 0.104 Uiso 1 calc R . . H2B H 0.5661 0.1551 0.4676 0.104 Uiso 1 calc R . . C3 C 0.5984(5) 0.2136(5) 0.5855(4) 0.0726(17) Uani 1 d . . . N4 N 0.6859(4) 0.2812(3) 0.6100(3) 0.0549(10) Uani 1 d . . . C5 C 0.6826(6) 0.3568(5) 0.6594(3) 0.0682(16) Uani 1 d . . . C6 C 0.7902(7) 0.4230(5) 0.6846(4) 0.0773(18) Uani 1 d . . . H6A H 0.7656 0.4912 0.6849 0.093 Uiso 1 calc R . . H6B H 0.8410 0.4063 0.7410 0.093 Uiso 1 calc R . . N7 N 0.8562(4) 0.4132(3) 0.6278(3) 0.0648(12) Uani 1 d . . . H7 H 0.9334 0.4090 0.6608 0.078 Uiso 1 calc R . . C8 C 0.8450(7) 0.5021(5) 0.5767(5) 0.089(2) Uani 1 d . . . H8A H 0.9107 0.5038 0.5566 0.107 Uiso 1 calc R . . H8B H 0.8521 0.5593 0.6124 0.107 Uiso 1 calc R . . C9 C 0.7358(8) 0.5117(5) 0.5043(5) 0.101(2) Uani 1 d . . . H9A H 0.7247 0.5811 0.4892 0.121 Uiso 1 calc R . . H9B H 0.6708 0.4919 0.5216 0.121 Uiso 1 calc R . . C10 C 0.7276(6) 0.4540(4) 0.4272(4) 0.0756(17) Uani 1 d . . . H10A H 0.6627 0.4798 0.3803 0.091 Uiso 1 calc R . . H10B H 0.7993 0.4640 0.4152 0.091 Uiso 1 calc R . . N11 N 0.7098(4) 0.3462(3) 0.4342(3) 0.0564(11) Uani 1 d . . . H11 H 0.6314 0.3343 0.4208 0.068 Uiso 1 calc R . . C12 C 0.7523(5) 0.2905(4) 0.3773(3) 0.0584(13) Uani 1 d . . . H12A H 0.7376 0.3277 0.3260 0.070 Uiso 1 calc R . . H12B H 0.7102 0.2283 0.3631 0.070 Uiso 1 calc R . . C13 C 0.8825(4) 0.2707(3) 0.4173(3) 0.0481(11) Uani 1 d . . . N14 N 0.9239(4) 0.2630(3) 0.5002(3) 0.0472(9) Uani 1 d . . . C15 C 1.0402(5) 0.2432(4) 0.5397(4) 0.0556(12) Uani 1 d . . . C16 C 1.0812(5) 0.2434(5) 0.6328(4) 0.0721(16) Uani 1 d . . . H16A H 1.1498 0.2011 0.6545 0.087 Uiso 1 calc R . . H16B H 1.1047 0.3099 0.6530 0.087 Uiso 1 calc R . . N17 N 0.9912(5) 0.2095(4) 0.6647(3) 0.0743(15) Uani 1 d . . . H17 H 1.0028 0.2420 0.7136 0.089 Uiso 1 calc R . . C18 C 0.9999(7) 0.1039(5) 0.6835(5) 0.091(2) Uani 1 d . . . H18A H 1.0816 0.0838 0.6989 0.109 Uiso 1 calc R . . H18B H 0.9760 0.0924 0.7314 0.109 Uiso 1 calc R . . C19 C 0.9291(7) 0.0430(5) 0.6150(5) 0.094(2) Uani 1 d . . . H19A H 0.9546 -0.0250 0.6275 0.112 Uiso 1 calc R . . H19B H 0.9452 0.0621 0.5652 0.112 Uiso 1 calc R . . C20 C 0.7987(7) 0.0467(5) 0.5950(6) 0.100(2) Uani 1 d . . . H20A H 0.7830 0.0578 0.6464 0.120 Uiso 1 calc R . . H20B H 0.7651 -0.0168 0.5726 0.120 Uiso 1 calc R . . C21 C 0.5039(8) 0.2205(8) 0.6110(6) 0.109(3) Uani 1 d . . . H21 H 0.4445 0.1733 0.5948 0.131 Uiso 1 calc R . . C22 C 0.4982(9) 0.2973(11) 0.6606(7) 0.129(4) Uani 1 d . . . H22 H 0.4340 0.3026 0.6782 0.155 Uiso 1 calc R . . C23 C 0.5859(9) 0.3679(8) 0.6852(5) 0.107(3) Uani 1 d . . . H23 H 0.5807 0.4214 0.7181 0.129 Uiso 1 calc R . . C31 C 0.9543(6) 0.2580(4) 0.3703(4) 0.0665(15) Uani 1 d . . . H31 H 0.9237 0.2648 0.3124 0.080 Uiso 1 calc R . . C32 C 1.0705(6) 0.2355(4) 0.4098(5) 0.0717(16) Uani 1 d . . . H32 H 1.1195 0.2259 0.3790 0.086 Uiso 1 calc R . . C33 C 1.1139(5) 0.2273(4) 0.4953(5) 0.0736(18) Uani 1 d . . . H33 H 1.1926 0.2112 0.5231 0.088 Uiso 1 calc R . . Cl1 Cl 0.87473(12) 0.20957(12) 0.85935(9) 0.0671(4) Uani 1 d . . . O11 O 0.9354(5) 0.1335(6) 0.9128(5) 0.153(3) Uani 1 d . . . O12 O 0.9579(5) 0.2570(4) 0.8296(3) 0.0897(14) Uani 1 d . . . O13 O 0.7784(5) 0.1711(4) 0.7931(3) 0.1066(18) Uani 1 d . . . O14 O 0.8350(6) 0.2783(7) 0.9047(5) 0.167(4) Uani 1 d . . . Cl2 Cl 0.67053(17) 0.00575(12) 0.30358(12) 0.0918(6) Uani 0.557(12) d PD A 1 O21 O 0.6735(8) -0.1007(6) 0.3116(7) 0.086(3) Uiso 0.557(12) d PD A 1 O22 O 0.7773(9) 0.0450(10) 0.3552(8) 0.129(5) Uiso 0.557(12) d PD A 1 O23 O 0.6256(14) 0.0284(12) 0.2214(8) 0.185(7) Uiso 0.557(12) d PD A 1 O24 O 0.5797(11) 0.0292(11) 0.3416(9) 0.168(6) Uiso 0.557(12) d PD A 1 Cl23 Cl 0.67053(17) 0.00575(12) 0.30358(12) 0.0918(6) Uani 0.443(12) d P A 2 O21' O 0.7574(12) 0.0078(11) 0.3880(8) 0.120(5) Uiso 0.443(12) d PD A 2 O22' O 0.7610(13) 0.0601(12) 0.2640(10) 0.143(7) Uiso 0.443(12) d PD A 2 O23' O 0.6597(13) -0.0818(9) 0.2684(10) 0.117(5) Uiso 0.443(12) d PD A 2 O24' O 0.5916(9) 0.0770(8) 0.2894(7) 0.090(4) Uiso 0.443(12) d PD 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 Cu1 0.0493(4) 0.0433(4) 0.0496(4) -0.0015(2) 0.0192(3) 0.0042(2) N1 0.098(4) 0.057(3) 0.068(3) -0.002(2) 0.033(3) -0.015(3) C2 0.086(5) 0.070(4) 0.077(4) 0.006(3) -0.005(4) -0.020(3) C3 0.053(3) 0.097(4) 0.064(3) 0.031(3) 0.014(3) 0.000(3) N4 0.049(2) 0.064(3) 0.053(2) 0.0113(19) 0.0195(19) 0.0047(19) C5 0.085(4) 0.079(4) 0.049(3) 0.012(3) 0.035(3) 0.029(3) C6 0.110(5) 0.060(3) 0.065(3) -0.012(3) 0.034(3) 0.014(3) N7 0.061(3) 0.054(2) 0.072(3) -0.009(2) 0.015(2) 0.002(2) C8 0.118(6) 0.059(4) 0.095(5) -0.007(3) 0.044(5) -0.019(4) C9 0.135(7) 0.052(3) 0.114(6) 0.008(4) 0.041(6) 0.018(4) C10 0.091(4) 0.065(3) 0.074(4) 0.016(3) 0.032(3) 0.017(3) N11 0.046(2) 0.061(3) 0.058(2) 0.0047(19) 0.0137(19) 0.0061(18) C12 0.058(3) 0.066(3) 0.046(3) 0.000(2) 0.012(2) 0.003(2) C13 0.051(3) 0.044(2) 0.052(3) 0.001(2) 0.022(2) -0.0005(19) N14 0.044(2) 0.049(2) 0.047(2) -0.0013(17) 0.0144(18) 0.0041(16) C15 0.049(3) 0.051(3) 0.062(3) -0.006(2) 0.014(2) 0.004(2) C16 0.054(3) 0.081(4) 0.069(4) -0.004(3) 0.005(3) 0.009(3) N17 0.089(4) 0.078(3) 0.051(3) 0.004(2) 0.018(3) 0.023(3) C18 0.110(6) 0.075(4) 0.090(5) 0.019(4) 0.037(4) 0.025(4) C19 0.100(5) 0.053(3) 0.110(5) 0.014(4) 0.013(4) 0.021(3) C20 0.101(6) 0.058(4) 0.143(7) 0.002(4) 0.046(5) -0.003(4) C21 0.072(5) 0.174(10) 0.087(5) 0.042(6) 0.035(4) 0.004(5) C22 0.081(6) 0.226(13) 0.106(7) 0.063(8) 0.064(5) 0.038(7) C23 0.116(7) 0.151(8) 0.072(4) 0.019(5) 0.054(5) 0.061(6) C31 0.083(4) 0.060(3) 0.070(3) -0.003(3) 0.043(3) -0.001(3) C32 0.072(4) 0.070(4) 0.093(5) -0.003(3) 0.053(4) 0.002(3) C33 0.047(3) 0.060(3) 0.118(6) -0.012(3) 0.034(3) 0.004(2) Cl1 0.0510(8) 0.0877(10) 0.0634(8) 0.0076(7) 0.0210(6) -0.0120(6) O11 0.095(4) 0.176(6) 0.163(6) 0.108(5) 0.013(4) -0.008(4) O12 0.084(3) 0.107(3) 0.090(3) 0.009(3) 0.046(3) -0.025(3) O13 0.092(3) 0.119(4) 0.084(3) 0.007(3) 0.000(3) -0.037(3) O14 0.083(4) 0.264(10) 0.175(7) -0.113(7) 0.070(5) -0.027(5) Cl2 0.0932(12) 0.0675(9) 0.0924(12) -0.0196(8) 0.0044(10) 0.0291(8) Cl23 0.0932(12) 0.0675(9) 0.0924(12) -0.0196(8) 0.0044(10) 0.0291(8) _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 N4 1.949(5) . ? Cu1 N14 2.017(5) . ? Cu1 N1 2.129(5) . ? Cu1 N7 2.170(5) . ? Cu1 N11 2.341(5) . ? Cu1 N17 2.411(5) . ? N1 C2 1.459(9) . ? N1 C20 1.560(9) . ? C2 C3 1.530(11) . ? C3 N4 1.352(8) . ? C3 C21 1.363(11) . ? N4 C5 1.335(7) . ? C5 C23 1.396(10) . ? C5 C6 1.515(10) . ? C6 N7 1.462(8) . ? N7 C8 1.465(8) . ? C8 C9 1.466(10) . ? C9 C10 1.502(10) . ? C10 N11 1.486(8) . ? N11 C12 1.459(7) . ? C12 C13 1.508(8) . ? C13 N14 1.327(7) . ? C13 C31 1.384(8) . ? N14 C15 1.361(7) . ? C15 C33 1.375(9) . ? C15 C16 1.488(9) . ? C16 N17 1.451(9) . ? N17 C18 1.461(8) . ? C18 C19 1.441(10) . ? C19 C20 1.497(11) . ? C21 C22 1.357(16) . ? C22 C23 1.381(15) . ? C31 C32 1.366(9) . ? C32 C33 1.370(10) . ? Cl1 O14 1.399(7) . ? Cl1 O11 1.401(6) . ? Cl1 O13 1.410(5) . ? Cl1 O12 1.429(5) . ? Cl2 O23 1.349(12) . ? Cl2 O22 1.391(10) . ? Cl2 O21 1.447(8) . ? Cl2 O24 1.494(12) . ? Cl23 O23 1.314(12) . ? Cl23 O24 1.320(10) . ? Cl23 O21 1.456(12) . ? Cl23 O22 1.648(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N14 172.20(16) . . ? N4 Cu1 N1 80.9(2) . . ? N14 Cu1 N1 96.1(2) . . ? N4 Cu1 N7 80.4(2) . . ? N14 Cu1 N7 103.27(18) . . ? N1 Cu1 N7 160.0(2) . . ? N4 Cu1 N11 97.30(19) . . ? N14 Cu1 N11 75.77(18) . . ? N1 Cu1 N11 96.05(19) . . ? N7 Cu1 N11 93.28(19) . . ? N4 Cu1 N17 111.7(2) . . ? N14 Cu1 N17 75.5(2) . . ? N1 Cu1 N17 93.5(2) . . ? N7 Cu1 N17 86.88(19) . . ? N11 Cu1 N17 150.55(18) . . ? C2 N1 C20 109.3(5) . . ? C2 N1 Cu1 106.6(4) . . ? C20 N1 Cu1 114.3(4) . . ? N1 C2 C3 111.2(5) . . ? N4 C3 C21 120.7(8) . . ? N4 C3 C2 113.6(6) . . ? C21 C3 C2 125.6(7) . . ? C5 N4 C3 121.3(6) . . ? C5 N4 Cu1 120.2(4) . . ? C3 N4 Cu1 118.2(4) . . ? N4 C5 C23 119.7(7) . . ? N4 C5 C6 114.8(5) . . ? C23 C5 C6 125.5(7) . . ? N7 C6 C5 112.0(5) . . ? C6 N7 C8 111.2(5) . . ? C6 N7 Cu1 108.5(4) . . ? C8 N7 Cu1 117.8(4) . . ? N7 C8 C9 116.2(6) . . ? C8 C9 C10 117.0(7) . . ? N11 C10 C9 114.1(5) . . ? C12 N11 C10 111.0(5) . . ? C12 N11 Cu1 102.4(3) . . ? C10 N11 Cu1 116.8(3) . . ? N11 C12 C13 110.4(4) . . ? N14 C13 C31 121.8(5) . . ? N14 C13 C12 116.2(5) . . ? C31 C13 C12 122.0(5) . . ? C13 N14 C15 118.9(5) . . ? C13 N14 Cu1 119.4(3) . . ? C15 N14 Cu1 121.6(4) . . ? N14 C15 C33 121.2(6) . . ? N14 C15 C16 115.4(5) . . ? C33 C15 C16 123.3(5) . . ? N17 C16 C15 112.6(5) . . ? C16 N17 C18 112.7(5) . . ? C16 N17 Cu1 103.3(3) . . ? C18 N17 Cu1 118.7(5) . . ? C19 C18 N17 113.9(6) . . ? C18 C19 C20 116.6(7) . . ? C19 C20 N1 113.2(6) . . ? C22 C21 C3 118.9(9) . . ? C21 C22 C23 121.2(8) . . ? C22 C23 C5 118.1(9) . . ? C32 C31 C13 119.4(6) . . ? C31 C32 C33 119.2(6) . . ? C32 C33 C15 119.4(6) . . ? O14 Cl1 O11 109.4(6) . . ? O14 Cl1 O13 109.8(4) . . ? O11 Cl1 O13 110.5(4) . . ? O14 Cl1 O12 108.7(4) . . ? O11 Cl1 O12 106.6(4) . . ? O13 Cl1 O12 111.7(3) . . ? O23 Cl2 O22 121.3(9) . . ? O23 Cl2 O21 108.2(8) . . ? O22 Cl2 O21 109.5(6) . . ? O23 Cl2 O24 108.1(8) . . ? O22 Cl2 O24 108.0(7) . . ? O21 Cl2 O24 99.7(7) . . ? O23 Cl23 O24 128.7(8) . . ? O23 Cl23 O21 113.0(8) . . ? O24 Cl23 O21 113.2(7) . . ? O23 Cl23 O22 100.9(8) . . ? O24 Cl23 O22 98.2(7) . . ? O21 Cl23 O22 92.4(7) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.760 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.095