# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/107 data_cobpye _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cobalt 4,4'-azopyridine Nitrate Complex, Dichloromethane solvate ; _chemical_name_common '{[Co2(4-apy)3(NO3)4]CH2Cl2}' _chemical_formula_moiety ? _chemical_formula_sum 'C15.50 H13 Cl Co N8 O6' _chemical_formula_weight 501.72 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' '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 '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 20.802(9) _cell_length_b 11.124(4) _cell_length_c 20.806(9) _cell_angle_alpha 90.00 _cell_angle_beta 119.27(4) _cell_angle_gamma 90.00 _cell_volume 4200(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.6519 _exptl_absorpt_correction_T_max 0.8411 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'STOE STADI-4 FOUR-CIRCLE' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% '+/- 4.4' _diffrn_reflns_number 5502 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3609 _reflns_number_gt 2681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR nd goodness of fit S are based on F^2^, conventional R-factors R are ased on F, with F set to zero for negative F^2^. The threshold expression f F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. nd is not relevant to the choice of reflections for refinement. R-factors ased on F^2^ are statistically about twice as large as those based on F, nd 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^)+(0.0598P)^2^+60.4364P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct Methods' _atom_sites_solution_secondary 'Difference Fourier Map' _atom_sites_solution_hydrogens 'Geometrically Placed ' _refine_ls_hydrogen_treatment 'Riding Model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3609 _refine_ls_number_parameters 293 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.134 _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 Co Co 0.71781(4) 0.88374(7) 0.84279(5) 0.0225(3) Uani 1 d U . . N1 N 0.6244(3) 0.9897(5) 0.7667(3) 0.0276(11) Uani 1 d U . . C2 C 0.6236(4) 1.1093(7) 0.7675(4) 0.0363(15) Uani 1 d U . . H2 H 0.6648 1.1505 0.8052 0.044 Uiso 1 calc R . . C3 C 0.5644(4) 1.1766(7) 0.7149(4) 0.0458(18) Uani 1 d U . . H3 H 0.5656 1.2620 0.7167 0.055 Uiso 1 calc R . . C4 C 0.5037(4) 1.1167(8) 0.6598(4) 0.0421(16) Uani 1 d U . . C5 C 0.5035(4) 0.9947(8) 0.6592(4) 0.0399(16) Uani 1 d U . . H5 H 0.4626 0.9511 0.6229 0.048 Uiso 1 calc R . . C6 C 0.5643(3) 0.9360(7) 0.7128(4) 0.0326(15) Uani 1 d U . . H6 H 0.5638 0.8507 0.7115 0.039 Uiso 1 calc R . . N7 N 0.4403(4) 1.1735(7) 0.5950(4) 0.0483(16) Uani 1 d U . . N10 N 0.6254(3) 0.7659(6) 0.8732(3) 0.0350(13) Uani 1 d U . . O11 O 0.6422(3) 0.7356(4) 0.8237(3) 0.0408(11) Uani 1 d U . . O12 O 0.6606(3) 0.8535(5) 0.9131(3) 0.0408(11) Uani 1 d U . . O13 O 0.5770(3) 0.7145(6) 0.8794(4) 0.0641(18) Uani 1 d U . . N20 N 0.7560(3) 0.8691(5) 0.7359(3) 0.0332(12) Uani 1 d U . . O21 O 0.7777(3) 0.9498(4) 0.7878(3) 0.0348(10) Uani 1 d U . . O22 O 0.7092(3) 0.7961(4) 0.7342(3) 0.0372(10) Uani 1 d U . . O23 O 0.7803(3) 0.8668(5) 0.6920(3) 0.0539(15) Uani 1 d U . . N31 N 0.7756(3) 1.0200(5) 0.9272(3) 0.0289(11) Uani 1 d U . . C32 C 0.8076(3) 1.1145(6) 0.9139(4) 0.0324(14) Uani 1 d U . . H32 H 0.7982 1.1290 0.8651 0.039 Uiso 1 calc R . . C33 C 0.8549(4) 1.1927(7) 0.9710(5) 0.0410(16) Uani 1 d U . . H33 H 0.8763 1.2602 0.9605 0.049 Uiso 1 calc R . . C34 C 0.8702(4) 1.1695(8) 1.0438(5) 0.0495(18) Uani 1 d U . . C35 C 0.8382(5) 1.0736(10) 1.0584(5) 0.061(3) Uani 1 d U . . H35 H 0.8483 1.0562 1.1071 0.073 Uiso 1 calc R . . C36 C 0.7902(4) 1.0023(8) 0.9989(4) 0.0453(19) Uani 1 d U . . H36 H 0.7660 0.9377 1.0082 0.054 Uiso 1 calc R . . N37 N 0.9286(4) 1.2307(7) 1.1120(4) 0.059(2) Uani 1 d U . . N61 N 0.8066(3) 0.7572(5) 0.8997(3) 0.0327(12) Uani 1 d U . . C62 C 0.7954(5) 0.6386(7) 0.8865(5) 0.0457(18) Uani 1 d U . . H62 H 0.7463 0.6114 0.8561 0.055 Uiso 1 calc R . . C63 C 0.8506(6) 0.5546(8) 0.9143(5) 0.059(2) Uani 1 d U . . H63 H 0.8393 0.4720 0.9028 0.071 Uiso 1 calc R . . C64 C 0.9215(5) 0.5897(10) 0.9585(5) 0.060(2) Uani 1 d U . . C65 C 0.9354(4) 0.7111(10) 0.9731(5) 0.057(2) Uani 1 d U . . H65 H 0.9844 0.7389 1.0032 0.069 Uiso 1 calc R . . C66 C 0.8762(4) 0.7929(8) 0.9428(4) 0.0466(18) Uani 1 d U . . H66 H 0.8860 0.8761 0.9534 0.056 Uiso 1 calc R . . N67 N 0.9755(4) 0.4723(7) 0.9812(4) 0.0538(16) Uani 1 d U . . C1 C 0.9309(9) 1.0671(16) 0.8117(8) 0.052(4) Uiso 0.50 d PDU . . H1A H 0.9436 1.1529 0.8115 0.062 Uiso 0.50 calc PR . . H1B H 0.8767 1.0608 0.7885 0.062 Uiso 0.50 calc PR . . Cl1 Cl 0.9618(6) 0.9827(10) 0.7592(7) 0.189(4) Uani 0.50 d PDU . . Cl2 Cl 0.9705(4) 1.0165(7) 0.9011(6) 0.140(3) Uani 0.50 d PDU . . 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 Co 0.0164(4) 0.0187(4) 0.0238(5) 0.0002(4) 0.0033(3) 0.0022(4) N1 0.022(2) 0.031(2) 0.024(2) 0.002(2) 0.0068(18) 0.004(2) C2 0.026(3) 0.031(3) 0.043(4) 0.005(3) 0.010(3) 0.007(3) C3 0.046(4) 0.036(4) 0.050(4) 0.018(3) 0.019(3) 0.013(3) C4 0.027(3) 0.064(4) 0.036(4) 0.020(3) 0.015(2) 0.014(3) C5 0.025(3) 0.060(4) 0.026(3) 0.014(3) 0.006(3) 0.001(3) C6 0.021(3) 0.044(4) 0.025(3) 0.006(3) 0.006(2) 0.002(2) N7 0.044(3) 0.045(4) 0.054(4) 0.007(3) 0.022(3) 0.008(3) N10 0.028(3) 0.039(3) 0.030(3) 0.007(2) 0.007(2) -0.005(2) O11 0.040(2) 0.030(2) 0.053(3) 0.001(2) 0.023(2) -0.002(2) O12 0.033(2) 0.047(3) 0.036(3) -0.002(2) 0.013(2) -0.013(2) O13 0.058(4) 0.065(4) 0.081(5) -0.006(3) 0.043(3) -0.031(3) N20 0.036(3) 0.029(3) 0.036(3) 0.001(2) 0.019(3) 0.006(2) O21 0.036(2) 0.032(3) 0.037(3) -0.0020(18) 0.019(2) 0.0000(19) O22 0.039(3) 0.032(3) 0.038(2) -0.004(2) 0.017(2) -0.0012(19) O23 0.070(4) 0.054(4) 0.061(4) -0.004(3) 0.050(3) 0.004(3) N31 0.019(2) 0.030(3) 0.030(2) -0.004(2) 0.006(2) -0.0011(19) C32 0.025(3) 0.022(3) 0.039(3) -0.002(3) 0.007(3) 0.003(2) C33 0.027(3) 0.029(4) 0.060(3) -0.012(3) 0.015(3) -0.008(3) C34 0.032(4) 0.058(5) 0.051(3) -0.023(4) 0.015(3) -0.008(3) C35 0.049(5) 0.096(7) 0.036(4) -0.028(4) 0.019(4) -0.034(5) C36 0.037(4) 0.064(5) 0.029(3) -0.013(3) 0.011(3) -0.017(4) N37 0.065(5) 0.057(5) 0.055(4) -0.016(4) 0.029(4) -0.018(4) N61 0.030(2) 0.031(2) 0.033(3) 0.006(2) 0.012(2) 0.012(2) C62 0.057(4) 0.028(3) 0.049(5) 0.003(3) 0.023(4) 0.016(3) C63 0.087(4) 0.041(4) 0.057(5) 0.020(4) 0.042(4) 0.035(3) C64 0.070(4) 0.084(4) 0.043(5) 0.038(4) 0.041(4) 0.045(4) C65 0.027(3) 0.094(4) 0.047(5) 0.022(5) 0.015(3) 0.027(3) C66 0.023(3) 0.061(4) 0.045(5) 0.004(4) 0.009(3) 0.010(3) N67 0.060(4) 0.058(4) 0.048(4) -0.010(3) 0.030(4) -0.021(3) Cl1 0.165(10) 0.149(9) 0.215(9) 0.080(8) 0.063(9) -0.011(7) Cl2 0.073(4) 0.080(5) 0.286(10) -0.016(6) 0.104(6) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. lanes) are estimated using the full covariance matrix. The cell esds are aken into account individually in the estimation of esds in distances, ngles and torsion angles; correlations between esds in cell parameters are nly used when they are defined by crystal symmetry. An approximate isotropic) treatment of cell esds is used for estimating esds involving l.s. lanes. ; 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 Co N61 2.159(5) . y Co N1 2.159(5) . y Co O11 2.176(5) . y Co N31 2.182(6) . y Co O21 2.191(5) . y Co O12 2.318(5) . y Co O22 2.387(5) . y N1 C2 1.330(9) . ? N1 C6 1.345(8) . ? C2 C3 1.400(10) . ? C3 C4 1.392(11) . ? C4 C5 1.358(12) . ? C4 N7 1.489(9) . ? C5 C6 1.373(9) . ? N7 N37 1.184(10) 8_475 ? N10 O13 1.219(8) . ? N10 O12 1.256(8) . ? N10 O11 1.285(8) . ? N20 O23 1.242(7) . ? N20 O22 1.254(7) . ? N20 O21 1.303(7) . ? N31 C32 1.344(9) . ? N31 C36 1.383(9) . ? C32 C33 1.412(10) . ? C33 C34 1.412(12) . ? C34 C35 1.366(13) . ? C34 N37 1.506(10) . ? C35 C36 1.397(11) . ? N37 N7 1.184(10) 8_576 ? N61 C66 1.337(9) . ? N61 C62 1.344(9) . ? C62 C63 1.369(11) . ? C63 C64 1.360(14) . ? C64 C65 1.383(15) . ? C64 N67 1.634(12) . ? C65 C66 1.409(11) . ? N67 N67 1.118(13) 5_767 ? C1 Cl2 1.720(14) . ? C1 Cl1 1.781(15) . ? Cl1 Cl1 1.81(2) 2_756 ? 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 N61 Co N1 168.6(2) . . y N61 Co O11 87.4(2) . . ? N1 Co O11 88.2(2) . . ? N61 Co N31 91.4(2) . . y N1 Co N31 98.9(2) . . y O11 Co N31 137.5(2) . . ? N61 Co O21 87.3(2) . . ? N1 Co O21 88.4(2) . . ? O11 Co O21 134.7(2) . . ? N31 Co O21 87.5(2) . . ? N61 Co O12 97.2(2) . . ? N1 Co O12 89.2(2) . . ? O11 Co O12 57.12(19) . . ? N31 Co O12 81.00(19) . . ? O21 Co O12 167.78(18) . . ? N61 Co O22 84.3(2) . . ? N1 Co O22 84.55(19) . . ? O11 Co O22 78.74(19) . . ? N31 Co O22 143.4(2) . . ? O21 Co O22 55.99(18) . . ? O12 Co O22 135.61(18) . . ? C2 N1 C6 116.2(6) . . ? C2 N1 Co 123.3(5) . . ? C6 N1 Co 120.4(5) . . ? N1 C2 C3 122.5(7) . . ? C4 C3 C2 119.0(8) . . ? C5 C4 C3 118.9(7) . . ? C5 C4 N7 114.8(7) . . ? C3 C4 N7 126.0(8) . . ? C4 C5 C6 118.1(7) . . ? N1 C6 C5 125.3(7) . . ? N37 N7 C4 109.4(7) 8_475 . ? O13 N10 O12 122.6(7) . . ? O13 N10 O11 121.6(6) . . ? O12 N10 O11 115.8(6) . . ? N10 O11 Co 96.3(4) . . ? N10 O12 Co 90.5(4) . . ? O23 N20 O22 123.7(6) . . ? O23 N20 O21 121.4(6) . . ? O22 N20 O21 114.9(5) . . ? N20 O21 Co 98.4(4) . . ? N20 O22 Co 90.6(4) . . ? C32 N31 C36 117.6(6) . . ? C32 N31 Co 120.7(5) . . ? C36 N31 Co 120.9(5) . . ? N31 C32 C33 121.4(7) . . ? C34 C33 C32 119.3(7) . . ? C35 C34 C33 120.2(7) . . ? C35 C34 N37 113.6(8) . . ? C33 C34 N37 125.6(8) . . ? C34 C35 C36 117.5(8) . . ? N31 C36 C35 124.0(8) . . ? N7 N37 C34 108.4(8) 8_576 . ? C66 N61 C62 116.9(7) . . ? C66 N61 Co 122.0(5) . . ? C62 N61 Co 120.7(5) . . ? N61 C62 C63 123.8(9) . . ? C64 C63 C62 119.9(9) . . ? C63 C64 C65 118.0(8) . . ? C63 C64 N67 109.4(9) . . ? C65 C64 N67 132.6(9) . . ? C64 C65 C66 119.3(9) . . ? N61 C66 C65 122.0(9) . . ? N67 N67 C64 91.4(10) 5_767 . ? Cl2 C1 Cl1 111.4(10) . . ? C1 Cl1 Cl1 138.4(9) . 2_756 ? _diffrn_measured_fraction_theta_max 0.462 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.462 _refine_diff_density_max 1.174 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.121 #===END data_cdaznt _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cadmium 4,4'-azopyridine Nitrate Complex, water/dichloromethane solvate ; _chemical_name_common '[Cd2(4-apy)3(NO3)4](CH2Cl2)(H2O)2' _chemical_formula_moiety ? _chemical_formula_sum 'C15.50 H15 Cd Cl N8 O7' _chemical_formula_weight 573.21 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' 'Cd' 'Cd' -0.8075 1.2024 '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 21.197(5) _cell_length_b 11.166(12) _cell_length_c 21.389(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.24(2) _cell_angle_gamma 90.00 _cell_volume 4282(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description 'Irregular Tablet' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5326 _exptl_absorpt_correction_T_max 0.7374 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'STOE STADI-4 FOUR-CIRCLE' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 3801 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.08 _reflns_number_total 3771 _reflns_number_gt 3210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR nd goodness of fit S are based on F^2^, conventional R-factors R are ased on F, with F set to zero for negative F^2^. The threshold expression f F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. nd is not relevant to the choice of reflections for refinement. R-factors ased on F^2^ are statistically about twice as large as those based on F, nd 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^)+(0.0342P)^2^+53.6746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct Methods' _atom_sites_solution_secondary 'Difference Fourier Maps' _atom_sites_solution_hydrogens 'Geometrically Placed' _refine_ls_hydrogen_treatment 'Riding Model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3771 _refine_ls_number_parameters 306 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.160 _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 Cd Cd 0.21593(2) 0.88306(3) 0.84283(2) 0.02657(14) Uani 1 d U . . N1 N 0.3064(2) 0.7427(4) 0.8976(3) 0.0308(10) Uani 1 d U . . C1 C 0.0577(7) 0.5509(12) 0.6847(7) 0.059(3) Uani 0.50 d PDU A -1 H1A H 0.0445 0.6367 0.6812 0.070 Uiso 0.50 calc PR A -1 H1B H 0.1128 0.5453 0.7142 0.070 Uiso 0.50 calc PR A -1 Cl1 Cl 0.0261(2) 0.4989(4) 0.5975(2) 0.0611(10) Uani 0.50 d PDU A -1 O1W O 0.0777(7) 0.6741(12) 0.6453(7) 0.075(3) Uiso 0.50 d P B -2 C2 C 0.2938(3) 0.6266(5) 0.8796(3) 0.0395(15) Uani 1 d U . . H2 H 0.2439 0.6026 0.8453 0.047 Uiso 1 calc R . . N2 N 0.4697(3) 0.4811(5) 0.9783(3) 0.0360(11) Uani 1 d U . . Cl2 Cl 0.0217(3) 0.4724(5) 0.7352(3) 0.0899(15) Uani 0.50 d PDU A -1 O2W O 0.0045(13) 0.496(2) 0.5322(11) 0.141(7) Uiso 0.50 d P C -2 C3 C 0.3473(3) 0.5406(6) 0.9066(3) 0.0408(15) Uani 1 d U . . H3 H 0.3357 0.4590 0.8927 0.049 Uiso 1 calc R . . C4 C 0.4164(3) 0.5763(5) 0.9533(3) 0.0332(13) Uani 1 d U . . C5 C 0.4300(3) 0.6951(6) 0.9722(4) 0.0401(15) Uani 1 d U . . H5 H 0.4797 0.7213 1.0058 0.048 Uiso 1 calc R . . C6 C 0.3737(3) 0.7751(6) 0.9437(4) 0.0393(15) Uani 1 d U . . H6 H 0.3842 0.8568 0.9580 0.047 Uiso 1 calc R . . N10 N 0.1236(3) 0.7489(5) 0.8771(3) 0.0466(13) Uani 1 d U . . O13 O 0.0778(4) 0.6968(7) 0.8865(4) 0.098(3) Uani 1 d U . . O12 O 0.1585(2) 0.8360(4) 0.9180(3) 0.0479(11) Uani 1 d U . . O11 O 0.1350(2) 0.7219(4) 0.8246(2) 0.0396(10) Uani 1 d U . . N20 N 0.2647(3) 0.8717(5) 0.7357(3) 0.0404(12) Uani 1 d U . . O21 O 0.2169(3) 0.7997(4) 0.7307(2) 0.0464(11) Uani 1 d U . . O23 O 0.2922(3) 0.8641(5) 0.6941(3) 0.0564(13) Uani 1 d U . . O22 O 0.2842(2) 0.9534(4) 0.7845(2) 0.0422(10) Uani 1 d U . . N31 N 0.1172(2) 0.9915(5) 0.7604(3) 0.0328(11) Uani 1 d U . . C32 C 0.0585(3) 0.9342(7) 0.7104(3) 0.0442(16) Uani 1 d U . . H32 H 0.0579 0.8491 0.7117 0.053 Uiso 1 calc R . . C33 C -0.0011(3) 0.9929(8) 0.6571(4) 0.0518(18) Uani 1 d U . . H33 H -0.0437 0.9498 0.6208 0.062 Uiso 1 calc R . . C34 C -0.0004(3) 1.1125(8) 0.6552(3) 0.0508(17) Uani 1 d U . . C35 C 0.0584(4) 1.1742(7) 0.7061(4) 0.0568(19) Uani 1 d U . . H35 H 0.0589 1.2593 0.7059 0.068 Uiso 1 calc R . . C36 C 0.1173(3) 1.1105(6) 0.7583(3) 0.0417(15) Uani 1 d U . . H36 H 0.1605 1.1523 0.7949 0.050 Uiso 1 calc R . . N61 N 0.2733(2) 1.0322(4) 0.9301(3) 0.0342(11) Uani 1 d U . . C62 C 0.2834(4) 1.0197(8) 0.9989(4) 0.060(2) Uani 1 d U . . H62 H 0.2567 0.9581 1.0057 0.072 Uiso 1 calc R . . N62 N 0.4192(4) 1.2444(7) 1.1080(4) 0.068(2) Uani 1 d U . . C63 C 0.3295(5) 1.0904(9) 1.0577(5) 0.075(3) Uani 1 d U . . H63 H 0.3371 1.0786 1.1052 0.091 Uiso 1 calc R . . N63 N 0.4380(4) 1.3326(7) 1.0938(4) 0.0678(19) Uani 1 d U . . C64 C 0.3649(4) 1.1822(7) 1.0429(4) 0.0515(18) Uani 1 d U . . C65 C 0.3549(3) 1.1978(6) 0.9731(4) 0.0447(15) Uani 1 d U . . H65 H 0.3798 1.2605 0.9646 0.054 Uiso 1 calc R . . C66 C 0.3085(3) 1.1207(6) 0.9174(4) 0.0432(15) Uani 1 d U . . H66 H 0.3010 1.1296 0.8697 0.052 Uiso 1 calc R . . 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 Cd 0.01569(19) 0.0251(2) 0.0249(2) 0.00059(16) 0.00144(15) 0.00158(15) N1 0.018(2) 0.030(2) 0.031(2) 0.0035(19) 0.0038(18) 0.0039(18) C1 0.031(7) 0.032(7) 0.082(8) -0.009(6) 0.010(6) 0.003(5) Cl1 0.0411(18) 0.069(3) 0.071(2) -0.012(2) 0.0287(18) 0.0048(17) C2 0.022(3) 0.030(3) 0.044(3) -0.003(3) 0.003(2) 0.001(2) N2 0.027(2) 0.036(3) 0.034(3) 0.005(2) 0.009(2) 0.007(2) Cl2 0.111(4) 0.071(3) 0.087(4) -0.012(3) 0.052(3) -0.006(3) C3 0.031(3) 0.028(3) 0.042(3) 0.001(3) 0.005(3) 0.005(2) C4 0.026(3) 0.032(3) 0.033(3) 0.009(2) 0.010(2) 0.011(2) C5 0.021(3) 0.037(3) 0.044(3) 0.001(3) 0.005(2) 0.004(2) C6 0.022(3) 0.032(3) 0.048(4) 0.000(3) 0.007(3) 0.002(2) N10 0.036(3) 0.049(3) 0.051(3) -0.004(3) 0.021(3) -0.012(2) O13 0.106(5) 0.115(6) 0.109(5) -0.048(5) 0.081(5) -0.075(5) O12 0.035(2) 0.056(3) 0.047(3) -0.011(2) 0.018(2) -0.014(2) O11 0.028(2) 0.038(2) 0.043(2) 0.0000(19) 0.0128(18) -0.0039(17) N20 0.039(3) 0.042(3) 0.036(3) 0.011(2) 0.017(2) 0.020(2) O21 0.044(2) 0.043(3) 0.038(2) -0.004(2) 0.013(2) -0.001(2) O23 0.064(3) 0.055(3) 0.061(3) 0.012(3) 0.040(3) 0.017(3) O22 0.039(2) 0.040(2) 0.045(3) 0.0003(19) 0.021(2) 0.0003(19) N31 0.018(2) 0.039(3) 0.028(2) 0.005(2) 0.0031(18) 0.0023(19) C32 0.026(3) 0.054(4) 0.033(3) 0.013(3) 0.003(2) -0.004(3) C33 0.023(3) 0.080(5) 0.034(3) 0.023(3) 0.003(3) 0.001(3) C34 0.027(3) 0.085(5) 0.029(3) 0.016(3) 0.007(2) 0.024(3) C35 0.056(4) 0.049(4) 0.046(4) 0.017(3) 0.014(3) 0.023(3) C36 0.030(3) 0.038(3) 0.036(3) 0.004(3) 0.004(3) 0.006(3) N61 0.021(2) 0.033(3) 0.033(2) -0.005(2) 0.0037(19) -0.0024(19) C62 0.050(4) 0.083(6) 0.049(4) -0.026(4) 0.027(4) -0.037(4) N62 0.065(4) 0.083(5) 0.059(4) -0.037(4) 0.034(4) -0.044(4) C63 0.072(5) 0.111(7) 0.051(4) -0.043(5) 0.038(4) -0.058(5) N63 0.058(4) 0.086(5) 0.046(4) -0.016(3) 0.019(3) -0.032(4) C64 0.033(3) 0.065(5) 0.046(4) -0.027(3) 0.015(3) -0.017(3) C65 0.032(3) 0.033(3) 0.048(3) -0.003(3) 0.007(3) -0.006(3) C66 0.037(3) 0.033(3) 0.033(3) -0.001(3) 0.001(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. lanes) are estimated using the full covariance matrix. The cell esds are aken into account individually in the estimation of esds in distances, ngles and torsion angles; correlations between esds in cell parameters are nly used when they are defined by crystal symmetry. An approximate isotropic) treatment of cell esds is used for estimating esds involving l.s. lanes. ; 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 Cd N31 2.240(4) . y Cd N1 2.260(5) . y Cd N61 2.305(5) . y Cd O11 2.370(4) . y Cd O22 2.489(5) . y Cd O12 2.535(5) . y Cd O21 2.583(5) . y N1 C6 1.280(7) . ? N1 C2 1.339(8) . ? C1 Cl1 1.712(12) . ? C1 Cl2 1.842(13) . ? C2 C3 1.358(8) . ? N2 N2 1.192(10) 5_667 ? N2 C4 1.431(7) . ? C3 C4 1.319(8) . ? C4 C5 1.372(9) . ? C5 C6 1.349(8) . ? N10 O13 1.237(8) . ? N10 O12 1.252(7) . ? N10 O11 1.304(7) . ? N20 O21 1.252(7) . ? N20 O22 1.277(7) . ? N20 O23 1.300(7) . ? N31 C32 1.296(8) . ? N31 C36 1.329(8) . ? C32 C33 1.338(8) . ? C33 C34 1.337(11) . ? C34 C35 1.328(11) . ? C34 N63 1.407(8) 8_475 ? C35 C36 1.351(8) . ? N61 C66 1.349(8) . ? N61 C62 1.377(9) . ? C62 C63 1.360(10) . ? N62 N63 1.162(10) . ? N62 C64 1.427(8) . ? C63 C64 1.402(11) . ? N63 C34 1.407(8) 8_576 ? C64 C65 1.403(10) . ? C65 C66 1.371(9) . ? 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 N31 Cd N1 163.93(18) . . y N31 Cd N61 96.57(18) . . y N1 Cd N61 98.38(17) . . y N31 Cd O11 89.47(17) . . ? N1 Cd O11 84.15(17) . . ? N61 Cd O11 134.79(17) . . ? N31 Cd O22 89.07(16) . . ? N1 Cd O22 85.38(16) . . ? N61 Cd O22 88.92(17) . . ? O11 Cd O22 136.08(15) . . ? N31 Cd O12 92.76(17) . . ? N1 Cd O12 95.08(17) . . ? N61 Cd O12 82.01(17) . . ? O11 Cd O12 52.90(15) . . ? O22 Cd O12 170.90(15) . . ? N31 Cd O21 86.05(17) . . ? N1 Cd O21 78.86(16) . . ? N61 Cd O21 138.57(17) . . ? O11 Cd O21 86.42(16) . . ? O22 Cd O21 49.70(15) . . ? O12 Cd O21 139.32(16) . . ? C6 N1 C2 117.7(5) . . ? C6 N1 Cd 119.5(4) . . ? C2 N1 Cd 122.6(4) . . ? Cl1 C1 Cl2 115.7(7) . . ? N1 C2 C3 124.7(5) . . ? N2 N2 C4 109.6(6) 5_667 . ? C4 C3 C2 116.5(6) . . ? C3 C4 C5 119.3(5) . . ? C3 C4 N2 113.2(5) . . ? C5 C4 N2 127.5(5) . . ? C6 C5 C4 120.7(6) . . ? N1 C6 C5 121.0(6) . . ? O13 N10 O12 118.4(6) . . ? O13 N10 O11 123.6(6) . . ? O12 N10 O11 117.9(5) . . ? N10 O12 Cd 91.3(4) . . ? N10 O11 Cd 97.7(3) . . ? O21 N20 O22 115.0(5) . . ? O21 N20 O23 122.4(6) . . ? O22 N20 O23 122.5(6) . . ? N20 O21 Cd 95.5(3) . . ? N20 O22 Cd 99.4(4) . . ? C32 N31 C36 118.9(5) . . ? C32 N31 Cd 117.7(4) . . ? C36 N31 Cd 123.3(4) . . ? N31 C32 C33 121.0(7) . . ? C34 C33 C32 119.6(7) . . ? C35 C34 C33 121.0(6) . . ? C35 C34 N63 122.5(8) . 8_475 ? C33 C34 N63 116.3(7) . 8_475 ? C34 C35 C36 117.0(7) . . ? N31 C36 C35 122.5(6) . . ? C66 N61 C62 120.1(5) . . ? C66 N61 Cd 118.4(4) . . ? C62 N61 Cd 120.4(4) . . ? C63 C62 N61 123.7(7) . . ? N63 N62 C64 111.6(7) . . ? C62 C63 C64 115.0(7) . . ? N62 N63 C34 113.6(7) . 8_576 ? C63 C64 C65 122.4(6) . . ? C63 C64 N62 112.7(7) . . ? C65 C64 N62 124.3(7) . . ? C66 C65 C64 118.6(6) . . ? N61 C66 C65 120.2(6) . . ? _diffrn_measured_fraction_theta_max 0.421 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.421 _refine_diff_density_max 1.092 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.117