Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'G. Ciani' 'Lucia Carlucci' 'Francesca Porta' 'Davide M. Prosperio' _publ_contact_author_name 'Gianfranco Ciani' _publ_contact_author_address ; Dipartimento di Chimica Strutturale e Stereochimica Universita di Milano Inorganica and Centro CNR Via G. Venezian 21 Milano 20133 ITALY ; _publ_contact_author_email DAVIDE.PROSERPIO@ISTM.CNR.IT _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; New metal-organic frameworks and supramolecular arrays assembled with the bent ditopic ligand 4,4-diaminodiphenylmethane ; data_1 _database_code_depnum_ccdc_archive 'CCDC 606682' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C13 H14 Cl2 Co N2' _chemical_formula_weight 328.09 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' 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 Orthorhombic _symmetry_space_group_name_H-M Im2m _symmetry_Int_Tables_number 44 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y, -z' '-x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 12.7148(8) _cell_length_b 4.4248(3) _cell_length_c 11.6928(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 657.84(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 984 _cell_measurement_theta_min 2 _cell_measurement_theta_max 21 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 334 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 3308 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 24.93 _reflns_number_total 622 _reflns_number_observed 521 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^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 constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(3) _refine_ls_number_reflns 622 _refine_ls_number_parameters 52 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_obs 0.0264 _refine_ls_wR_factor_all 0.0437 _refine_ls_wR_factor_obs 0.0411 _refine_ls_goodness_of_fit_all 0.930 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.0000 -0.80011(19) 0.0000 0.0292(3) Uani 1 4 d S . . Cl Cl 0.0000 -0.5273(3) 0.16228(9) 0.0385(4) Uani 1 2 d S . . N1 N -0.1378(2) -1.0418(8) 0.0000 0.0319(9) Uani 1 2 d S . . H1 H -0.1395 -1.1614 -0.0622 0.038 Uiso 1 1 d R . . C4 C -0.4029(3) -0.4622(9) 0.0000 0.0230(11) Uani 1 2 d S . . C1 C -0.2292(3) -0.8500(10) 0.0000 0.0242(11) Uani 1 2 d S . . C2 C -0.2724(2) -0.7523(8) 0.1005(3) 0.0308(8) Uani 1 1 d . . . H2 H -0.2434 -0.8149 0.1696 0.037 Uiso 1 1 calc R . . C3 C -0.3586(2) -0.5616(7) 0.1009(3) 0.0290(8) Uani 1 1 d . . . H3 H -0.3872 -0.4995 0.1702 0.035 Uiso 1 1 calc R . . C5 C -0.5000 -0.270(2) 0.0000 0.0314(16) Uani 1 4 d S . . H5 H -0.5000 -0.1409 -0.0671 0.038 Uiso 1 2 d SR . . 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 0.0209(5) 0.0302(6) 0.0366(7) 0.000 0.000 0.000 Cl 0.0409(8) 0.0402(8) 0.0344(8) -0.0019(7) 0.000 0.000 N1 0.026(2) 0.023(2) 0.047(2) 0.000 0.000 -0.0019(19) C4 0.012(2) 0.021(3) 0.035(3) 0.000 0.000 -0.0057(19) C1 0.0118(19) 0.016(3) 0.045(3) 0.000 0.000 -0.004(2) C2 0.0273(15) 0.036(2) 0.029(2) 0.006(2) -0.0021(14) 0.0001(18) C3 0.0189(16) 0.035(2) 0.033(2) -0.0053(19) 0.0030(14) -0.0006(16) C5 0.021(3) 0.030(4) 0.044(4) 0.000 0.000 0.000 _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 Co N1 2.052(3) . ? Co N1 2.052(3) 3 ? Co Cl 2.2488(12) . ? Co Cl 2.2488(12) 2 ? Co Cl 3.7357(14) 2_545 ? Co Cl 3.7357(14) 1_545 ? Cl Co 3.7357(14) 1_565 ? N1 C1 1.439(5) . ? N1 C5 5.734(6) . ? N1 N1 9.212(6) 3_455 ? N1 H1 0.9000 . ? C4 C3 1.379(3) . ? C4 C3 1.379(3) 2 ? C4 C5 1.500(6) . ? C1 C2 1.367(3) . ? C1 C2 1.367(3) 2 ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C4 1.500(6) 3_455 ? C5 N1 5.734(6) 3_455 ? C5 H5 0.9700 . ? 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 N1 Co N1 117.2(2) . 3 ? N1 Co Cl 106.24(5) . . ? N1 Co Cl 106.24(5) 3 . ? N1 Co Cl 106.24(5) . 2 ? N1 Co Cl 106.24(5) 3 2 ? Cl Co Cl 115.08(7) . 2 ? N1 Co Cl 63.33(9) . 2_545 ? N1 Co Cl 63.33(9) 3 2_545 ? Cl Co Cl 152.99(4) . 2_545 ? Cl Co Cl 91.93(4) 2 2_545 ? N1 Co Cl 63.33(8) . 1_545 ? N1 Co Cl 63.33(8) 3 1_545 ? Cl Co Cl 91.93(4) . 1_545 ? Cl Co Cl 152.99(4) 2 1_545 ? Cl Co Cl 61.05(4) 2_545 1_545 ? Co Cl Co 91.93(4) . 1_565 ? C1 N1 Co 112.5(3) . . ? C1 N1 C5 0.4(2) . . ? Co N1 C5 112.04(13) . . ? C1 N1 N1 36.1(2) . 3_455 ? Co N1 N1 148.60(10) . 3_455 ? C5 N1 N1 36.56(7) . 3_455 ? C1 N1 H1 109.1 . . ? Co N1 H1 109.1 . . ? C5 N1 H1 109.3 . . ? N1 N1 H1 88.6 3_455 . ? C3 C4 C3 117.6(4) . 2 ? C3 C4 C5 121.13(19) . . ? C3 C4 C5 121.13(19) 2 . ? C2 C1 C2 118.5(4) . 2 ? C2 C1 N1 120.71(19) . . ? C2 C1 N1 120.71(19) 2 . ? C1 C2 C3 120.9(3) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C4 C5 C4 110.9(6) 3_455 . ? C4 C5 N1 2.0(3) 3_455 3_455 ? C4 C5 N1 108.9(4) . 3_455 ? C4 C5 N1 108.9(4) 3_455 . ? C4 C5 N1 2.0(3) . . ? N1 C5 N1 106.88(15) 3_455 . ? C4 C5 H5 109.5 3_455 . ? C4 C5 H5 109.5 . . ? N1 C5 H5 110.5 3_455 . ? N1 C5 H5 110.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co N1 C5 N1 180.0 . . . 3_455 ? Co N1 N1 Co 0.0 . . 3_455 3_455 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.232 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.059 data_2 _database_code_depnum_ccdc_archive 'CCDC 606683' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C13 H14 Cd Cl2 N2' _chemical_formula_weight 381.56 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.3881(10) _cell_length_b 4.2929(3) _cell_length_c 12.2521(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.273(2) _cell_angle_gamma 90.00 _cell_volume 668.67(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 678 _cell_measurement_theta_min 3 _cell_measurement_theta_max 21 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 2.014 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 3613 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1638 _reflns_number_observed 1562 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.2441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1638 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_obs 0.0222 _refine_ls_wR_factor_all 0.0561 _refine_ls_wR_factor_obs 0.0556 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.5000 0.04279(5) 0.2500 0.03595(8) Uani 1 2 d S . . Cl Cl 0.42390(4) -0.37469(13) 0.10099(4) 0.04025(12) Uani 1 1 d . . . N1 N 0.64246(12) 0.2030(4) 0.20198(15) 0.0372(4) Uani 1 1 d . . . H11 H 0.6192 0.2618 0.1278 0.045 Uiso 1 1 calc R . . H12 H 0.6673 0.3754 0.2434 0.045 Uiso 1 1 calc R . . C1 C 0.73041(15) -0.0011(4) 0.21494(18) 0.0303(4) Uani 1 1 d . . . C2 C 0.80071(17) -0.0622(5) 0.32281(18) 0.0364(4) Uani 1 1 d . . . H2 H 0.7902 0.0254 0.3878 0.044 Uiso 1 1 calc R . . C3 C 0.88633(14) -0.2532(5) 0.33384(17) 0.0388(4) Uani 1 1 d . . . H3 H 0.9333 -0.2915 0.4066 0.047 Uiso 1 1 calc R . . C4 C 0.90375(14) -0.3895(4) 0.23844(19) 0.0349(4) Uani 1 1 d . . . C5 C 0.83068(16) -0.3348(5) 0.13232(18) 0.0386(4) Uani 1 1 d . . . H5 H 0.8393 -0.4296 0.0676 0.046 Uiso 1 1 calc R . . C6 C 0.74486(15) -0.1421(5) 0.11998(17) 0.0364(4) Uani 1 1 d . . . H6 H 0.6969 -0.1078 0.0475 0.044 Uiso 1 1 calc R . . C7 C 1.0000 -0.5867(7) 0.2500 0.0480(8) Uani 1 2 d S . . H7 H 1.0129 -0.7196 0.3170 0.058 Uiso 1 1 d 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 0.02666(11) 0.04115(13) 0.04403(13) 0.000 0.01681(8) 0.000 Cl 0.0421(3) 0.0425(3) 0.0344(2) -0.00388(18) 0.00950(19) 0.0025(2) N1 0.0323(8) 0.0293(8) 0.0550(10) 0.0045(7) 0.0209(7) 0.0031(6) C1 0.0254(8) 0.0256(8) 0.0438(10) 0.0022(7) 0.0166(7) -0.0024(6) C2 0.0350(10) 0.0401(10) 0.0382(10) -0.0039(8) 0.0173(8) -0.0028(8) C3 0.0290(8) 0.0443(11) 0.0412(10) 0.0052(8) 0.0083(7) -0.0016(8) C4 0.0262(8) 0.0242(8) 0.0580(12) 0.0003(8) 0.0184(8) -0.0037(7) C5 0.0394(10) 0.0359(10) 0.0466(10) -0.0069(8) 0.0223(8) -0.0024(8) C6 0.0352(9) 0.0379(10) 0.0361(9) 0.0008(8) 0.0112(7) 0.0000(8) C7 0.0293(14) 0.0271(14) 0.091(3) 0.000 0.0232(15) 0.000 _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 Cd N1 2.2717(15) . ? Cd N1 2.2717(15) 2_655 ? Cd Cl 2.5331(5) . ? Cd Cl 2.5331(5) 2_655 ? Cd Cl 3.0754(6) 2_665 ? Cd Cl 3.0754(6) 1_565 ? Cl Cd 3.0754(6) 1_545 ? N1 C1 1.436(2) . ? N1 C7 5.743(2) . ? N1 N1 9.272(3) 2_755 ? N1 H11 0.9000 . ? N1 H12 0.9000 . ? C1 C6 1.378(3) . ? C1 C2 1.386(3) . ? C2 C3 1.381(3) . ? C2 H2 0.9300 . ? C3 C4 1.391(3) . ? C3 H3 0.9300 . ? C4 C5 1.380(3) . ? C4 C7 1.511(2) . ? C5 C6 1.385(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C4 1.511(2) 2_755 ? C7 N1 5.743(2) 2_755 ? C7 H7 0.9700 . ? 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 N1 Cd N1 144.75(8) . 2_655 ? N1 Cd Cl 102.02(5) . . ? N1 Cd Cl 102.72(4) 2_655 . ? N1 Cd Cl 102.72(4) . 2_655 ? N1 Cd Cl 102.02(5) 2_655 2_655 ? Cl Cd Cl 89.94(3) . 2_655 ? N1 Cd Cl 76.04(5) . 2_665 ? N1 Cd Cl 75.46(4) 2_655 2_665 ? Cl Cd Cl 170.630(16) . 2_665 ? Cl Cd Cl 99.434(16) 2_655 2_665 ? N1 Cd Cl 75.46(4) . 1_565 ? N1 Cd Cl 76.04(5) 2_655 1_565 ? Cl Cd Cl 99.434(16) . 1_565 ? Cl Cd Cl 170.630(16) 2_655 1_565 ? Cl Cd Cl 71.20(2) 2_665 1_565 ? Cd Cl Cd 99.434(16) . 1_545 ? C1 N1 Cd 120.83(12) . . ? C1 N1 C7 1.53(9) . . ? Cd N1 C7 122.36(6) . . ? C1 N1 N1 37.61(10) . 2_755 ? Cd N1 N1 152.18(5) . 2_755 ? C7 N1 N1 36.17(3) . 2_755 ? C1 N1 H11 107.1 . . ? Cd N1 H11 107.1 . . ? C7 N1 H11 106.4 . . ? N1 N1 H11 98.3 2_755 . ? C1 N1 H12 107.1 . . ? Cd N1 H12 107.1 . . ? C7 N1 H12 106.2 . . ? N1 N1 H12 75.2 2_755 . ? H11 N1 H12 106.8 . . ? C6 C1 C2 119.27(18) . . ? C6 C1 N1 120.13(18) . . ? C2 C1 N1 120.59(18) . . ? C3 C2 C1 120.02(19) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.35(18) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 117.65(17) . . ? C5 C4 C7 121.03(17) . . ? C3 C4 C7 121.31(16) . . ? C4 C5 C6 121.54(18) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 120.09(18) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C4 C7 C4 111.9(2) 2_755 . ? C4 C7 N1 2.19(10) 2_755 2_755 ? C4 C7 N1 109.75(14) . 2_755 ? C4 C7 N1 109.75(14) 2_755 . ? C4 C7 N1 2.19(10) . . ? N1 C7 N1 107.65(6) 2_755 . ? C4 C7 H7 109.2 2_755 . ? C4 C7 H7 109.2 . . ? N1 C7 H7 109.8 2_755 . ? N1 C7 H7 110.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd N1 C7 N1 -155.14(8) . . . 2_755 ? N1 C7 N1 Cd -155.14(8) . . 2_755 2_755 ? Cd N1 N1 Cd 99.1(2) . . 2_755 2_755 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.451 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.094 data_3 _database_code_depnum_ccdc_archive 'CCDC 606684' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C13 H14 Ag N3 O3' _chemical_formula_weight 368.14 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcca _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 25.028(3) _cell_length_b 4.4533(5) _cell_length_c 11.8686(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1322.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 564 _cell_measurement_theta_min 2 _cell_measurement_theta_max 22 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 9624 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.06 _reflns_number_total 1172 _reflns_number_observed 1167 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+14.5130P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1172 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_obs 0.0897 _refine_ls_wR_factor_all 0.1402 _refine_ls_wR_factor_obs 0.1401 _refine_ls_goodness_of_fit_all 1.401 _refine_ls_restrained_S_all 1.401 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.2500 0.0000 0.09048(11) 0.0580(4) Uani 1 2 d S . . C1 C 0.1297(3) 0.003(3) 0.1590(9) 0.046(2) Uani 1 1 d . . . N1 N 0.1720(3) -0.2003(17) 0.1303(7) 0.044(2) Uani 1 1 d . . . H1A H 0.1615 -0.3094 0.0705 0.052 Uiso 1 1 calc R . . H1B H 0.1765 -0.3282 0.1883 0.052 Uiso 1 1 calc R . . C6 C 0.1273(3) 0.131(2) 0.2648(8) 0.044(2) Uani 1 1 d . . . H6 H 0.1532 0.0857 0.3182 0.052 Uiso 1 1 calc R . . C4 C 0.0469(3) 0.3962(18) 0.2167(8) 0.037(2) Uani 1 1 d . . . C2 C 0.0913(3) 0.0784(17) 0.0804(8) 0.038(2) Uani 1 1 d . . . H2 H 0.0929 0.0011 0.0077 0.046 Uiso 1 1 calc R . . C7 C 0.0000 0.587(3) 0.2500 0.046(3) Uani 1 2 d S . . H7B H 0.0100 0.7153 0.3127 0.055 Uiso 0.50 1 calc PR . . H7A H -0.0100 0.7153 0.1873 0.055 Uiso 0.50 1 calc PR . . C3 C 0.0506(3) 0.270(2) 0.1114(8) 0.039(2) Uani 1 1 d . . . H3 H 0.0244 0.3167 0.0585 0.047 Uiso 1 1 calc R . . C5 C 0.0866(3) 0.325(2) 0.2913(8) 0.042(2) Uani 1 1 d . . . H5 H 0.0860 0.4116 0.3626 0.051 Uiso 1 1 calc R . . O12 O 0.2130(3) 0.379(2) -0.0654(7) 0.078(3) Uani 1 1 d . . . O11 O 0.2500 0.5000 -0.2199(9) 0.083(4) Uani 1 2 d S . . N2 N 0.2500 0.5000 -0.1174(10) 0.050(3) Uani 1 2 d S . . 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 Ag 0.0343(5) 0.0646(7) 0.0752(8) 0.000 0.000 0.0056(6) C1 0.040(4) 0.035(4) 0.063(6) 0.019(6) 0.014(5) 0.004(5) N1 0.038(4) 0.033(4) 0.059(5) 0.005(4) 0.011(4) 0.006(4) C6 0.034(5) 0.057(6) 0.040(5) 0.004(5) 0.001(4) -0.005(4) C4 0.038(5) 0.025(4) 0.047(5) 0.001(4) 0.009(4) -0.007(4) C2 0.054(5) 0.022(4) 0.039(5) -0.007(4) 0.005(4) -0.001(4) C7 0.059(8) 0.021(6) 0.058(9) 0.000 0.014(7) 0.000 C3 0.039(5) 0.038(5) 0.040(5) 0.007(4) -0.001(4) 0.002(4) C5 0.044(5) 0.043(5) 0.041(5) -0.007(5) 0.009(4) -0.008(5) O12 0.073(5) 0.092(7) 0.069(5) 0.024(5) 0.011(4) -0.012(5) O11 0.078(7) 0.123(11) 0.049(7) 0.000 0.000 -0.013(10) N2 0.055(7) 0.046(6) 0.050(7) 0.000 0.000 0.006(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 Ag N1 2.197(7) 2 ? Ag N1 2.197(7) . ? Ag O12 2.669(8) 2 ? Ag O12 2.669(8) . ? C1 C2 1.379(12) . ? C1 C6 1.381(14) . ? C1 N1 1.435(11) . ? N1 C7 5.732(10) . ? N1 N1 9.068(13) 4 ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C6 C5 1.371(12) . ? C6 H6 0.9300 . ? C4 C5 1.369(13) . ? C4 C3 1.372(12) . ? C4 C7 1.502(10) . ? C2 C3 1.382(12) . ? C2 H2 0.9300 . ? C7 C4 1.502(10) 4 ? C7 N1 5.732(10) 4 ? C7 H7B 0.9700 . ? C7 H7A 0.9700 . ? C3 H3 0.9300 . ? C5 H5 0.9300 . ? O12 N2 1.236(9) . ? O11 N2 1.216(14) . ? N2 O12 1.236(9) 2_565 ? 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 N1 Ag N1 155.1(4) 2 . ? N1 Ag O12 95.6(3) 2 2 ? N1 Ag O12 101.6(3) . 2 ? N1 Ag O12 101.6(3) 2 . ? N1 Ag O12 95.6(3) . . ? O12 Ag O12 92.2(4) 2 . ? C2 C1 C6 119.0(9) . . ? C2 C1 N1 120.5(9) . . ? C6 C1 N1 120.6(9) . . ? C2 C1 Ag 119.7(6) . . ? C6 C1 Ag 106.3(6) . . ? N1 C1 Ag 38.9(4) . . ? C1 N1 Ag 116.8(6) . . ? C1 N1 C7 1.4(5) . . ? Ag N1 C7 118.2(3) . . ? C1 N1 N1 39.1(5) . 4 ? Ag N1 N1 155.6(2) . 4 ? C7 N1 N1 37.72(12) . 4 ? C1 N1 H1A 108.1 . . ? Ag N1 H1A 108.1 . . ? C7 N1 H1A 107.8 . . ? N1 N1 H1A 88.2 4 . ? C1 N1 H1B 108.1 . . ? Ag N1 H1B 108.1 . . ? C7 N1 H1B 107.0 . . ? N1 N1 H1B 83.1 4 . ? H1A N1 H1B 107.3 . . ? C5 C6 C1 120.1(9) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C5 C4 C3 116.5(8) . . ? C5 C4 C7 121.9(7) . . ? C3 C4 C7 121.6(8) . . ? C1 C2 C3 119.0(9) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C7 C4 111.0(9) 4 . ? C4 C7 N1 3.2(4) 4 4 ? C4 C7 N1 107.8(5) . 4 ? C4 C7 N1 107.8(5) 4 . ? C4 C7 N1 3.2(4) . . ? N1 C7 N1 104.6(2) 4 . ? C4 C7 H7B 109.4 4 . ? C4 C7 H7B 109.4 . . ? N1 C7 H7B 111.3 4 . ? N1 C7 H7B 110.8 . . ? C4 C7 H7A 109.4 4 . ? C4 C7 H7A 109.4 . . ? N1 C7 H7A 110.8 4 . ? N1 C7 H7A 111.3 . . ? H7B C7 H7A 108.0 . . ? C4 C3 C2 123.0(9) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C4 C5 C6 122.5(9) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? N2 O12 Ag 111.3(6) . . ? O11 N2 O12 119.9(6) . 2_565 ? O11 N2 O12 119.9(6) . . ? O12 N2 O12 120.1(12) 2_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag N1 C7 N1 -175.2(4) . . . 4 ? N1 C7 N1 Ag -175.2(4) . . 4 4 ? Ag N1 N1 Ag 20.6(15) . . 4 4 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.650 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.110 data_4 _database_code_depnum_ccdc_archive 'CCDC 606685' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C26 H32 Cl2 N4 Ni O2' _chemical_formula_weight 562.17 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' 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' O O 0.0106 0.0060 '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/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.029(3) _cell_length_b 11.995(3) _cell_length_c 9.153(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.951(6) _cell_angle_gamma 90.00 _cell_volume 1319.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2463 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description cube _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 4695 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2224 _reflns_number_observed 1827 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+4.7759P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2224 _refine_ls_number_parameters 166 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_obs 0.0470 _refine_ls_wR_factor_all 0.1638 _refine_ls_wR_factor_obs 0.1516 _refine_ls_goodness_of_fit_all 1.203 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.0000 0.5000 0.0286(3) Uani 1 2 d S . . Cl Cl 0.95571(13) 0.34589(12) 0.60461(16) 0.0478(4) Uani 1 1 d . . . O O 0.1005(3) -0.1308(3) 0.5687(4) 0.0400(9) Uani 1 1 d D . . H2W H 0.086(5) -0.198(2) 0.516(4) 0.048 Uiso 1 1 d D . . H1W H 0.086(5) -0.157(4) 0.665(2) 0.048 Uiso 1 1 d D . . N1 N 0.0614(3) 0.0928(4) 0.6938(5) 0.0354(10) Uani 1 1 d . . . H1A H 0.0213 0.1561 0.6964 0.042 Uiso 1 1 calc RD . . H1B H 0.0425 0.0524 0.7720 0.042 Uiso 1 1 calc RD . . N2 N 0.8689(3) -0.0657(4) 0.6274(5) 0.0339(10) Uani 1 1 d . . . H2A H 0.8381 -0.1226 0.5762 0.041 Uiso 1 1 calc RD . . H2B H 0.9010 -0.0954 0.7087 0.041 Uiso 1 1 calc RD . . C10 C 0.7873(5) 0.0603(5) 0.8039(6) 0.0443(14) Uani 1 1 d . . . H10 H 0.8510 0.0522 0.8633 0.053 Uiso 1 1 calc R . . C3 C 0.3284(5) 0.2501(5) 0.6831(7) 0.0427(13) Uani 1 1 d . . . H3 H 0.3556 0.3144 0.6401 0.051 Uiso 1 1 calc R . . C1 C 0.1768(4) 0.1251(4) 0.7192(6) 0.0336(12) Uani 1 1 d . . . C8 C 0.6074(4) 0.1437(5) 0.7598(6) 0.0398(13) Uani 1 1 d . . . C6 C 0.2467(5) 0.0597(5) 0.8054(6) 0.0406(13) Uani 1 1 d . . . H6 H 0.2201 -0.0051 0.8478 0.049 Uiso 1 1 calc R . . C2 C 0.2181(4) 0.2203(4) 0.6572(6) 0.0375(12) Uani 1 1 d . . . H2 H 0.1720 0.2647 0.5979 0.045 Uiso 1 1 calc R . . C11 C 0.7791(4) 0.0039(4) 0.6734(6) 0.0340(11) Uani 1 1 d . . . C13 C 0.5995(5) 0.0857(5) 0.6308(7) 0.0441(14) Uani 1 1 d . . . H13 H 0.5358 0.0936 0.5712 0.053 Uiso 1 1 calc R . . C5 C 0.3569(5) 0.0911(5) 0.8285(7) 0.0474(15) Uani 1 1 d . . . H5 H 0.4038 0.0454 0.8850 0.057 Uiso 1 1 calc R . . C4 C 0.3987(4) 0.1864(5) 0.7713(7) 0.0439(14) Uani 1 1 d . . . C7 C 0.5177(5) 0.2238(6) 0.8067(8) 0.0586(18) Uani 1 1 d . . . H7A H 0.5296 0.2952 0.7600 0.070 Uiso 1 1 calc R . . H7B H 0.5261 0.2351 0.9115 0.070 Uiso 1 1 calc R . . C9 C 0.7029(5) 0.1285(5) 0.8483(7) 0.0484(15) Uani 1 1 d . . . H9 H 0.7097 0.1648 0.9379 0.058 Uiso 1 1 calc R . . C12 C 0.6831(4) 0.0161(5) 0.5867(6) 0.0396(13) Uani 1 1 d . . . H12 H 0.6752 -0.0226 0.4990 0.048 Uiso 1 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 Ni 0.0242(5) 0.0281(5) 0.0332(5) 0.0010(4) -0.0047(3) 0.0014(4) Cl 0.0551(9) 0.0417(8) 0.0452(8) -0.0096(6) -0.0176(6) 0.0140(6) O 0.039(2) 0.0317(19) 0.049(2) 0.0011(17) -0.0088(18) 0.0044(16) N1 0.030(2) 0.037(2) 0.038(3) 0.000(2) -0.0046(18) 0.0006(18) N2 0.031(2) 0.038(2) 0.032(2) 0.0050(19) -0.0036(18) -0.0048(18) C10 0.031(3) 0.067(4) 0.034(3) -0.010(3) -0.009(2) -0.004(3) C3 0.041(3) 0.034(3) 0.054(4) -0.009(3) 0.007(3) -0.005(2) C1 0.029(3) 0.036(3) 0.035(3) -0.007(2) -0.003(2) -0.001(2) C8 0.033(3) 0.044(3) 0.041(3) -0.007(3) -0.002(2) -0.007(2) C6 0.039(3) 0.042(3) 0.041(3) 0.004(3) -0.006(2) -0.006(2) C2 0.035(3) 0.033(3) 0.044(3) -0.003(2) 0.000(2) 0.004(2) C11 0.027(2) 0.033(3) 0.042(3) -0.001(2) 0.001(2) -0.005(2) C13 0.032(3) 0.052(3) 0.048(4) -0.010(3) -0.007(2) 0.002(3) C5 0.038(3) 0.049(4) 0.054(4) -0.005(3) -0.014(3) 0.007(3) C4 0.029(3) 0.044(3) 0.060(4) -0.018(3) 0.003(2) -0.002(2) C7 0.035(3) 0.058(4) 0.082(5) -0.030(4) -0.003(3) -0.004(3) C9 0.033(3) 0.064(4) 0.048(4) -0.018(3) -0.003(3) -0.004(3) C12 0.038(3) 0.052(3) 0.029(3) -0.008(3) -0.005(2) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O 2.066(4) . ? Ni O 2.066(4) 3_556 ? Ni N2 2.144(4) 3_656 ? Ni N2 2.144(4) 1_455 ? Ni N1 2.201(4) . ? Ni N1 2.201(4) 3_556 ? Cl O 3.091(4) 3_656 ? Cl O 3.100(4) 2_656 ? Cl Cl 4.314(3) 3_766 ? O Cl 3.091(4) 3_656 ? O Cl 3.100(4) 2_646 ? O H2W 0.951(10) . ? O H1W 0.952(10) . ? N1 C1 1.452(6) . ? N1 C7 5.769(7) . ? N1 N2 9.936(6) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C11 1.439(7) . ? N2 Ni 2.144(4) 1_655 ? N2 C7 5.751(7) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C10 C11 1.373(8) . ? C10 C9 1.375(8) . ? C10 H10 0.9300 . ? C3 C4 1.380(8) . ? C3 C2 1.387(7) . ? C3 H3 0.9300 . ? C1 C2 1.375(8) . ? C1 C6 1.378(8) . ? C8 C13 1.371(8) . ? C8 C9 1.395(8) . ? C8 C7 1.518(8) . ? C6 C5 1.388(8) . ? C6 H6 0.9300 . ? C2 H2 0.9300 . ? C11 C12 1.387(7) . ? C13 C12 1.378(8) . ? C13 H13 0.9300 . ? C5 C4 1.361(9) . ? C5 H5 0.9300 . ? C4 C7 1.524(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 H9 0.9300 . ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Ni O 180.0 . 3_556 ? O Ni N2 90.65(16) . 3_656 ? O Ni N2 89.35(16) 3_556 3_656 ? O Ni N2 89.35(16) . 1_455 ? O Ni N2 90.65(16) 3_556 1_455 ? N2 Ni N2 180.00(14) 3_656 1_455 ? O Ni N1 87.82(16) . . ? O Ni N1 92.18(16) 3_556 . ? N2 Ni N1 91.12(16) 3_656 . ? N2 Ni N1 88.88(16) 1_455 . ? O Ni N1 92.18(16) . 3_556 ? O Ni N1 87.82(16) 3_556 3_556 ? N2 Ni N1 88.88(16) 3_656 3_556 ? N2 Ni N1 91.12(16) 1_455 3_556 ? N1 Ni N1 180.0 . 3_556 ? O Cl O 121.26(11) 3_656 2_656 ? O Cl Cl 122.70(9) 3_656 3_766 ? O Cl Cl 114.60(8) 2_656 3_766 ? Ni O Cl 111.21(15) . 3_656 ? Ni O Cl 102.55(15) . 2_646 ? Cl O Cl 111.64(12) 3_656 2_646 ? Ni O H2W 113(3) . . ? Cl O H2W 2(4) 3_656 . ? Cl O H2W 112(3) 2_646 . ? Ni O H1W 114(3) . . ? Cl O H1W 99(3) 3_656 . ? Cl O H1W 14(3) 2_646 . ? H2W O H1W 99.0(13) . . ? C1 N1 Ni 123.8(3) . . ? C1 N1 C7 1.2(3) . . ? Ni N1 C7 124.99(16) . . ? C1 N1 N2 29.5(3) . . ? Ni N1 N2 98.96(12) . . ? C7 N1 N2 30.34(7) . . ? C1 N1 H1A 106.4 . . ? Ni N1 H1A 106.4 . . ? C7 N1 H1A 105.9 . . ? N2 N1 H1A 133.6 . . ? C1 N1 H1B 106.4 . . ? Ni N1 H1B 106.4 . . ? C7 N1 H1B 105.6 . . ? N2 N1 H1B 102.6 . . ? H1A N1 H1B 106.5 . . ? C11 N2 Ni 121.2(3) . 1_655 ? C11 N2 C7 1.7(2) . . ? Ni N2 C7 119.63(16) 1_655 . ? C11 N2 N1 29.1(2) . . ? Ni N2 N1 134.57(13) 1_655 . ? C7 N2 N1 30.45(7) . . ? C11 N2 H2A 107.0 . . ? Ni N2 H2A 107.0 1_655 . ? C7 N2 H2A 108.2 . . ? N1 N2 H2A 77.9 . . ? C11 N2 H2B 107.0 . . ? Ni N2 H2B 107.0 1_655 . ? C7 N2 H2B 107.5 . . ? N1 N2 H2B 114.7 . . ? H2A N2 H2B 106.8 . . ? C11 C10 C9 121.2(5) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C4 C3 C2 121.4(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C2 C1 C6 119.2(5) . . ? C2 C1 N1 120.8(5) . . ? C6 C1 N1 120.0(5) . . ? C13 C8 C9 117.7(5) . . ? C13 C8 C7 122.4(5) . . ? C9 C8 C7 119.9(5) . . ? C1 C6 C5 119.6(5) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C1 C2 C3 120.0(5) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C10 C11 C12 118.6(5) . . ? C10 C11 N2 120.6(5) . . ? C12 C11 N2 120.8(5) . . ? C8 C13 C12 122.0(5) . . ? C8 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C4 C5 C6 122.2(6) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C4 C3 117.6(5) . . ? C5 C4 C7 121.5(6) . . ? C3 C4 C7 120.9(6) . . ? C8 C7 C4 115.2(5) . . ? C8 C7 N2 2.1(3) . . ? C4 C7 N2 117.1(3) . . ? C8 C7 N1 117.3(3) . . ? C4 C7 N1 2.4(3) . . ? N2 C7 N1 119.21(12) . . ? C8 C7 H7A 108.5 . . ? C4 C7 H7A 108.5 . . ? N2 C7 H7A 106.6 . . ? N1 C7 H7A 108.3 . . ? C8 C7 H7B 108.5 . . ? C4 C7 H7B 108.5 . . ? N2 C7 H7B 108.3 . . ? N1 C7 H7B 106.4 . . ? H7A C7 H7B 107.5 . . ? C10 C9 C8 120.5(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni N1 C7 N2 -35.0(3) . . . . ? N1 C7 N2 Ni 128.72(19) . . . 1_655 ? Ni N1 N2 Ni 79.4(2) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.752 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.104 data_5a _database_code_depnum_ccdc_archive 'CCDC 606686' _exptl_absorpt_correction_nazim 3 _diffrn_measurement_domega 1.1+0.35tg(theta) _diffrn_measurement_rtime 60 _chemical_formula_sum 'C26 H32 Cl2 N4 Ni O2' _chemical_formula_weight 562.17 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.6600(10) _cell_length_b 9.323(3) _cell_length_c 12.687(4) _cell_angle_alpha 103.60(2) _cell_angle_beta 93.39(2) _cell_angle_gamma 102.01(2) _cell_volume 632.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4 _cell_measurement_theta_max 24 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 294 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _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 CAD4 _diffrn_measurement_method omega-scan _diffrn_standards_number 3 _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 0 _diffrn_reflns_number 2210 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1650 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2210 _reflns_number_observed 1179 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 2210 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1767 _refine_ls_R_factor_obs 0.0619 _refine_ls_wR_factor_all 0.1660 _refine_ls_wR_factor_obs 0.1350 _refine_ls_goodness_of_fit_all 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 -0.5000 0.5000 0.0309(4) Uani 1 2 d S . . Cl Cl 0.2246(3) -0.5403(2) 0.63822(14) 0.0473(5) Uani 1 1 d . . . O1W O 0.2158(8) -0.6114(5) 0.3801(4) 0.0426(12) Uiso 1 1 d . . . H1W1 H 0.2784 -0.6376 0.3112 0.064 Uiso 1 1 d R . . H1W2 H 0.1070 -0.5459 0.3761 0.064 Uiso 1 1 d R . . N1 N 0.3951(9) -0.2988(6) 0.4924(4) 0.0338(13) Uani 1 1 d . . . H1A H 0.4339 -0.2811 0.4281 0.041 Uiso 1 1 calc R . . H1B H 0.2317 -0.3203 0.4878 0.041 Uiso 1 1 calc R . . C3 C 0.4070(11) 0.0350(7) 0.7220(5) 0.0347(16) Uani 1 1 d . . . H3 H 0.3020 0.0703 0.7702 0.042 Uiso 1 1 calc R . . N2 N 1.3151(11) 0.2313(7) 1.1807(5) 0.0549(17) Uani 1 1 d . . . H2A H 1.4664 0.2851 1.1844 0.082 Uiso 1 1 d R . . H2B H 1.3170 0.1343 1.1735 0.082 Uiso 1 1 d R . . C1 C 0.4781(11) -0.1562(7) 0.5727(5) 0.0324(15) Uani 1 1 d . . . C6 C 0.7124(11) -0.0696(8) 0.5772(5) 0.0345(16) Uani 1 1 d . . . H6 H 0.8171 -0.1044 0.5287 0.041 Uiso 1 1 calc R . . C4 C 0.6395(11) 0.1228(7) 0.7271(5) 0.0322(15) Uani 1 1 d . . . C2 C 0.3275(11) -0.1039(8) 0.6467(5) 0.0395(17) Uani 1 1 d . . . H2 H 0.1723 -0.1620 0.6461 0.047 Uiso 1 1 calc R . . C5 C 0.7887(12) 0.0666(7) 0.6529(5) 0.0378(17) Uani 1 1 d . . . H5 H 0.9455 0.1233 0.6546 0.045 Uiso 1 1 calc R . . C8 C 0.8816(12) 0.2633(7) 0.9081(5) 0.0356(16) Uani 1 1 d . . . C7 C 0.7281(12) 0.2749(8) 0.8108(5) 0.0407(17) Uani 1 1 d . . . H7A H 0.8225 0.3468 0.7765 0.049 Uiso 1 1 calc R . . H7B H 0.5888 0.3133 0.8353 0.049 Uiso 1 1 calc R . . C12 C 1.2634(13) 0.3341(8) 1.0220(6) 0.0447(18) Uani 1 1 d . . . H12 H 1.4237 0.3896 1.0369 0.054 Uiso 1 1 calc R . . C9 C 0.7930(13) 0.1753(8) 0.9765(6) 0.0491(19) Uani 1 1 d . . . H9 H 0.6317 0.1215 0.9625 0.059 Uiso 1 1 calc R . . C10 C 0.9325(14) 0.1641(9) 1.0636(6) 0.051(2) Uani 1 1 d . . . H10 H 0.8661 0.1026 1.1075 0.061 Uiso 1 1 calc R . . C11 C 1.1742(13) 0.2442(8) 1.0880(5) 0.0417(17) Uani 1 1 d . . . C13 C 1.1209(12) 0.3439(8) 0.9345(6) 0.0450(18) Uani 1 1 d . . . H13 H 1.1867 0.4067 0.8913 0.054 Uiso 1 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 Ni 0.0243(7) 0.0363(8) 0.0292(8) 0.0069(6) -0.0026(5) 0.0034(6) Cl 0.0377(11) 0.0625(14) 0.0481(12) 0.0214(10) 0.0135(9) 0.0149(9) N1 0.034(3) 0.032(3) 0.031(3) 0.004(2) -0.004(2) 0.004(2) C3 0.030(3) 0.043(4) 0.033(4) 0.009(3) 0.006(3) 0.012(3) N2 0.053(4) 0.063(4) 0.042(4) 0.004(3) -0.009(3) 0.014(3) C1 0.029(3) 0.034(4) 0.037(4) 0.015(3) -0.004(3) 0.009(3) C6 0.031(4) 0.047(4) 0.029(4) 0.010(3) 0.009(3) 0.015(3) C4 0.030(4) 0.031(4) 0.035(4) 0.011(3) -0.003(3) 0.006(3) C2 0.024(3) 0.047(4) 0.041(4) 0.012(3) 0.001(3) -0.005(3) C5 0.030(4) 0.036(4) 0.047(4) 0.019(4) 0.001(3) -0.002(3) C8 0.042(4) 0.029(4) 0.033(4) 0.000(3) 0.000(3) 0.011(3) C7 0.040(4) 0.040(4) 0.040(4) 0.008(3) 0.003(3) 0.008(3) C12 0.035(4) 0.038(4) 0.050(5) 0.006(4) -0.006(3) -0.007(3) C9 0.040(4) 0.051(5) 0.048(5) 0.010(4) 0.000(4) -0.002(4) C10 0.053(5) 0.055(5) 0.043(4) 0.018(4) 0.008(4) 0.001(4) C11 0.050(4) 0.043(4) 0.026(4) 0.001(3) -0.003(3) 0.010(3) C13 0.041(4) 0.039(4) 0.047(4) 0.009(3) 0.004(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1W 2.062(4) . ? Ni O1W 2.062(4) 2_646 ? Ni N1 2.103(5) . ? Ni N1 2.103(5) 2_646 ? Ni Cl 2.4569(17) 2_646 ? Ni Cl 2.4569(17) . ? O1W H1W1 0.9600 . ? O1W H1W2 0.9600 . ? N1 C1 1.440(8) . ? N1 C7 5.764(8) . ? N1 N2 9.561(8) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C3 C2 1.385(9) . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? N2 C11 1.424(8) . ? N2 H1W1 1.8646 1_666 ? N2 C7 5.730(9) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? C1 C2 1.377(9) . ? C1 C6 1.392(9) . ? C6 C5 1.368(9) . ? C6 H6 0.9300 . ? C4 C5 1.385(9) . ? C4 C7 1.525(9) . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C8 C9 1.376(10) . ? C8 C13 1.385(9) . ? C8 C7 1.504(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C12 C11 1.365(9) . ? C12 C13 1.365(10) . ? C12 H12 0.9300 . ? C9 C10 1.357(10) . ? C9 H9 0.9300 . ? C10 C11 1.393(10) . ? C10 H10 0.9300 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Ni O1W 180.0(2) . 2_646 ? O1W Ni N1 86.83(19) . . ? O1W Ni N1 93.17(19) 2_646 . ? O1W Ni N1 93.17(19) . 2_646 ? O1W Ni N1 86.83(19) 2_646 2_646 ? N1 Ni N1 180.0 . 2_646 ? O1W Ni Cl 91.01(13) . 2_646 ? O1W Ni Cl 88.99(13) 2_646 2_646 ? N1 Ni Cl 88.70(15) . 2_646 ? N1 Ni Cl 91.30(15) 2_646 2_646 ? O1W Ni Cl 88.99(13) . . ? O1W Ni Cl 91.01(13) 2_646 . ? N1 Ni Cl 91.30(15) . . ? N1 Ni Cl 88.70(15) 2_646 . ? Cl Ni Cl 180.00(6) 2_646 . ? Ni O1W H1W1 109.3 . . ? Ni O1W H1W2 109.2 . . ? H1W1 O1W H1W2 109.5 . . ? C1 N1 Ni 124.5(4) . . ? C1 N1 C7 0.5(3) . . ? Ni N1 C7 124.92(18) . . ? C1 N1 N2 33.2(3) . . ? Ni N1 N2 91.44(14) . . ? C7 N1 N2 33.60(9) . . ? C1 N1 H1A 106.2 . . ? Ni N1 H1A 106.2 . . ? C7 N1 H1A 105.7 . . ? N2 N1 H1A 124.1 . . ? C1 N1 H1B 106.2 . . ? Ni N1 H1B 106.2 . . ? C7 N1 H1B 106.3 . . ? N2 N1 H1B 119.0 . . ? H1A N1 H1B 106.4 . . ? C2 C3 C4 121.5(6) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C11 N2 H1W1 113.8 . 1_666 ? C11 N2 C7 1.4(4) . . ? H1W1 N2 C7 113.5 1_666 . ? C11 N2 N1 34.3(4) . . ? H1W1 N2 N1 139.1 1_666 . ? C7 N2 N1 33.83(8) . . ? C11 N2 H2A 109.2 . . ? H1W1 N2 H2A 89.1 1_666 . ? C7 N2 H2A 110.6 . . ? N1 N2 H2A 121.0 . . ? C11 N2 H2B 109.0 . . ? H1W1 N2 H2B 123.8 1_666 . ? C7 N2 H2B 108.4 . . ? N1 N2 H2B 74.7 . . ? H2A N2 H2B 109.5 . . ? C2 C1 C6 119.0(6) . . ? C2 C1 N1 120.5(6) . . ? C6 C1 N1 120.4(6) . . ? C5 C6 C1 120.0(6) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C5 C4 C3 117.3(6) . . ? C5 C4 C7 121.2(6) . . ? C3 C4 C7 121.5(6) . . ? C1 C2 C3 120.1(6) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C6 C5 C4 122.0(6) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C9 C8 C13 116.3(6) . . ? C9 C8 C7 122.5(6) . . ? C13 C8 C7 121.2(6) . . ? C8 C7 C4 112.4(5) . . ? C8 C7 N2 0.2(3) . . ? C4 C7 N2 112.4(4) . . ? C8 C7 N1 112.6(4) . . ? C4 C7 N1 0.3(3) . . ? N2 C7 N1 112.57(15) . . ? C8 C7 H7A 109.1 . . ? C4 C7 H7A 109.1 . . ? N2 C7 H7A 109.0 . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7B 109.1 . . ? C4 C7 H7B 109.1 . . ? N2 C7 H7B 109.3 . . ? N1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C11 C12 C13 121.0(6) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C10 C9 C8 122.4(7) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 120.6(7) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 117.7(6) . . ? C12 C11 N2 123.0(7) . . ? C10 C11 N2 119.2(6) . . ? C12 C13 C8 122.0(7) . . ? C12 C13 H13 119.0 . . ? C8 C13 H13 119.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni N1 C7 N2 -5.7(3) . . . . ? N1 C7 N2 H1W1 -146.2 . . . 1_666 ? Ni N1 N2 H1W1 -133.5 . . . 1_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.594 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.105 data_5b _database_code_depnum_ccdc_archive 'CCDC 606687' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 30 _chemical_formula_sum 'C26 H32 Cl2 Mn N4 O2' _chemical_formula_weight 558.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.6911(7) _cell_length_b 9.5004(12) _cell_length_c 12.7455(16) _cell_angle_alpha 104.059(5) _cell_angle_beta 92.721(5) _cell_angle_gamma 102.425(5) _cell_volume 649.19(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 472 _cell_measurement_theta_min 4 _cell_measurement_theta_max 24 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 291 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 6558 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2293 _reflns_number_observed 1762 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.1176P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2293 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_obs 0.0385 _refine_ls_wR_factor_all 0.1084 _refine_ls_wR_factor_obs 0.0990 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.5000 -0.5000 0.5000 0.0327(2) Uani 1 2 d S . . Cl Cl 0.22326(13) -0.54489(9) 0.64539(6) 0.0564(3) Uani 1 1 d . . . O1W O 0.1971(3) -0.6126(2) 0.37560(16) 0.0498(5) Uiso 1 1 d . . . H1W1 H 0.2598 -0.6388 0.3067 0.075 Uiso 1 1 d R . . H1W2 H 0.0884 -0.5472 0.3715 0.075 Uiso 1 1 d R . . N1 N 0.3841(4) -0.2850(2) 0.49460(18) 0.0437(6) Uani 1 1 d . . . H1A H 0.4214 -0.2667 0.4306 0.052 Uiso 1 1 calc R . . H1B H 0.2216 -0.3064 0.4916 0.052 Uiso 1 1 calc R . . C3 C 0.4083(5) 0.0421(3) 0.7278(2) 0.0441(7) Uani 1 1 d . . . H3 H 0.3065 0.0775 0.7775 0.053 Uiso 1 1 calc R . . N2 N 1.3122(5) 0.2288(3) 1.1815(2) 0.0646(8) Uani 1 1 d . . . H2A H 1.4635 0.2826 1.1852 0.097 Uiso 1 1 d R . . H2B H 1.3140 0.1317 1.1744 0.097 Uiso 1 1 d R . . C1 C 0.4702(5) -0.1466(3) 0.5761(2) 0.0375(6) Uani 1 1 d . . . C6 C 0.7043(5) -0.0655(3) 0.5801(2) 0.0399(7) Uani 1 1 d . . . H6 H 0.8062 -0.1014 0.5306 0.048 Uiso 1 1 calc R . . C4 C 0.6412(5) 0.1260(3) 0.7322(2) 0.0382(6) Uani 1 1 d . . . C2 C 0.3226(5) -0.0936(3) 0.6510(2) 0.0438(7) Uani 1 1 d . . . H2 H 0.1659 -0.1485 0.6502 0.053 Uiso 1 1 calc R . . C5 C 0.7882(5) 0.0693(3) 0.6575(2) 0.0399(6) Uani 1 1 d . . . H5 H 0.9464 0.1228 0.6593 0.048 Uiso 1 1 calc R . . C8 C 0.8863(5) 0.2636(3) 0.9123(2) 0.0415(7) Uani 1 1 d . . . C7 C 0.7347(6) 0.2751(3) 0.8152(2) 0.0475(7) Uani 1 1 d . . . H7A H 0.8313 0.3444 0.7804 0.057 Uiso 1 1 calc R . . H7B H 0.5983 0.3152 0.8402 0.057 Uiso 1 1 calc R . . C12 C 1.2649(6) 0.3315(3) 1.0261(3) 0.0549(8) Uani 1 1 d . . . H12 H 1.4242 0.3868 1.0419 0.066 Uiso 1 1 calc R . . C9 C 0.7941(6) 0.1728(4) 0.9776(2) 0.0550(8) Uani 1 1 d . . . H9 H 0.6342 0.1183 0.9622 0.066 Uiso 1 1 calc R . . C10 C 0.9346(6) 0.1609(4) 1.0657(3) 0.0599(9) Uani 1 1 d . . . H10 H 0.8676 0.0998 1.1089 0.072 Uiso 1 1 calc R . . C11 C 1.1735(6) 0.2395(3) 1.0898(2) 0.0482(7) Uani 1 1 d . . . C13 C 1.1226(5) 0.3431(3) 0.9384(3) 0.0518(8) Uani 1 1 d . . . H13 H 1.1887 0.4061 0.8964 0.062 Uiso 1 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 Mn 0.0297(3) 0.0341(3) 0.0321(3) 0.0071(2) -0.0034(2) 0.0058(2) Cl 0.0482(5) 0.0767(6) 0.0566(5) 0.0316(4) 0.0187(4) 0.0214(4) N1 0.0490(14) 0.0375(13) 0.0432(14) 0.0108(11) -0.0087(11) 0.0100(11) C3 0.0414(16) 0.0531(18) 0.0403(16) 0.0122(14) 0.0086(13) 0.0148(13) N2 0.0746(19) 0.0707(19) 0.0442(16) 0.0044(13) -0.0115(14) 0.0235(15) C1 0.0412(15) 0.0356(15) 0.0372(15) 0.0143(12) -0.0062(12) 0.0091(12) C6 0.0414(16) 0.0438(16) 0.0379(15) 0.0128(13) 0.0068(13) 0.0145(13) C4 0.0396(15) 0.0408(15) 0.0349(15) 0.0118(12) -0.0028(12) 0.0099(12) C2 0.0333(15) 0.0471(17) 0.0512(18) 0.0177(14) 0.0023(13) 0.0045(13) C5 0.0338(14) 0.0418(16) 0.0450(16) 0.0164(13) 0.0015(13) 0.0054(12) C8 0.0514(17) 0.0344(15) 0.0345(15) 0.0024(12) 0.0030(13) 0.0092(13) C7 0.0566(18) 0.0398(16) 0.0433(17) 0.0075(13) -0.0004(14) 0.0103(14) C12 0.0464(18) 0.0522(19) 0.058(2) 0.0104(16) -0.0044(16) 0.0019(14) C9 0.0487(18) 0.060(2) 0.0496(19) 0.0160(16) -0.0009(15) -0.0024(15) C10 0.067(2) 0.067(2) 0.0441(19) 0.0222(16) 0.0028(17) 0.0043(17) C11 0.0557(19) 0.0487(17) 0.0365(16) 0.0000(13) -0.0019(14) 0.0178(15) C13 0.0507(19) 0.0491(18) 0.0540(19) 0.0172(15) 0.0029(15) 0.0042(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn O1W 2.1800(19) 2_646 ? Mn O1W 2.1800(19) . ? Mn N1 2.292(2) . ? Mn N1 2.292(2) 2_646 ? Mn Cl 2.5432(7) . ? Mn Cl 2.5432(7) 2_646 ? O1W H1W1 0.9601 . ? O1W H1W2 0.9752 . ? N1 C1 1.435(3) . ? N1 C7 5.752(4) . ? N1 N2 9.598(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C3 C4 1.383(4) . ? C3 C2 1.389(4) . ? C3 H3 0.9300 . ? N2 C11 1.416(4) . ? N2 H1W1 1.8572 1_666 ? N2 C7 5.741(4) . ? N2 H2A 0.8941 . ? N2 H2B 0.9064 . ? C1 C6 1.380(4) . ? C1 C2 1.377(4) . ? C6 C5 1.385(4) . ? C6 H6 0.9300 . ? C4 C5 1.385(4) . ? C4 C7 1.517(4) . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C8 C13 1.374(4) . ? C8 C9 1.381(4) . ? C8 C7 1.515(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C12 C11 1.372(4) . ? C12 C13 1.389(4) . ? C12 H12 0.9300 . ? C9 C10 1.389(4) . ? C9 H9 0.9300 . ? C10 C11 1.382(4) . ? C10 H10 0.9300 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Mn O1W 180.00(8) 2_646 . ? O1W Mn N1 94.36(8) 2_646 . ? O1W Mn N1 85.64(8) . . ? O1W Mn N1 85.64(8) 2_646 2_646 ? O1W Mn N1 94.36(8) . 2_646 ? N1 Mn N1 180.000(1) . 2_646 ? O1W Mn Cl 90.64(6) 2_646 . ? O1W Mn Cl 89.36(6) . . ? N1 Mn Cl 91.98(6) . . ? N1 Mn Cl 88.02(6) 2_646 . ? O1W Mn Cl 89.36(6) 2_646 2_646 ? O1W Mn Cl 90.64(6) . 2_646 ? N1 Mn Cl 88.02(6) . 2_646 ? N1 Mn Cl 91.98(6) 2_646 2_646 ? Cl Mn Cl 180.0 . 2_646 ? Mn O1W H1W1 108.5 . . ? Mn O1W H1W2 110.6 . . ? H1W1 O1W H1W2 109.1 . . ? C1 N1 Mn 123.27(16) . . ? C1 N1 C7 1.03(13) . . ? Mn N1 C7 123.86(8) . . ? C1 N1 N2 32.65(13) . . ? Mn N1 N2 90.74(6) . . ? C7 N1 N2 33.34(4) . . ? C1 N1 H1A 106.5 . . ? Mn N1 H1A 106.5 . . ? C7 N1 H1A 105.5 . . ? N2 N1 H1A 124.4 . . ? C1 N1 H1B 106.5 . . ? Mn N1 H1B 106.5 . . ? C7 N1 H1B 106.9 . . ? N2 N1 H1B 118.6 . . ? H1A N1 H1B 106.5 . . ? C4 C3 C2 121.6(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C11 N2 H1W1 110.5 . 1_666 ? C11 N2 C7 1.17(15) . . ? H1W1 N2 C7 109.5 1_666 . ? C11 N2 N1 32.96(16) . . ? H1W1 N2 N1 134.9 1_666 . ? C7 N2 N1 33.41(4) . . ? C11 N2 H2A 109.5 . . ? H1W1 N2 H2A 90.5 1_666 . ? C7 N2 H2A 110.2 . . ? N1 N2 H2A 121.3 . . ? C11 N2 H2B 108.9 . . ? H1W1 N2 H2B 125.9 1_666 . ? C7 N2 H2B 109.3 . . ? N1 N2 H2B 75.9 . . ? H2A N2 H2B 109.6 . . ? C6 C1 C2 119.3(2) . . ? C6 C1 N1 119.8(2) . . ? C2 C1 N1 120.9(2) . . ? C1 C6 C5 120.3(3) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C3 C4 C5 117.6(2) . . ? C3 C4 C7 121.8(3) . . ? C5 C4 C7 120.6(2) . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C5 C6 121.3(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C13 C8 C9 117.4(3) . . ? C13 C8 C7 120.9(3) . . ? C9 C8 C7 121.7(3) . . ? C8 C7 C4 112.8(2) . . ? C8 C7 N2 0.37(14) . . ? C4 C7 N2 112.53(16) . . ? C8 C7 N1 113.54(16) . . ? C4 C7 N1 0.98(13) . . ? N2 C7 N1 113.25(6) . . ? C8 C7 H7A 109.0 . . ? C4 C7 H7A 109.0 . . ? N2 C7 H7A 109.0 . . ? N1 C7 H7A 108.1 . . ? C8 C7 H7B 109.0 . . ? C4 C7 H7B 109.0 . . ? N2 C7 H7B 109.4 . . ? N1 C7 H7B 109.2 . . ? H7A C7 H7B 107.8 . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 118.3(3) . . ? C12 C11 N2 122.0(3) . . ? C10 C11 N2 119.6(3) . . ? C8 C13 C12 121.5(3) . . ? C8 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn N1 C7 N2 -7.41(13) . . . . ? N1 C7 N2 H1W1 -145.3 . . . 1_666 ? Mn N1 N2 H1W1 -136.9 . . . 1_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.632 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.052 data_6 _database_code_depnum_ccdc_archive 'CCDC 606688' _exptl_absorpt_correction_nazim 3 _diffrn_measurement_domega 1.1+0.35tg(theta) _diffrn_measurement_rtime 60 _chemical_formula_sum 'C26 H32 N6 Ni O8' _chemical_formula_weight 615.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.837(3) _cell_length_b 9.424(5) _cell_length_c 13.329(5) _cell_angle_alpha 105.58(4) _cell_angle_beta 98.08(4) _cell_angle_gamma 105.89(4) _cell_volume 660.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 12 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 322 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _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 CAD4 _diffrn_measurement_method omega-scan _diffrn_standards_number 3 _diffrn_standards_interval_time 2h _diffrn_standards_decay_% 3 _diffrn_reflns_number 2069 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 23.97 _reflns_number_total 2069 _reflns_number_observed 1581 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 2067 _refine_ls_number_parameters 193 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_obs 0.0405 _refine_ls_wR_factor_all 0.1122 _refine_ls_wR_factor_obs 0.1012 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.5000 0.5000 0.0310(2) Uani 1 2 d S . . N3 N 0.2229(5) 0.4527(3) 0.6704(2) 0.0393(7) Uani 1 1 d . . . O31 O 0.3582(5) 0.3877(4) 0.7022(2) 0.0600(8) Uani 1 1 d . . . O32 O 0.0971(6) 0.5069(4) 0.7268(2) 0.0616(8) Uani 1 1 d . . . O33 O 0.2076(5) 0.4671(3) 0.57881(19) 0.0466(7) Uani 1 1 d . . . O1W O 0.2404(4) 0.3703(3) 0.36210(17) 0.0370(6) Uani 1 1 d D . . H1W1 H 0.284(6) 0.320(4) 0.2998(17) 0.056 Uiso 1 1 d D . . H1W2 H 0.126(6) 0.408(4) 0.330(2) 0.056 Uiso 1 1 d D . . N1 N 0.4072(6) 0.6945(3) 0.4827(2) 0.0403(7) Uani 1 1 d . . . H1A H 0.4652 0.7157 0.4275 0.048 Uiso 1 1 calc RD . . H1B H 0.2429 0.6631 0.4621 0.048 Uiso 1 1 calc RD . . C3 C 0.3899(6) 1.0112(4) 0.7122(3) 0.0383(8) Uani 1 1 d . . . H3 H 0.2784 1.0327 0.7525 0.046 Uiso 1 1 calc R . . N2 N 1.3505(6) 1.2174(4) 1.1784(2) 0.0485(8) Uani 1 1 d . . . H2A H 1.5018 1.2713 1.1822 0.073 Uiso 1 1 d RD . . H2B H 1.3524 1.1204 1.1713 0.073 Uiso 1 1 d RD . . C1 C 0.4795(6) 0.8392(4) 0.5677(3) 0.0319(8) Uani 1 1 d . . . C6 C 0.7123(7) 0.9445(4) 0.5919(3) 0.0368(8) Uani 1 1 d . . . H6 H 0.8226 0.9233 0.5508 0.044 Uiso 1 1 calc R . . C4 C 0.6224(6) 1.1179(4) 0.7381(3) 0.0336(8) Uani 1 1 d . . . C2 C 0.3186(6) 0.8737(4) 0.6282(3) 0.0378(8) Uani 1 1 d . . . H2 H 0.1606 0.8040 0.6125 0.045 Uiso 1 1 calc R . . C5 C 0.7823(6) 1.0808(4) 0.6766(3) 0.0381(9) Uani 1 1 d . . . H5 H 0.9410 1.1495 0.6928 0.046 Uiso 1 1 calc R . . C8 C 0.8724(6) 1.2573(4) 0.9268(3) 0.0355(8) Uani 1 1 d . . . C7 C 0.7028(7) 1.2656(4) 0.8332(3) 0.0420(9) Uani 1 1 d . . . H7A H 0.5593 1.2839 0.8555 0.050 Uiso 1 1 calc R . . H7B H 0.7857 1.3531 0.8118 0.050 Uiso 1 1 calc R . . C12 C 1.2788(7) 1.3221(4) 1.0329(3) 0.0435(9) Uani 1 1 d . . . H12 H 1.4455 1.3762 1.0479 0.052 Uiso 1 1 calc R . . C9 C 0.7869(7) 1.1687(4) 0.9886(3) 0.0413(9) Uani 1 1 d . . . H9 H 0.6198 1.1166 0.9748 0.050 Uiso 1 1 calc R . . C10 C 0.9426(7) 1.1552(4) 1.0706(3) 0.0421(9) Uani 1 1 d . . . H10 H 0.8796 1.0950 1.1115 0.051 Uiso 1 1 calc R . . C11 C 1.1911(7) 1.2303(4) 1.0923(3) 0.0365(8) Uani 1 1 d . . . C13 C 1.1207(7) 1.3346(4) 0.9507(3) 0.0427(9) Uani 1 1 d . . . H13 H 1.1832 1.3966 0.9107 0.051 Uiso 1 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 Ni 0.0337(4) 0.0299(4) 0.0256(3) 0.0085(3) -0.0016(3) 0.0094(3) N3 0.0334(17) 0.0428(18) 0.0425(18) 0.0213(15) 0.0029(14) 0.0094(14) O31 0.0603(18) 0.084(2) 0.0646(19) 0.0486(17) 0.0196(15) 0.0420(17) O32 0.0638(19) 0.097(2) 0.0553(18) 0.0425(17) 0.0303(15) 0.0492(18) O33 0.0426(15) 0.0691(19) 0.0335(14) 0.0232(13) 0.0032(11) 0.0226(13) O1W 0.0375(14) 0.0392(14) 0.0279(12) 0.0075(10) -0.0038(10) 0.0113(11) N1 0.0477(18) 0.0362(16) 0.0325(16) 0.0102(13) -0.0045(13) 0.0143(14) C3 0.037(2) 0.045(2) 0.040(2) 0.0186(17) 0.0110(16) 0.0185(17) N2 0.058(2) 0.0496(19) 0.0349(17) 0.0086(15) -0.0005(15) 0.0233(16) C1 0.0377(19) 0.0290(17) 0.0295(17) 0.0124(14) 0.0003(14) 0.0126(15) C6 0.041(2) 0.040(2) 0.0363(19) 0.0168(16) 0.0121(16) 0.0164(17) C4 0.039(2) 0.0321(18) 0.0330(18) 0.0148(15) 0.0016(15) 0.0148(16) C2 0.0302(18) 0.0337(19) 0.046(2) 0.0159(17) 0.0013(16) 0.0053(15) C5 0.0300(18) 0.035(2) 0.045(2) 0.0182(17) 0.0023(16) 0.0028(15) C8 0.039(2) 0.0326(19) 0.0300(18) 0.0051(15) 0.0020(15) 0.0127(16) C7 0.049(2) 0.037(2) 0.039(2) 0.0115(16) 0.0046(17) 0.0169(17) C12 0.034(2) 0.044(2) 0.044(2) 0.0119(18) 0.0032(16) 0.0045(17) C9 0.038(2) 0.042(2) 0.040(2) 0.0128(17) 0.0092(16) 0.0095(17) C10 0.047(2) 0.046(2) 0.035(2) 0.0190(17) 0.0115(17) 0.0116(18) C11 0.046(2) 0.0353(19) 0.0260(17) 0.0024(15) 0.0036(15) 0.0194(17) C13 0.047(2) 0.039(2) 0.040(2) 0.0184(17) 0.0062(17) 0.0056(17) _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 Ni O1W 2.041(3) 2_666 ? Ni O1W 2.041(3) . ? Ni N1 2.107(3) . ? Ni N1 2.107(3) 2_666 ? Ni O33 2.121(3) 2_666 ? Ni O33 2.121(3) . ? N3 O31 1.220(4) . ? N3 O32 1.232(4) . ? N3 O33 1.258(4) . ? O1W H1W1 0.946(10) . ? O1W H1W2 0.943(10) . ? N1 C1 1.429(4) . ? N1 C7 5.737(6) . ? N1 N2 9.318(7) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C3 C2 1.379(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9300 . ? N2 C11 1.426(4) . ? N2 H1W1 1.800(11) 1_666 ? N2 C7 5.732(5) . ? N2 H2A 0.8763 . ? N2 H2B 0.8968 . ? C1 C2 1.371(5) . ? C1 C6 1.379(5) . ? C6 C5 1.377(5) . ? C6 H6 0.9300 . ? C4 C5 1.380(5) . ? C4 C7 1.514(5) . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C8 C9 1.371(5) . ? C8 C13 1.378(5) . ? C8 C7 1.514(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C12 C11 1.370(5) . ? C12 C13 1.382(5) . ? C12 H12 0.9300 . ? C9 C10 1.377(5) . ? C9 H9 0.9300 . ? C10 C11 1.378(5) . ? C10 H10 0.9300 . ? C13 H13 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Ni O1W 180.0 2_666 . ? O1W Ni N1 92.97(11) 2_666 . ? O1W Ni N1 87.03(11) . . ? O1W Ni N1 87.03(11) 2_666 2_666 ? O1W Ni N1 92.97(11) . 2_666 ? N1 Ni N1 180.00(15) . 2_666 ? O1W Ni O33 85.90(11) 2_666 2_666 ? O1W Ni O33 94.10(10) . 2_666 ? N1 Ni O33 95.30(12) . 2_666 ? N1 Ni O33 84.70(12) 2_666 2_666 ? O1W Ni O33 94.10(11) 2_666 . ? O1W Ni O33 85.90(11) . . ? N1 Ni O33 84.70(12) . . ? N1 Ni O33 95.30(12) 2_666 . ? O33 Ni O33 180.0 2_666 . ? O31 N3 O32 121.4(3) . . ? O31 N3 O33 121.0(3) . . ? O32 N3 O33 117.6(3) . . ? N3 O33 Ni 125.2(2) . . ? Ni O1W H1W1 121(2) . . ? Ni O1W H1W2 124(2) . . ? H1W1 O1W H1W2 98.5(12) . . ? C1 N1 Ni 122.7(2) . . ? C1 N1 C7 1.81(16) . . ? Ni N1 C7 121.04(10) . . ? C1 N1 N2 37.26(16) . . ? Ni N1 N2 85.65(9) . . ? C7 N1 N2 35.64(5) . . ? C1 N1 H1A 106.6 . . ? Ni N1 H1A 106.6 . . ? C7 N1 H1A 108.1 . . ? N2 N1 H1A 119.5 . . ? C1 N1 H1B 106.6 . . ? Ni N1 H1B 106.6 . . ? C7 N1 H1B 107.1 . . ? N2 N1 H1B 126.5 . . ? H1A N1 H1B 106.6 . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C11 N2 H1W1 106.5(10) . 1_666 ? C11 N2 C7 0.5(2) . . ? H1W1 N2 C7 106.3(10) 1_666 . ? C11 N2 N1 35.81(18) . . ? H1W1 N2 N1 132.8(11) 1_666 . ? C7 N2 N1 35.68(5) . . ? C11 N2 H2A 109.3 . . ? H1W1 N2 H2A 104.1 1_666 . ? C7 N2 H2A 109.8 . . ? N1 N2 H2A 114.2 . . ? C11 N2 H2B 114.7 . . ? H1W1 N2 H2B 116.6 1_666 . ? C7 N2 H2B 114.5 . . ? N1 N2 H2B 79.6 . . ? H2A N2 H2B 105.0 . . ? C2 C1 C6 118.9(3) . . ? C2 C1 N1 120.0(3) . . ? C6 C1 N1 121.0(3) . . ? C5 C6 C1 120.3(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C7 121.3(3) . . ? C3 C4 C7 121.5(3) . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C6 C5 C4 121.6(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C9 C8 C13 117.5(3) . . ? C9 C8 C7 121.5(3) . . ? C13 C8 C7 121.0(3) . . ? C4 C7 C8 112.3(3) . . ? C4 C7 N2 110.5(2) . . ? C8 C7 N2 1.85(16) . . ? C4 C7 N1 1.99(16) . . ? C8 C7 N1 110.4(2) . . ? N2 C7 N1 108.69(9) . . ? C4 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7A 110.5 . . ? N1 C7 H7A 109.5 . . ? C4 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? N2 C7 H7B 109.6 . . ? N1 C7 H7B 110.7 . . ? H7A C7 H7B 107.9 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 118.7(3) . . ? C12 C11 N2 121.2(3) . . ? C10 C11 N2 120.1(3) . . ? C8 C13 C12 121.5(3) . . ? C8 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni N1 C7 N2 7.47(17) . . . . ? N1 C7 N2 H1W1 -143.8(14) . . . 1_666 ? Ni N1 N2 H1W1 -123.0(17) . . . 1_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.490 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.071 data_7 _database_code_depnum_ccdc_archive 'CCDC 606689' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C13 H14 Cd Cl2 N2' _chemical_formula_weight 381.56 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Triclinc _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.678(2) _cell_length_b 12.213(3) _cell_length_c 13.691(3) _cell_angle_alpha 85.497(4) _cell_angle_beta 77.327(4) _cell_angle_gamma 82.580(4) _cell_volume 1402.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1342 _cell_measurement_theta_min 4. _cell_measurement_theta_max 22. _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 15569 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.74 _reflns_number_total 5914 _reflns_number_observed 5387 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.3744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5914 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_obs 0.0193 _refine_ls_wR_factor_all 0.0522 _refine_ls_wR_factor_obs 0.0509 _refine_ls_goodness_of_fit_all 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.861506(15) 0.115803(10) 0.065643(9) 0.03500(5) Uani 1 1 d . . . Cd2 Cd 0.908173(16) 0.399991(10) -0.055387(9) 0.03591(5) Uani 1 1 d . . . Cl1 Cl 1.09397(5) 0.23982(4) 0.01473(4) 0.04125(10) Uani 1 1 d . . . Cl2 Cl 1.03821(6) -0.04534(4) 0.12636(3) 0.03804(10) Uani 1 1 d . . . Cl3 Cl 0.66340(5) 0.28002(4) -0.00134(3) 0.03913(10) Uani 1 1 d . . . Cl4 Cl 0.86325(6) 0.48167(4) 0.12661(3) 0.03949(10) Uani 1 1 d . . . N1 N 0.7353(2) 0.20711(14) 0.21532(12) 0.0475(4) Uani 1 1 d . . . H1A H 0.7535 0.2783 0.2028 0.057 Uiso 1 1 calc R . . H1B H 0.6303 0.2063 0.2206 0.057 Uiso 1 1 calc R . . C1 C 0.7637(2) 0.17754(16) 0.31457(13) 0.0398(4) Uani 1 1 d . . . C2 C 0.7003(3) 0.08681(17) 0.36942(15) 0.0463(5) Uani 1 1 d . . . H2 H 0.6413 0.0441 0.3416 0.056 Uiso 1 1 calc R . . C3 C 0.7253(2) 0.06026(17) 0.46571(15) 0.0455(4) Uani 1 1 d . . . H3 H 0.6809 0.0002 0.5020 0.055 Uiso 1 1 calc R . . C4 C 0.8146(2) 0.12099(17) 0.50916(14) 0.0406(4) Uani 1 1 d . . . C5 C 0.8775(2) 0.21082(17) 0.45276(15) 0.0463(5) Uani 1 1 d . . . H5 H 0.9375 0.2532 0.4801 0.056 Uiso 1 1 calc R . . C6 C 0.8530(2) 0.23882(17) 0.35661(15) 0.0472(5) Uani 1 1 d . . . H6 H 0.8969 0.2991 0.3204 0.057 Uiso 1 1 calc R . . C9 C 0.5900(2) 0.14534(18) 0.73069(16) 0.0480(5) Uani 1 1 d . . . H9 H 0.5910 0.2158 0.6996 0.058 Uiso 1 1 calc R . . C10 C 0.4680(2) 0.12505(16) 0.81129(16) 0.0454(4) Uani 1 1 d . . . H10 H 0.3885 0.1817 0.8337 0.054 Uiso 1 1 calc R . . C11 C 0.4636(2) 0.02050(15) 0.85897(13) 0.0350(4) Uani 1 1 d . . . C12 C 0.5840(2) -0.06273(16) 0.82353(15) 0.0422(4) Uani 1 1 d . . . H12 H 0.5828 -0.1335 0.8540 0.051 Uiso 1 1 calc R . . N2 N 0.33743(18) -0.00242(14) 0.94211(12) 0.0406(3) Uani 1 1 d . . . H2A H 0.2860 0.0635 0.9620 0.049 Uiso 1 1 calc R . . H2B H 0.3841 -0.0320 0.9922 0.049 Uiso 1 1 calc R . . N3 N 0.9093(2) 0.32413(14) -0.21087(11) 0.0419(4) Uani 1 1 d . . . H3A H 0.8980 0.2519 -0.1979 0.050 Uiso 1 1 calc R . . H3B H 0.8215 0.3559 -0.2313 0.050 Uiso 1 1 calc R . . C14 C 1.0406(2) 0.33181(15) -0.29450(13) 0.0360(4) Uani 1 1 d . . . C15 C 1.1601(2) 0.24522(16) -0.31318(15) 0.0453(4) Uani 1 1 d . . . H15 H 1.1537 0.1804 -0.2727 0.054 Uiso 1 1 calc R . . C16 C 1.2891(2) 0.25422(16) -0.39159(15) 0.0444(4) Uani 1 1 d . . . H16 H 1.3681 0.1948 -0.4033 0.053 Uiso 1 1 calc R . . C17 C 1.3042(2) 0.34965(15) -0.45346(13) 0.0369(4) Uani 1 1 d . . . C18 C 1.1817(3) 0.43594(16) -0.43451(15) 0.0473(5) Uani 1 1 d . . . H18 H 1.1876 0.5005 -0.4753 0.057 Uiso 1 1 calc R . . C19 C 1.0518(2) 0.42777(16) -0.35645(15) 0.0465(5) Uani 1 1 d . . . H19 H 0.9716 0.4865 -0.3452 0.056 Uiso 1 1 calc R . . C20 C 1.4470(2) 0.35780(18) -0.53876(14) 0.0435(4) Uani 1 1 d . . . H20A H 1.5158 0.2885 -0.5405 0.052 Uiso 1 1 calc R . . H20B H 1.5062 0.4153 -0.5259 0.052 Uiso 1 1 calc R . . C22 C 1.4705(2) 0.46448(17) -0.70689(14) 0.0419(4) Uani 1 1 d . . . H22 H 1.5410 0.5060 -0.6882 0.050 Uiso 1 1 calc R . . N4 N 1.28533(19) 0.44667(14) -0.92529(12) 0.0410(3) Uani 1 1 d . . . H4A H 1.2494 0.3857 -0.9407 0.049 Uiso 1 1 calc R . . H4B H 1.3745 0.4568 -0.9713 0.049 Uiso 1 1 calc R . . C23 C 1.4335(2) 0.48518(17) -0.80099(14) 0.0431(4) Uani 1 1 d . . . H23 H 1.4791 0.5402 -0.8444 0.052 Uiso 1 1 calc R . . C24 C 1.3288(2) 0.42404(15) -0.83023(13) 0.0356(4) Uani 1 1 d . . . C25 C 1.2608(2) 0.34285(15) -0.76407(15) 0.0407(4) Uani 1 1 d . . . H25 H 1.1899 0.3016 -0.7826 0.049 Uiso 1 1 calc R . . C26 C 1.2984(2) 0.32330(15) -0.67047(14) 0.0415(4) Uani 1 1 d . . . H26 H 1.2518 0.2689 -0.6267 0.050 Uiso 1 1 calc R . . C13 C 0.7051(2) -0.04047(16) 0.74325(15) 0.0431(4) Uani 1 1 d . . . H13 H 0.7850 -0.0969 0.7210 0.052 Uiso 1 1 calc R . . C8 C 0.7111(2) 0.06323(17) 0.69502(13) 0.0398(4) Uani 1 1 d . . . C7 C 0.8518(2) 0.0880(2) 0.61169(15) 0.0515(5) Uani 1 1 d . . . H7A H 0.9007 0.1472 0.6318 0.062 Uiso 1 1 calc R . . H7B H 0.9297 0.0230 0.6052 0.062 Uiso 1 1 calc R . . C21 C 1.4043(2) 0.38307(15) -0.64040(13) 0.0368(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03731(8) 0.03449(8) 0.03145(8) -0.00182(5) -0.00277(5) -0.00529(5) Cd2 0.04260(8) 0.03645(8) 0.02887(7) -0.00094(5) -0.00598(5) -0.00844(5) Cl1 0.0388(2) 0.0328(2) 0.0531(3) -0.00361(19) -0.01012(19) -0.00599(17) Cl2 0.0461(2) 0.0377(2) 0.0300(2) -0.00003(17) -0.00862(17) -0.00369(17) Cl3 0.0364(2) 0.0404(2) 0.0388(2) 0.00199(18) -0.00456(18) -0.00569(17) Cl4 0.0435(2) 0.0458(2) 0.0282(2) -0.00403(17) 0.00034(17) -0.01386(18) N1 0.0543(10) 0.0518(10) 0.0306(8) -0.0041(7) -0.0031(7) 0.0062(8) C1 0.0421(10) 0.0438(10) 0.0280(9) -0.0054(7) 0.0016(7) 0.0025(8) C2 0.0548(12) 0.0502(11) 0.0373(10) -0.0057(8) -0.0113(9) -0.0136(9) C3 0.0530(11) 0.0477(11) 0.0366(10) 0.0030(8) -0.0071(8) -0.0161(9) C4 0.0339(9) 0.0560(11) 0.0299(9) -0.0044(8) -0.0010(7) -0.0067(8) C5 0.0430(10) 0.0558(12) 0.0414(11) -0.0080(9) -0.0028(8) -0.0176(9) C6 0.0476(11) 0.0485(11) 0.0408(11) -0.0003(8) 0.0037(9) -0.0122(9) C9 0.0456(11) 0.0498(11) 0.0454(11) 0.0106(9) -0.0083(9) -0.0045(9) C10 0.0405(10) 0.0438(10) 0.0475(11) -0.0029(8) -0.0044(8) 0.0034(8) C11 0.0345(9) 0.0433(9) 0.0294(9) -0.0047(7) -0.0081(7) -0.0083(7) C12 0.0431(10) 0.0376(9) 0.0447(11) -0.0021(8) -0.0070(8) -0.0042(8) N2 0.0383(8) 0.0490(9) 0.0344(8) -0.0055(7) -0.0044(6) -0.0081(7) N3 0.0448(9) 0.0479(9) 0.0312(8) -0.0068(7) -0.0006(7) -0.0090(7) C14 0.0398(9) 0.0421(9) 0.0255(8) -0.0063(7) -0.0040(7) -0.0053(7) C15 0.0517(11) 0.0409(10) 0.0396(10) 0.0054(8) -0.0068(8) -0.0008(8) C16 0.0430(10) 0.0437(10) 0.0414(11) -0.0004(8) -0.0062(8) 0.0077(8) C17 0.0384(9) 0.0430(10) 0.0270(8) -0.0037(7) -0.0042(7) 0.0004(7) C18 0.0556(12) 0.0395(10) 0.0380(10) 0.0047(8) 0.0009(9) 0.0050(9) C19 0.0515(11) 0.0414(10) 0.0372(10) -0.0031(8) 0.0018(8) 0.0107(8) C20 0.0371(10) 0.0564(12) 0.0339(10) -0.0026(8) -0.0035(8) -0.0004(8) C22 0.0363(9) 0.0530(11) 0.0371(10) -0.0043(8) -0.0039(8) -0.0128(8) N4 0.0394(8) 0.0488(9) 0.0336(8) -0.0052(7) -0.0058(6) -0.0022(7) C23 0.0387(10) 0.0532(11) 0.0365(10) 0.0021(8) -0.0028(8) -0.0135(8) C24 0.0326(9) 0.0397(9) 0.0314(9) -0.0068(7) -0.0023(7) 0.0020(7) C25 0.0420(10) 0.0384(9) 0.0429(10) -0.0079(8) -0.0080(8) -0.0070(8) C26 0.0458(10) 0.0390(10) 0.0379(10) -0.0005(8) -0.0035(8) -0.0081(8) C13 0.0375(10) 0.0469(11) 0.0443(11) -0.0123(8) -0.0064(8) -0.0005(8) C8 0.0342(9) 0.0583(11) 0.0287(9) -0.0022(8) -0.0097(7) -0.0070(8) C7 0.0370(10) 0.0825(15) 0.0358(10) 0.0014(10) -0.0077(8) -0.0125(10) C21 0.0332(9) 0.0415(9) 0.0314(9) -0.0060(7) -0.0002(7) 0.0022(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 Cd1 N2 2.3729(16) 2_656 ? Cd1 N1 2.3876(16) . ? Cd1 Cl2 2.5374(6) . ? Cd1 Cl1 2.6185(7) . ? Cd1 Cl3 2.7076(6) . ? Cd1 Cl2 2.7506(8) 2_755 ? Cd2 N3 2.3850(16) . ? Cd2 N4 2.3879(16) 2_764 ? Cd2 Cl4 2.5778(6) 2_765 ? Cd2 Cl1 2.6301(6) . ? Cd2 Cl3 2.6741(7) . ? Cd2 Cl4 2.6869(7) . ? Cl2 Cd1 2.7506(8) 2_755 ? Cl4 Cd2 2.5778(6) 2_765 ? N1 C1 1.444(2) . ? N1 C7 5.777(3) . ? N1 N2 10.035(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 C6 1.380(3) . ? C1 C2 1.393(3) . ? C2 C3 1.389(3) . ? C2 H2 0.9300 . ? C3 C4 1.388(3) . ? C3 H3 0.9300 . ? C4 C5 1.391(3) . ? C4 C7 1.521(3) . ? C5 C6 1.389(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C9 C10 1.383(3) . ? C9 C8 1.388(3) . ? C9 H9 0.9300 . ? C10 C11 1.389(3) . ? C10 H10 0.9300 . ? C11 C12 1.393(3) . ? C11 N2 1.433(2) . ? C12 C13 1.381(3) . ? C12 H12 0.9300 . ? N2 Cd1 2.3729(16) 2_656 ? N2 C7 5.765(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C14 1.434(2) . ? N3 C20 5.754(3) . ? N3 N4 9.670(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C14 C15 1.379(3) . ? C14 C19 1.393(3) . ? C15 C16 1.380(3) . ? C15 H15 0.9300 . ? C16 C17 1.389(3) . ? C16 H16 0.9300 . ? C17 C18 1.393(3) . ? C17 C20 1.512(2) . ? C18 C19 1.381(3) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.516(3) . ? C20 N4 5.754(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 C21 1.387(3) . ? C22 C23 1.392(3) . ? C22 H22 0.9300 . ? N4 C24 1.430(2) . ? N4 Cd2 2.3879(16) 2_764 ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C23 C24 1.387(3) . ? C23 H23 0.9300 . ? C24 C25 1.388(3) . ? C25 C26 1.386(3) . ? C25 H25 0.9300 . ? C26 C21 1.390(3) . ? C26 H26 0.9300 . ? C13 C8 1.383(3) . ? C13 H13 0.9300 . ? C8 C7 1.521(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N1 99.21(6) 2_656 . ? N2 Cd1 Cl2 92.57(5) 2_656 . ? N1 Cd1 Cl2 103.61(4) . . ? N2 Cd1 Cl1 162.47(4) 2_656 . ? N1 Cd1 Cl1 95.65(5) . . ? Cl2 Cd1 Cl1 92.93(2) . . ? N2 Cd1 Cl3 84.47(5) 2_656 . ? N1 Cd1 Cl3 77.51(4) . . ? Cl2 Cd1 Cl3 176.985(14) . . ? Cl1 Cd1 Cl3 89.73(2) . . ? N2 Cd1 Cl2 78.76(4) 2_656 2_755 ? N1 Cd1 Cl2 166.96(4) . 2_755 ? Cl2 Cd1 Cl2 89.376(19) . 2_755 ? Cl1 Cd1 Cl2 84.673(17) . 2_755 ? Cl3 Cd1 Cl2 89.466(19) . 2_755 ? N3 Cd2 N4 94.99(6) . 2_764 ? N3 Cd2 Cl4 95.39(4) . 2_765 ? N4 Cd2 Cl4 91.21(5) 2_764 2_765 ? N3 Cd2 Cl1 98.29(5) . . ? N4 Cd2 Cl1 165.35(4) 2_764 . ? Cl4 Cd2 Cl1 93.67(2) 2_765 . ? N3 Cd2 Cl3 79.17(4) . . ? N4 Cd2 Cl3 86.22(5) 2_764 . ? Cl4 Cd2 Cl3 173.740(15) 2_765 . ? Cl1 Cd2 Cl3 90.22(2) . . ? N3 Cd2 Cl4 171.94(4) . . ? N4 Cd2 Cl4 81.01(4) 2_764 . ? Cl4 Cd2 Cl4 91.693(17) 2_765 . ? Cl1 Cd2 Cl4 85.04(2) . . ? Cl3 Cd2 Cl4 93.533(17) . . ? Cd1 Cl1 Cd2 91.45(2) . . ? Cd1 Cl2 Cd1 90.624(19) . 2_755 ? Cd2 Cl3 Cd1 88.57(2) . . ? Cd2 Cl4 Cd2 88.307(17) 2_765 . ? C1 N1 Cd1 126.36(12) . . ? C1 N1 C7 0.25(10) . . ? Cd1 N1 C7 126.14(6) . . ? C1 N1 N2 29.36(10) . . ? Cd1 N1 N2 137.62(5) . . ? C7 N1 N2 29.58(3) . . ? C1 N1 H1A 105.7 . . ? Cd1 N1 H1A 105.7 . . ? C7 N1 H1A 105.7 . . ? N2 N1 H1A 114.4 . . ? C1 N1 H1B 105.7 . . ? Cd1 N1 H1B 105.7 . . ? C7 N1 H1B 106.0 . . ? N2 N1 H1B 76.4 . . ? H1A N1 H1B 106.2 . . ? C6 C1 C2 119.11(18) . . ? C6 C1 N1 120.67(18) . . ? C2 C1 N1 120.22(18) . . ? C3 C2 C1 119.90(19) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 121.74(18) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 117.32(18) . . ? C3 C4 C7 122.09(18) . . ? C5 C4 C7 120.50(18) . . ? C6 C5 C4 121.66(19) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C1 C6 C5 120.25(18) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C10 C9 C8 121.71(19) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 120.30(18) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 118.53(17) . . ? C10 C11 N2 121.14(17) . . ? C12 C11 N2 120.32(17) . . ? C13 C12 C11 120.19(18) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C11 N2 Cd1 123.71(11) . 2_656 ? C11 N2 C7 0.89(9) . . ? Cd1 N2 C7 124.30(5) 2_656 . ? C11 N2 N1 28.76(9) . . ? Cd1 N2 N1 101.85(4) 2_656 . ? C7 N2 N1 29.65(3) . . ? C11 N2 H2A 106.4 . . ? Cd1 N2 H2A 106.4 2_656 . ? C7 N2 H2A 106.6 . . ? N1 N2 H2A 98.7 . . ? C11 N2 H2B 106.4 . . ? Cd1 N2 H2B 106.4 2_656 . ? C7 N2 H2B 105.5 . . ? N1 N2 H2B 134.4 . . ? H2A N2 H2B 106.5 . . ? C14 N3 Cd2 120.94(12) . . ? C14 N3 C20 1.63(9) . . ? Cd2 N3 C20 119.38(5) . . ? C14 N3 N4 31.33(9) . . ? Cd2 N3 N4 141.28(5) . . ? C20 N3 N4 32.83(2) . . ? C14 N3 H3A 107.1 . . ? Cd2 N3 H3A 107.1 . . ? C20 N3 H3A 107.5 . . ? N4 N3 H3A 108.3 . . ? C14 N3 H3B 107.1 . . ? Cd2 N3 H3B 107.1 . . ? C20 N3 H3B 108.3 . . ? N4 N3 H3B 77.0 . . ? H3A N3 H3B 106.8 . . ? C15 C14 C19 118.94(17) . . ? C15 C14 N3 120.41(17) . . ? C19 C14 N3 120.62(17) . . ? C14 C15 C16 120.33(18) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 121.81(17) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C18 117.25(17) . . ? C16 C17 C20 120.89(16) . . ? C18 C17 C20 121.85(17) . . ? C19 C18 C17 121.46(18) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C14 120.20(17) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C17 C20 C21 113.63(16) . . ? C17 C20 N3 0.75(9) . . ? C21 C20 N3 114.36(11) . . ? C17 C20 N4 113.62(11) . . ? C21 C20 N4 0.86(9) . . ? N3 C20 N4 114.35(4) . . ? C17 C20 H20A 108.8 . . ? C21 C20 H20A 108.8 . . ? N3 C20 H20A 108.3 . . ? N4 C20 H20A 108.1 . . ? C17 C20 H20B 108.8 . . ? C21 C20 H20B 108.8 . . ? N3 C20 H20B 108.6 . . ? N4 C20 H20B 109.6 . . ? H20A C20 H20B 107.7 . . ? C21 C22 C23 121.19(18) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 N4 Cd2 118.86(11) . 2_764 ? C24 N4 C20 1.16(9) . . ? Cd2 N4 C20 117.97(5) 2_764 . ? C24 N4 N3 33.96(9) . . ? Cd2 N4 N3 95.77(4) 2_764 . ? C20 N4 N3 32.83(3) . . ? C24 N4 H4A 107.6 . . ? Cd2 N4 H4A 107.6 2_764 . ? C20 N4 H4A 107.5 . . ? N3 N4 H4A 94.1 . . ? C24 N4 H4B 107.6 . . ? Cd2 N4 H4B 107.6 2_764 . ? C20 N4 H4B 108.7 . . ? N3 N4 H4B 141.3 . . ? H4A N4 H4B 107.0 . . ? C24 C23 C22 120.26(18) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 119.10(17) . . ? C23 C24 N4 120.99(17) . . ? C25 C24 N4 119.86(17) . . ? C26 C25 C24 120.02(18) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 121.60(18) . . ? C25 C26 H26 119.2 . . ? C21 C26 H26 119.2 . . ? C12 C13 C8 121.92(18) . . ? C12 C13 H13 119.0 . . ? C8 C13 H13 119.0 . . ? C13 C8 C9 117.35(17) . . ? C13 C8 C7 120.97(18) . . ? C9 C8 C7 121.51(19) . . ? C4 C7 C8 116.04(16) . . ? C4 C7 N2 118.78(11) . . ? C8 C7 N2 2.92(9) . . ? C4 C7 N1 2.18(9) . . ? C8 C7 N1 118.00(11) . . ? N2 C7 N1 120.77(5) . . ? C4 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N2 C7 H7A 106.0 . . ? N1 C7 H7A 108.0 . . ? C4 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? N2 C7 H7B 107.6 . . ? N1 C7 H7B 106.4 . . ? H7A C7 H7B 107.4 . . ? C22 C21 C26 117.82(17) . . ? C22 C21 C20 121.65(17) . . ? C26 C21 C20 120.52(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd1 N1 C7 N2 -124.51(8) . . . . ? Cd1 N1 N2 Cd1 -61.81(9) . . . 2_656 ? Cd1 N3 C20 N4 145.69(4) . . . . ? N3 C20 N4 Cd1 -11.43(2) . . . 2_656 ? Cd1 N3 N4 Cd1 48.95(7) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.74 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.513 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.061 data_8 _database_code_depnum_ccdc_archive 'CCDC 606690' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C13 H14 Cl2 Mn N2' _chemical_formula_weight 324.10 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2160(13) _cell_length_b 8.7667(5) _cell_length_c 11.8792(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.216(2) _cell_angle_gamma 90.00 _cell_volume 2729.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2328 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _exptl_crystal_description rhombic _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.0 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 9485 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2981 _reflns_number_observed 2411 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.5947P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2981 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_obs 0.0284 _refine_ls_wR_factor_all 0.0817 _refine_ls_wR_factor_obs 0.0757 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.971565(9) 0.10800(3) 0.10926(2) 0.03548(10) Uani 1 1 d . . . Cl1 Cl 0.937134(16) -0.07755(5) -0.02766(4) 0.03929(13) Uani 1 1 d . . . Cl2 Cl 1.0000 0.31740(7) 0.2500 0.04108(16) Uani 1 2 d S . . Cl3 Cl 1.0000 -0.09275(7) 0.2500 0.04031(16) Uani 1 2 d S . . N1 N 0.89563(5) 0.16426(19) 0.19198(13) 0.0439(4) Uani 1 1 d . . . H1A H 0.9017 0.1599 0.2668 0.053 Uiso 1 1 calc R . . H1B H 0.8891 0.2627 0.1758 0.053 Uiso 1 1 calc R . . C1 C 0.84853(6) 0.0834(2) 0.17162(15) 0.0376(4) Uani 1 1 d . . . C2 C 0.83361(7) -0.0285(2) 0.24427(16) 0.0468(5) Uani 1 1 d . . . H2 H 0.8540 -0.0522 0.3068 0.056 Uiso 1 1 calc R . . C3 C 0.78853(8) -0.1063(2) 0.22544(17) 0.0477(5) Uani 1 1 d . . . H3 H 0.7790 -0.1819 0.2757 0.057 Uiso 1 1 calc R . . C4 C 0.75718(7) -0.0739(2) 0.13300(16) 0.0408(4) Uani 1 1 d . . . C5 C 0.77286(7) 0.0396(2) 0.06072(16) 0.0467(5) Uani 1 1 d . . . H5 H 0.7525 0.0640 -0.0017 0.056 Uiso 1 1 calc R . . C6 C 0.81824(7) 0.1178(2) 0.07897(17) 0.0458(5) Uani 1 1 d . . . H6 H 0.8282 0.1932 0.0289 0.055 Uiso 1 1 calc R . . C7 C 0.70841(7) -0.1627(2) 0.1122(2) 0.0513(5) Uani 1 1 d . . . H7A H 0.7016 -0.2233 0.1786 0.062 Uiso 1 1 calc R . . H7B H 0.7136 -0.2327 0.0502 0.062 Uiso 1 1 calc R . . C8 C 0.66188(7) -0.0662(2) 0.08523(16) 0.0400(4) Uani 1 1 d . . . C9 C 0.63344(7) -0.0866(2) -0.01267(17) 0.0435(4) Uani 1 1 d . . . H9 H 0.6437 -0.1592 -0.0646 0.052 Uiso 1 1 calc R . . C10 C 0.59012(7) -0.0014(2) -0.03527(15) 0.0421(4) Uani 1 1 d . . . H10 H 0.5718 -0.0162 -0.1023 0.051 Uiso 1 1 calc R . . C13 C 0.64535(7) 0.0431(2) 0.16057(16) 0.0445(4) Uani 1 1 d . . . H13 H 0.6641 0.0597 0.2268 0.053 Uiso 1 1 calc R . . C12 C 0.60185(7) 0.1277(2) 0.13984(16) 0.0425(4) Uani 1 1 d . . . H12 H 0.5914 0.1996 0.1921 0.051 Uiso 1 1 calc R . . C11 C 0.57377(7) 0.1058(2) 0.04126(15) 0.0368(4) Uani 1 1 d . . . N2 N 0.52961(6) 0.19685(18) 0.01805(13) 0.0420(4) Uani 1 1 d . . . H2A H 0.5203 0.2370 0.0842 0.050 Uiso 1 1 calc R . . H2B H 0.5046 0.1321 -0.0035 0.050 Uiso 1 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 Mn 0.03057(16) 0.04175(18) 0.03412(17) 0.00024(11) 0.00066(11) 0.00082(11) Cl1 0.0300(2) 0.0493(3) 0.0386(2) -0.00389(19) 0.00156(17) -0.00379(18) Cl2 0.0406(3) 0.0410(4) 0.0414(3) 0.000 -0.0058(3) 0.000 Cl3 0.0496(4) 0.0408(3) 0.0307(3) 0.000 0.0032(3) 0.000 N1 0.0326(8) 0.0534(10) 0.0458(9) -0.0056(7) 0.0033(6) -0.0012(7) C1 0.0282(8) 0.0451(10) 0.0397(10) -0.0041(8) 0.0050(7) 0.0027(7) C2 0.0408(10) 0.0539(12) 0.0454(10) 0.0074(9) -0.0046(8) 0.0039(9) C3 0.0453(11) 0.0465(11) 0.0514(12) 0.0141(9) 0.0057(9) 0.0019(9) C4 0.0301(9) 0.0400(10) 0.0526(11) 0.0037(8) 0.0051(8) 0.0025(7) C5 0.0358(10) 0.0587(13) 0.0452(10) 0.0120(9) -0.0049(8) -0.0035(9) C6 0.0380(10) 0.0522(12) 0.0473(11) 0.0130(9) 0.0027(8) -0.0058(8) C7 0.0375(10) 0.0415(11) 0.0750(15) 0.0037(10) 0.0030(9) -0.0012(8) C8 0.0313(9) 0.0371(9) 0.0516(11) 0.0025(8) 0.0054(8) -0.0048(7) C9 0.0417(10) 0.0400(10) 0.0492(11) -0.0062(8) 0.0091(8) -0.0014(8) C10 0.0405(10) 0.0472(11) 0.0386(9) -0.0026(8) 0.0000(8) -0.0048(8) C13 0.0403(10) 0.0500(11) 0.0429(10) -0.0022(9) -0.0054(8) -0.0007(9) C12 0.0438(10) 0.0436(11) 0.0403(10) -0.0060(8) 0.0033(8) 0.0023(8) C11 0.0324(9) 0.0382(10) 0.0401(10) 0.0043(7) 0.0048(7) -0.0033(7) N2 0.0394(8) 0.0446(9) 0.0421(8) 0.0033(7) 0.0033(6) 0.0010(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 Mn N2 2.2832(15) 7_655 ? Mn N1 2.2923(15) . ? Mn Cl1 2.4585(5) . ? Mn Cl3 2.5289(5) . ? Mn Cl2 2.5822(5) . ? Mn Cl1 2.6150(5) 5_755 ? Cl1 Mn 2.6150(5) 5_755 ? Cl2 Mn 2.5822(5) 2_755 ? Cl3 Mn 2.5289(5) 2_755 ? N1 C1 1.440(2) . ? N1 C7 5.745(2) . ? N1 N2 9.777(2) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 C2 1.369(3) . ? C1 C6 1.377(3) . ? C2 C3 1.379(3) . ? C2 H2 0.9300 . ? C3 C4 1.387(3) . ? C3 H3 0.9300 . ? C4 C5 1.382(3) . ? C4 C7 1.513(3) . ? C5 C6 1.387(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.513(3) . ? C7 N2 5.739(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.380(3) . ? C8 C13 1.387(3) . ? C9 C10 1.381(3) . ? C9 H9 0.9300 . ? C10 C11 1.382(3) . ? C10 H10 0.9300 . ? C13 C12 1.378(3) . ? C13 H13 0.9300 . ? C12 C11 1.383(3) . ? C12 H12 0.9300 . ? C11 N2 1.428(2) . ? N2 Mn 2.2832(15) 7_655 ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mn N1 97.07(6) 7_655 . ? N2 Mn Cl1 93.32(4) 7_655 . ? N1 Mn Cl1 96.66(4) . . ? N2 Mn Cl3 163.54(4) 7_655 . ? N1 Mn Cl3 96.48(4) . . ? Cl1 Mn Cl3 94.351(18) . . ? N2 Mn Cl2 84.02(4) 7_655 . ? N1 Mn Cl2 79.10(4) . . ? Cl1 Mn Cl2 174.643(16) . . ? Cl3 Mn Cl2 89.409(17) . . ? N2 Mn Cl1 80.24(4) 7_655 5_755 ? N1 Mn Cl1 172.26(4) . 5_755 ? Cl1 Mn Cl1 90.764(16) . 5_755 ? Cl3 Mn Cl1 85.108(13) . 5_755 ? Cl2 Mn Cl1 93.361(13) . 5_755 ? Mn Cl1 Mn 89.236(16) . 5_755 ? Mn Cl2 Mn 89.38(2) . 2_755 ? Mn Cl3 Mn 91.80(2) 2_755 . ? C1 N1 Mn 124.87(11) . . ? C1 N1 C7 0.47(10) . . ? Mn N1 C7 124.65(6) . . ? C1 N1 N2 31.17(9) . . ? Mn N1 N2 140.63(5) . . ? C7 N1 N2 31.63(2) . . ? C1 N1 H1A 106.1 . . ? Mn N1 H1A 106.1 . . ? C7 N1 H1A 105.9 . . ? N2 N1 H1A 111.2 . . ? C1 N1 H1B 106.1 . . ? Mn N1 H1B 106.1 . . ? C7 N1 H1B 106.6 . . ? N2 N1 H1B 75.2 . . ? H1A N1 H1B 106.3 . . ? C2 C1 C6 119.56(17) . . ? C2 C1 N1 120.14(16) . . ? C6 C1 N1 120.30(17) . . ? C1 C2 C3 120.50(17) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 121.24(18) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 117.40(17) . . ? C5 C4 C7 122.04(17) . . ? C3 C4 C7 120.55(18) . . ? C4 C5 C6 121.64(17) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 119.67(18) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C4 C7 C8 114.93(17) . . ? C4 C7 N2 115.66(12) . . ? C8 C7 N2 1.29(10) . . ? C4 C7 N1 1.05(9) . . ? C8 C7 N1 115.97(11) . . ? N2 C7 N1 116.71(4) . . ? C4 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N2 C7 H7A 107.2 . . ? N1 C7 H7A 108.0 . . ? C4 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? N2 C7 H7B 109.0 . . ? N1 C7 H7B 107.9 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C13 117.56(17) . . ? C9 C8 C7 121.67(18) . . ? C13 C8 C7 120.74(17) . . ? C8 C9 C10 121.43(17) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C11 C10 C9 120.34(17) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C13 C8 121.69(17) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C13 C12 C11 120.00(18) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C10 C11 C12 118.97(17) . . ? C10 C11 N2 120.96(16) . . ? C12 C11 N2 120.03(16) . . ? C11 N2 Mn 123.10(11) . 7_655 ? C11 N2 C7 0.66(9) . . ? Mn N2 C7 122.69(5) 7_655 . ? C11 N2 N1 32.32(9) . . ? Mn N2 N1 99.28(4) 7_655 . ? C7 N2 N1 31.66(2) . . ? C11 N2 H2A 106.6 . . ? Mn N2 H2A 106.6 7_655 . ? C7 N2 H2A 106.3 . . ? N1 N2 H2A 96.4 . . ? C11 N2 H2B 106.6 . . ? Mn N2 H2B 106.6 7_655 . ? C7 N2 H2B 107.2 . . ? N1 N2 H2B 138.4 . . ? H2A N2 H2B 106.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mn N1 C7 N2 -132.05(7) . . . . ? N1 C7 N2 Mn 47.50(8) . . . 7_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.254 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.052 data_9 _database_code_depnum_ccdc_archive 'CCDC 606691' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C13 H14 Cd Cl2 N2' _chemical_formula_weight 381.56 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' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4441(12) _cell_length_b 10.0237(19) _cell_length_c 12.366(2) _cell_angle_alpha 104.701(4) _cell_angle_beta 95.868(4) _cell_angle_gamma 94.544(4) _cell_volume 764.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3590 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 1.763 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 9035 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4385 _reflns_number_observed 3643 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.2636P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4385 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_obs 0.0331 _refine_ls_wR_factor_all 0.1017 _refine_ls_wR_factor_obs 0.0962 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.27301(3) 0.58291(2) 0.051204(18) 0.03278(9) Uani 1 1 d . . . Cl2 Cl 0.07217(12) 0.34952(8) 0.05611(7) 0.03855(17) Uani 1 1 d . . . Cl1 Cl 0.37753(12) 0.45823(9) -0.15117(6) 0.03872(17) Uani 1 1 d . . . N1 N 0.4438(4) 0.7825(3) 0.0112(2) 0.0378(6) Uani 1 1 d . . . H1A H 0.5754 0.7652 -0.0013 0.045 Uiso 1 1 calc R . . H1B H 0.3770 0.7921 -0.0534 0.045 Uiso 1 1 calc R . . C1 C 0.4560(5) 0.9115(3) 0.0938(3) 0.0365(6) Uani 1 1 d . . . C6 C 0.2796(6) 0.9810(4) 0.1078(3) 0.0423(7) Uani 1 1 d . . . H6 H 0.1546 0.9447 0.0613 0.051 Uiso 1 1 calc R . . C8 C 0.5795(9) 1.3004(4) 0.4641(3) 0.0653(13) Uani 1 1 d . . . C5 C 0.2880(7) 1.1038(4) 0.1904(3) 0.0525(9) Uani 1 1 d . . . H5 H 0.1672 1.1485 0.1988 0.063 Uiso 1 1 calc R . . C4 C 0.4695(8) 1.1624(4) 0.2607(3) 0.0568(10) Uani 1 1 d . . . C3 C 0.6422(8) 1.0929(5) 0.2455(3) 0.0614(11) Uani 1 1 d . . . H3 H 0.7666 1.1304 0.2921 0.074 Uiso 1 1 calc R . . C2 C 0.6410(6) 0.9684(4) 0.1632(3) 0.0478(8) Uani 1 1 d . . . H2 H 0.7623 0.9243 0.1552 0.057 Uiso 1 1 calc R . . C7 C 0.4776(11) 1.3009(5) 0.3488(3) 0.0863(18) Uani 1 1 d . . . H7A H 0.5544 1.3721 0.3235 0.104 Uiso 1 1 calc R . . H7B H 0.3357 1.3252 0.3546 0.104 Uiso 1 1 calc R . . C9 C 0.7494(9) 1.3913(5) 0.5182(4) 0.0727(14) Uani 1 1 d . . . H9 H 0.8030 1.4557 0.4829 0.087 Uiso 1 1 calc R . . C13 C 0.4996(10) 1.2105(6) 0.5196(4) 0.092(2) Uani 1 1 d . . . H13 H 0.3789 1.1508 0.4871 0.110 Uiso 1 1 calc R . . C10 C 0.8457(7) 1.3913(5) 0.6242(4) 0.0639(11) Uani 1 1 d . . . H10 H 0.9592 1.4565 0.6591 0.077 Uiso 1 1 calc R . . C12 C 0.5990(10) 1.2075(5) 0.6260(4) 0.0834(18) Uani 1 1 d . . . H12 H 0.5445 1.1441 0.6619 0.100 Uiso 1 1 calc R . . C11 C 0.7740(6) 1.2960(4) 0.6773(3) 0.0432(7) Uani 1 1 d . . . N2 N 0.8648(5) 1.2948(3) 0.7874(2) 0.0422(6) Uiso 1 1 d . . . H2A H 1.0012 1.3272 0.7947 0.051 Uiso 1 1 calc R . . H2B H 0.8603 1.2055 0.7893 0.051 Uiso 1 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 0.03007(12) 0.03530(13) 0.03298(13) 0.00915(9) 0.00347(8) 0.00384(8) Cl2 0.0327(3) 0.0394(4) 0.0476(4) 0.0204(3) 0.0011(3) 0.0045(3) Cl1 0.0328(3) 0.0514(4) 0.0308(4) 0.0089(3) 0.0013(3) 0.0078(3) N1 0.0426(14) 0.0358(13) 0.0359(14) 0.0100(11) 0.0075(11) 0.0045(11) C1 0.0457(17) 0.0355(15) 0.0318(15) 0.0152(12) 0.0065(13) 0.0029(13) C6 0.0476(18) 0.0417(17) 0.0406(17) 0.0158(14) 0.0041(14) 0.0089(14) C8 0.124(4) 0.0378(19) 0.0301(17) 0.0053(14) 0.002(2) 0.006(2) C5 0.075(3) 0.048(2) 0.0416(19) 0.0205(16) 0.0104(18) 0.0201(19) C4 0.099(3) 0.0422(19) 0.0302(17) 0.0124(15) 0.0046(19) 0.011(2) C3 0.078(3) 0.059(2) 0.039(2) 0.0122(18) -0.0153(19) -0.009(2) C2 0.0478(19) 0.051(2) 0.0432(19) 0.0125(16) -0.0010(15) 0.0028(16) C7 0.165(6) 0.051(2) 0.036(2) 0.0065(18) -0.010(3) 0.016(3) C9 0.110(4) 0.061(3) 0.051(2) 0.029(2) 0.013(2) -0.010(3) C13 0.126(5) 0.085(4) 0.048(3) 0.019(3) -0.021(3) -0.043(3) C10 0.071(3) 0.064(3) 0.057(2) 0.026(2) 0.003(2) -0.016(2) C12 0.127(5) 0.075(3) 0.040(2) 0.027(2) -0.014(2) -0.043(3) C11 0.056(2) 0.0415(17) 0.0318(16) 0.0063(13) 0.0131(14) 0.0042(15) _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 Cd N2 2.360(3) 2_676 ? Cd N1 2.392(3) . ? Cd Cl1 2.5703(8) 2_665 ? Cd Cl2 2.6000(9) . ? Cd Cl1 2.6776(9) . ? Cd Cl2 2.6943(8) 2_565 ? Cl2 Cd 2.6943(8) 2_565 ? Cl1 Cd 2.5703(8) 2_665 ? N1 C1 1.421(4) . ? N1 C7 5.754(5) . ? N1 N2 9.659(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 C6 1.383(5) . ? C1 C2 1.385(5) . ? C6 C5 1.379(5) . ? C6 H6 0.9300 . ? C8 C13 1.364(7) . ? C8 C9 1.364(7) . ? C8 C7 1.508(6) . ? C5 C4 1.376(6) . ? C5 H5 0.9300 . ? C4 C3 1.362(7) . ? C4 C7 1.526(6) . ? C3 C2 1.395(6) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C7 N2 5.750(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.393(6) . ? C9 H9 0.9300 . ? C13 C12 1.412(6) . ? C13 H13 0.9300 . ? C10 C11 1.366(5) . ? C10 H10 0.9300 . ? C12 C11 1.368(6) . ? C12 H12 0.9300 . ? C11 N2 1.429(4) . ? N2 Cd 2.360(3) 2_676 ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd N1 96.18(10) 2_676 . ? N2 Cd Cl1 97.66(7) 2_676 2_665 ? N1 Cd Cl1 89.84(7) . 2_665 ? N2 Cd Cl2 91.86(8) 2_676 . ? N1 Cd Cl2 169.84(7) . . ? Cl1 Cd Cl2 95.24(3) 2_665 . ? N2 Cd Cl1 170.51(7) 2_676 . ? N1 Cd Cl1 81.83(7) . . ? Cl1 Cd Cl1 91.63(3) 2_665 . ? Cl2 Cd Cl1 89.22(3) . . ? N2 Cd Cl2 82.56(7) 2_676 2_565 ? N1 Cd Cl2 84.20(7) . 2_565 ? Cl1 Cd Cl2 174.02(2) 2_665 2_565 ? Cl2 Cd Cl2 90.73(3) . 2_565 ? Cl1 Cd Cl2 88.00(3) . 2_565 ? Cd Cl2 Cd 89.27(3) . 2_565 ? Cd Cl1 Cd 88.37(3) 2_665 . ? C1 N1 Cd 117.66(19) . . ? C1 N1 C7 1.20(17) . . ? Cd N1 C7 116.58(10) . . ? C1 N1 N2 33.05(16) . . ? Cd N1 N2 96.13(7) . . ? C7 N1 N2 32.89(5) . . ? C1 N1 H1A 107.9 . . ? Cd N1 H1A 107.9 . . ? C7 N1 H1A 108.9 . . ? N2 N1 H1A 93.6 . . ? C1 N1 H1B 107.9 . . ? Cd N1 H1B 107.9 . . ? C7 N1 H1B 108.0 . . ? N2 N1 H1B 140.9 . . ? H1A N1 H1B 107.2 . . ? C6 C1 C2 118.8(3) . . ? C6 C1 N1 119.9(3) . . ? C2 C1 N1 121.3(3) . . ? C5 C6 C1 120.3(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C13 C8 C9 117.5(4) . . ? C13 C8 C7 120.6(5) . . ? C9 C8 C7 121.9(4) . . ? C4 C5 C6 122.0(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C3 C4 C5 116.9(4) . . ? C3 C4 C7 121.8(4) . . ? C5 C4 C7 121.2(4) . . ? C4 C3 C2 123.1(4) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C8 C7 C4 113.7(4) . . ? C8 C7 N2 0.4(2) . . ? C4 C7 N2 113.4(3) . . ? C8 C7 N1 114.6(3) . . ? C4 C7 N1 0.86(19) . . ? N2 C7 N1 114.21(9) . . ? C8 C7 H7A 108.8 . . ? C4 C7 H7A 108.8 . . ? N2 C7 H7A 109.1 . . ? N1 C7 H7A 108.2 . . ? C8 C7 H7B 108.8 . . ? C4 C7 H7B 108.8 . . ? N2 C7 H7B 108.9 . . ? N1 C7 H7B 108.5 . . ? H7A C7 H7B 107.7 . . ? C8 C9 C10 122.5(4) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C8 C13 C12 120.4(5) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C11 C12 C13 121.3(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C10 C11 C12 117.9(4) . . ? C10 C11 N2 122.0(3) . . ? C12 C11 N2 119.9(3) . . ? C11 N2 Cd 120.5(2) . 2_676 ? C11 N2 C7 1.54(18) . . ? Cd N2 C7 119.18(11) 2_676 . ? C11 N2 N1 32.37(17) . . ? Cd N2 N1 141.64(9) 2_676 . ? C7 N2 N1 32.91(5) . . ? C11 N2 H2A 107.2 . . ? Cd N2 H2A 107.2 2_676 . ? C7 N2 H2A 108.6 . . ? N1 N2 H2A 108.1 . . ? C11 N2 H2B 107.2 . . ? Cd N2 H2B 107.2 2_676 . ? C7 N2 H2B 107.2 . . ? N1 N2 H2B 76.2 . . ? H2A N2 H2B 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd N1 C7 N2 56.36(17) . . . . ? N1 C7 N2 Cd -142.19(12) . . . 2_676 ? Cd N1 N2 Cd -71.93(16) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.443 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.121 data_10 _database_code_depnum_ccdc_archive 'CCDC 606692' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C26 H28 Cd3 Cl6 N4' _chemical_formula_weight 946.42 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.884(2) _cell_length_b 8.1009(6) _cell_length_c 12.0897(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.4610(10) _cell_angle_gamma 90.00 _cell_volume 2983.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7425 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 2.682 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 15398 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.04 _reflns_number_total 3617 _reflns_number_observed 3505 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+5.4196P] 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_number_reflns 3617 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_obs 0.0309 _refine_ls_wR_factor_all 0.0965 _refine_ls_wR_factor_obs 0.0854 _refine_ls_goodness_of_fit_all 1.351 _refine_ls_restrained_S_all 1.351 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.052888(8) -0.13967(3) 0.49048(2) 0.01584(9) Uani 1 1 d . . . Cd2 Cd 0.0000 -0.13521(4) 0.7500 0.01700(10) Uani 1 2 d S . . Cl1 Cl -0.02882(2) -0.10135(11) 0.37850(6) 0.01661(17) Uani 1 1 d . . . Cl2 Cl 0.07801(3) 0.08152(11) 0.36743(7) 0.01924(17) Uani 1 1 d . . . Cl3 Cl 0.02402(3) -0.35835(10) 0.62309(6) 0.01836(19) Uani 1 1 d . . . N1 N 0.11775(9) -0.2006(4) 0.6149(3) 0.0207(6) Uani 1 1 d . . . H1A H 0.1106 -0.1988 0.6842 0.025 Uiso 1 1 calc R . . H1B H 0.1244 -0.3060 0.6014 0.025 Uiso 1 1 calc R . . C1 C 0.15797(11) -0.1095(4) 0.6221(3) 0.0184(7) Uani 1 1 d . . . C4 C 0.23656(11) 0.0665(4) 0.6368(3) 0.0194(7) Uani 1 1 d . . . C6 C 0.18604(12) -0.1379(4) 0.5447(3) 0.0221(7) Uani 1 1 d . . . H5 H 0.1787 -0.2152 0.4878 0.027 Uiso 1 1 calc R . . C3 C 0.20819(12) 0.0930(4) 0.7125(3) 0.0209(7) Uani 1 1 d . . . H3 H 0.2155 0.1709 0.7690 0.025 Uiso 1 1 calc R . . C2 C 0.16913(11) 0.0062(4) 0.7062(3) 0.0196(7) Uani 1 1 d . . . H2 H 0.1506 0.0256 0.7581 0.024 Uiso 1 1 calc R . . C5 C 0.22490(11) -0.0497(4) 0.5534(3) 0.0210(7) Uani 1 1 d . . . H6 H 0.2436 -0.0692 0.5019 0.025 Uiso 1 1 calc R . . C7 C 0.27748(12) 0.1727(4) 0.6439(4) 0.0253(8) Uani 1 1 d . . . H7A H 0.2727 0.2528 0.5835 0.030 Uiso 1 1 calc R . . H7B H 0.2812 0.2335 0.7139 0.030 Uiso 1 1 calc R . . C8 C 0.31968(11) 0.0812(4) 0.6374(3) 0.0205(7) Uani 1 1 d . . . C9 C 0.33621(11) -0.0320(4) 0.7204(3) 0.0198(7) Uani 1 1 d . . . H9 H 0.3199 -0.0573 0.7763 0.024 Uiso 1 1 calc R . . C13 C 0.34453(12) 0.1155(4) 0.5549(3) 0.0223(7) Uani 1 1 d . . . H13 H 0.3339 0.1897 0.4982 0.027 Uiso 1 1 calc R . . C10 C 0.37660(11) -0.1075(4) 0.7212(3) 0.0190(7) Uani 1 1 d . . . H10 H 0.3870 -0.1836 0.7769 0.023 Uiso 1 1 calc R . . C12 C 0.38499(12) 0.0417(4) 0.5549(3) 0.0204(7) Uani 1 1 d . . . H12 H 0.4011 0.0666 0.4986 0.024 Uiso 1 1 calc R . . C11 C 0.40141(11) -0.0690(4) 0.6385(3) 0.0168(6) Uani 1 1 d . . . N2 N 0.44314(10) -0.1464(4) 0.6387(3) 0.0198(6) Uani 1 1 d . . . H2A H 0.4523 -0.1869 0.7079 0.024 Uiso 1 1 calc R . . H2B H 0.4624 -0.0676 0.6265 0.024 Uiso 1 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 Cd1 0.01392(14) 0.01843(15) 0.01525(14) 0.00077(8) 0.00262(9) 0.00127(8) Cd2 0.01783(19) 0.01898(19) 0.01473(18) 0.000 0.00427(13) 0.000 Cl1 0.0156(4) 0.0183(4) 0.0157(4) -0.0008(3) 0.0020(3) -0.0005(3) Cl2 0.0167(4) 0.0236(4) 0.0173(4) 0.0019(3) 0.0023(3) -0.0039(3) Cl3 0.0209(4) 0.0174(4) 0.0178(4) -0.0022(3) 0.0063(3) -0.0023(3) N1 0.0164(14) 0.0221(15) 0.0224(15) 0.0049(12) 0.0000(11) -0.0022(11) C1 0.0127(15) 0.0183(16) 0.0226(17) 0.0053(13) -0.0021(12) 0.0017(12) C4 0.0123(15) 0.0130(15) 0.0316(19) -0.0006(13) -0.0003(13) 0.0031(12) C6 0.0188(17) 0.0233(18) 0.0239(18) -0.0069(13) 0.0024(14) -0.0038(13) C3 0.0230(17) 0.0145(15) 0.0241(17) -0.0043(13) 0.0005(14) 0.0018(13) C2 0.0184(16) 0.0213(16) 0.0199(16) -0.0001(13) 0.0052(13) 0.0054(13) C5 0.0179(16) 0.0222(17) 0.0244(17) -0.0035(14) 0.0078(13) -0.0007(13) C7 0.0165(16) 0.0164(16) 0.042(2) -0.0042(15) 0.0022(15) -0.0030(13) C8 0.0153(16) 0.0196(16) 0.0258(18) -0.0047(13) 0.0007(13) -0.0043(13) C9 0.0178(16) 0.0209(16) 0.0222(17) -0.0027(13) 0.0075(13) -0.0040(13) C13 0.0250(18) 0.0158(15) 0.0240(18) 0.0025(13) -0.0024(14) -0.0007(13) C10 0.0206(17) 0.0175(15) 0.0184(16) 0.0026(12) 0.0019(13) -0.0010(13) C12 0.0238(17) 0.0187(16) 0.0194(16) 0.0001(13) 0.0056(13) -0.0033(13) C11 0.0159(15) 0.0151(15) 0.0186(15) -0.0040(12) 0.0003(12) -0.0044(12) N2 0.0170(14) 0.0231(15) 0.0200(14) 0.0002(11) 0.0047(11) -0.0016(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 Cd1 N2 2.350(3) 7_546 ? Cd1 N1 2.351(3) . ? Cd1 Cl2 2.5309(8) . ? Cd1 Cl3 2.6407(8) . ? Cd1 Cl1 2.6785(8) . ? Cd1 Cl1 2.6946(9) 5_556 ? Cd1 Cd2 3.7680(3) . ? Cd1 Cd2 3.8102(4) 5_556 ? Cd2 Cl3 2.5586(8) . ? Cd2 Cl3 2.5586(8) 2_556 ? Cd2 Cl2 2.6240(8) 6_556 ? Cd2 Cl2 2.6240(8) 5_556 ? Cd2 Cl1 2.7079(9) 5_556 ? Cd2 Cl1 2.7079(9) 6_556 ? Cd2 Cd1 3.7680(3) 2_556 ? Cd2 Cd1 3.8102(4) 6_556 ? Cd2 Cd1 3.8102(4) 5_556 ? Cl1 Cd1 2.6946(9) 5_556 ? Cl1 Cd2 2.7079(9) 5_556 ? Cl2 Cd2 2.6240(8) 5_556 ? N1 C1 1.435(4) . ? N1 C7 5.747(5) . ? N1 N2 10.016(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 C2 1.384(5) . ? C1 C6 1.395(5) . ? C4 C3 1.384(5) . ? C4 C5 1.384(5) . ? C4 C7 1.519(5) . ? C6 C5 1.386(5) . ? C6 H5 0.9300 . ? C3 C2 1.387(5) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C5 H6 0.9300 . ? C7 C8 1.512(5) . ? C7 N2 5.742(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.383(5) . ? C8 C9 1.393(5) . ? C9 C10 1.388(5) . ? C9 H9 0.9300 . ? C13 C12 1.385(5) . ? C13 H13 0.9300 . ? C10 C11 1.392(5) . ? C10 H10 0.9300 . ? C12 C11 1.383(5) . ? C12 H12 0.9300 . ? C11 N2 1.433(4) . ? N2 Cd1 2.350(3) 7_546 ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N1 97.97(11) 7_546 . ? N2 Cd1 Cl2 94.41(8) 7_546 . ? N1 Cd1 Cl2 102.32(7) . . ? N2 Cd1 Cl3 88.20(8) 7_546 . ? N1 Cd1 Cl3 78.92(7) . . ? Cl2 Cd1 Cl3 176.91(3) . . ? N2 Cd1 Cl1 84.11(8) 7_546 . ? N1 Cd1 Cl1 168.66(8) . . ? Cl2 Cd1 Cl1 88.58(3) . . ? Cl3 Cd1 Cl1 90.03(3) . . ? N2 Cd1 Cl1 167.11(8) 7_546 5_556 ? N1 Cd1 Cl1 93.67(8) . 5_556 ? Cl2 Cd1 Cl1 88.47(3) . 5_556 ? Cl3 Cd1 Cl1 88.62(3) . 5_556 ? Cl1 Cd1 Cl1 83.41(3) . 5_556 ? N2 Cd1 Cd2 129.62(7) 7_546 . ? N1 Cd1 Cd2 84.80(8) . . ? Cl2 Cd1 Cd2 134.38(2) . . ? Cl3 Cd1 Cd2 42.700(18) . . ? Cl1 Cd1 Cd2 85.319(18) . . ? Cl1 Cd1 Cd2 45.923(18) 5_556 . ? N2 Cd1 Cd2 89.23(7) 7_546 5_556 ? N1 Cd1 Cd2 145.50(7) . 5_556 ? Cl2 Cd1 Cd2 43.292(19) . 5_556 ? Cl3 Cd1 Cd2 135.247(19) . 5_556 ? Cl1 Cd1 Cd2 45.292(18) . 5_556 ? Cl1 Cd1 Cd2 84.261(18) 5_556 5_556 ? Cd2 Cd1 Cd2 116.079(7) . 5_556 ? Cl3 Cd2 Cl3 90.09(4) . 2_556 ? Cl3 Cd2 Cl2 96.35(3) . 6_556 ? Cl3 Cd2 Cl2 97.10(3) 2_556 6_556 ? Cl3 Cd2 Cl2 97.10(3) . 5_556 ? Cl3 Cd2 Cl2 96.35(3) 2_556 5_556 ? Cl2 Cd2 Cl2 160.92(4) 6_556 5_556 ? Cl3 Cd2 Cl1 90.05(3) . 5_556 ? Cl3 Cd2 Cl1 177.54(2) 2_556 5_556 ? Cl2 Cd2 Cl1 80.44(3) 6_556 5_556 ? Cl2 Cd2 Cl1 86.07(2) 5_556 5_556 ? Cl3 Cd2 Cl1 177.54(2) . 6_556 ? Cl3 Cd2 Cl1 90.05(3) 2_556 6_556 ? Cl2 Cd2 Cl1 86.07(2) 6_556 6_556 ? Cl2 Cd2 Cl1 80.44(3) 5_556 6_556 ? Cl1 Cd2 Cl1 89.91(4) 5_556 6_556 ? Cl3 Cd2 Cd1 44.422(18) . . ? Cl3 Cd2 Cd1 134.48(2) 2_556 . ? Cl2 Cd2 Cd1 88.105(19) 6_556 . ? Cl2 Cd2 Cd1 92.077(19) 5_556 . ? Cl1 Cd2 Cd1 45.631(18) 5_556 . ? Cl1 Cd2 Cd1 135.47(2) 6_556 . ? Cl3 Cd2 Cd1 134.48(2) . 2_556 ? Cl3 Cd2 Cd1 44.422(18) 2_556 2_556 ? Cl2 Cd2 Cd1 92.077(19) 6_556 2_556 ? Cl2 Cd2 Cd1 88.105(19) 5_556 2_556 ? Cl1 Cd2 Cd1 135.47(2) 5_556 2_556 ? Cl1 Cd2 Cd1 45.631(18) 6_556 2_556 ? Cd1 Cd2 Cd1 178.900(12) . 2_556 ? Cl3 Cd2 Cd1 137.756(18) . 6_556 ? Cl3 Cd2 Cd1 94.906(19) 2_556 6_556 ? Cl2 Cd2 Cd1 41.407(18) 6_556 6_556 ? Cl2 Cd2 Cd1 123.80(2) 5_556 6_556 ? Cl1 Cd2 Cd1 83.341(18) 5_556 6_556 ? Cl1 Cd2 Cd1 44.667(17) 6_556 6_556 ? Cd1 Cd2 Cd1 116.797(8) . 6_556 ? Cd1 Cd2 Cd1 63.921(7) 2_556 6_556 ? Cl3 Cd2 Cd1 94.906(19) . 5_556 ? Cl3 Cd2 Cd1 137.756(18) 2_556 5_556 ? Cl2 Cd2 Cd1 123.80(2) 6_556 5_556 ? Cl2 Cd2 Cd1 41.407(18) 5_556 5_556 ? Cl1 Cd2 Cd1 44.667(17) 5_556 5_556 ? Cl1 Cd2 Cd1 83.341(18) 6_556 5_556 ? Cd1 Cd2 Cd1 63.921(7) . 5_556 ? Cd1 Cd2 Cd1 116.797(8) 2_556 5_556 ? Cd1 Cd2 Cd1 108.476(12) 6_556 5_556 ? Cd1 Cl1 Cd1 96.59(3) . 5_556 ? Cd1 Cl1 Cd2 90.04(2) . 5_556 ? Cd1 Cl1 Cd2 88.45(3) 5_556 5_556 ? Cd1 Cl2 Cd2 95.30(3) . 5_556 ? Cd2 Cl3 Cd1 92.88(3) . . ? C1 N1 Cd1 124.6(2) . . ? C1 N1 C7 0.81(17) . . ? Cd1 N1 C7 124.12(10) . . ? C1 N1 N2 28.51(18) . . ? Cd1 N1 N2 138.97(9) . . ? C7 N1 N2 29.32(4) . . ? C1 N1 H1A 106.2 . . ? Cd1 N1 H1A 106.2 . . ? C7 N1 H1A 105.9 . . ? N2 N1 H1A 111.8 . . ? C1 N1 H1B 106.2 . . ? Cd1 N1 H1B 106.2 . . ? C7 N1 H1B 107.0 . . ? N2 N1 H1B 77.8 . . ? H1A N1 H1B 106.4 . . ? C2 C1 C6 119.8(3) . . ? C2 C1 N1 120.0(3) . . ? C6 C1 N1 120.1(3) . . ? C3 C4 C5 118.1(3) . . ? C3 C4 C7 119.1(3) . . ? C5 C4 C7 122.7(3) . . ? C5 C6 C1 119.3(3) . . ? C5 C6 H5 120.3 . . ? C1 C6 H5 120.3 . . ? C4 C3 C2 121.6(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H6 119.2 . . ? C6 C5 H6 119.2 . . ? C8 C7 C4 115.8(3) . . ? C8 C7 N2 3.50(17) . . ? C4 C7 N2 118.6(2) . . ? C8 C7 N1 118.5(2) . . ? C4 C7 N1 2.73(16) . . ? N2 C7 N1 121.33(8) . . ? C8 C7 H7A 108.3 . . ? C4 C7 H7A 108.3 . . ? N2 C7 H7A 108.6 . . ? N1 C7 H7A 106.5 . . ? C8 C7 H7B 108.3 . . ? C4 C7 H7B 108.3 . . ? N2 C7 H7B 105.1 . . ? N1 C7 H7B 107.3 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 118.1(3) . . ? C13 C8 C7 121.6(3) . . ? C9 C8 C7 120.1(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C8 C13 C12 121.4(3) . . ? C8 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C11 C10 119.4(3) . . ? C12 C11 N2 120.4(3) . . ? C10 C11 N2 120.1(3) . . ? C11 N2 Cd1 117.8(2) . 7_546 ? C11 N2 C7 1.09(16) . . ? Cd1 N2 C7 118.90(10) 7_546 . ? C11 N2 N1 28.49(16) . . ? Cd1 N2 N1 96.34(8) 7_546 . ? C7 N2 N1 29.35(4) . . ? C11 N2 H2A 107.9 . . ? Cd1 N2 H2A 107.9 7_546 . ? C7 N2 H2A 107.4 . . ? N1 N2 H2A 99.9 . . ? C11 N2 H2B 107.9 . . ? Cd1 N2 H2B 107.9 7_546 . ? C7 N2 H2B 107.2 . . ? N1 N2 H2B 135.4 . . ? H2A N2 H2B 107.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cd1 N1 C7 N2 -130.87(13) . . . . ? N1 C7 N2 Cd1 43.59(15) . . . 7_546 ? Cd1 N1 N2 Cd1 -70.12(16) . . . 7_546 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.787 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.274 data_11 _database_code_depnum_ccdc_archive 'CCDC 606693' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C39 H30 Ag N7 O3' _chemical_formula_weight 752.57 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 18.0645(5) _cell_length_b 18.0645(5) _cell_length_c 19.0889(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5394.6(3) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4828 _cell_measurement_theta_min 4. _cell_measurement_theta_max 26. _exptl_crystal_description rhombic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0. _diffrn_reflns_number 16961 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0106 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.04 _reflns_number_total 1319 _reflns_number_observed 1086 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Topos _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+4.3435P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1319 _refine_ls_number_parameters 85 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_obs 0.0391 _refine_ls_wR_factor_all 0.1388 _refine_ls_wR_factor_obs 0.1288 _refine_ls_goodness_of_fit_all 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.0000 0.0000 0.5000 0.0667(3) Uani 1 6 d S . . N2 N 0.0000 0.0000 0.7500 0.0557(12) Uani 1 6 d SD . . C6 C 0.2621(2) 0.1110(2) 0.52921(15) 0.0673(7) Uani 1 1 d . . . H6 H 0.2542 0.0705 0.4956 0.081 Uiso 1 1 calc R . . N1 N 0.12138(15) 0.01278(14) 0.57724(12) 0.0697(6) Uani 1 1 d . . . C1 C 0.19887(19) 0.09253(15) 0.57834(14) 0.0568(6) Uani 1 1 d . . . C4 C 0.35135(16) 0.25123(16) 0.57888(13) 0.0609(6) Uani 1 1 d . . . C2 C 0.21196(16) 0.15463(16) 0.62718(12) 0.0587(6) Uani 1 1 d . . . H2 H 0.1698 0.1440 0.6601 0.070 Uiso 1 1 calc R . . C3 C 0.28691(17) 0.23191(16) 0.62727(13) 0.0616(6) Uani 1 1 d . . . H3 H 0.2946 0.2725 0.6608 0.074 Uiso 1 1 calc R . . C5 C 0.3367(2) 0.1891(2) 0.52972(15) 0.0687(7) Uani 1 1 d . . . H5 H 0.3782 0.2003 0.4961 0.082 Uiso 1 1 calc R . . C7 C 0.4364(2) 0.3333 0.5833 0.0753(10) Uani 1 2 d S . . H7A H 0.4699 0.3366 0.5425 0.090 Uiso 0.50 1 calc PR . . H7B H 0.4666 0.3300 0.6242 0.090 Uiso 0.50 1 calc PR . . O1 O 0.0000 0.0000 0.8119(5) 0.163(6) Uani 0.75 3 d SPD . . O2 O -0.0708(8) -0.0358(10) 0.7275(10) 0.145(7) Uani 0.25 1 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 Ag 0.0638(3) 0.0638(3) 0.0725(4) 0.000 0.000 0.03190(14) N2 0.061(2) 0.061(2) 0.044(3) 0.000 0.000 0.0307(10) C6 0.0728(17) 0.0746(16) 0.0651(15) -0.0141(12) -0.0047(12) 0.0448(14) N1 0.0663(13) 0.0573(12) 0.0823(15) -0.0038(10) -0.0145(10) 0.0284(10) C1 0.0615(15) 0.0576(13) 0.0582(13) -0.0023(10) -0.0099(11) 0.0350(11) C4 0.0594(13) 0.0599(13) 0.0696(14) 0.0064(10) 0.0001(11) 0.0345(11) C2 0.0635(13) 0.0595(13) 0.0572(13) 0.0015(10) 0.0042(10) 0.0337(11) C3 0.0703(14) 0.0586(13) 0.0624(13) -0.0047(10) -0.0021(11) 0.0371(12) C5 0.0674(16) 0.0799(17) 0.0672(15) -0.0016(13) 0.0085(12) 0.0431(15) C7 0.0590(14) 0.066(2) 0.103(3) 0.006(2) 0.0030(10) 0.0329(11) O1 0.207(10) 0.207(10) 0.074(5) 0.000 0.000 0.104(5) O2 0.103(12) 0.206(16) 0.131(14) -0.074(10) -0.044(10) 0.081(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.555(2) 19_556 ? Ag N1 2.555(2) 2 ? Ag N1 2.555(2) 20_556 ? Ag N1 2.555(2) . ? Ag N1 2.555(2) 21_556 ? Ag N1 2.555(2) 3 ? N2 O1 1.182(9) 4_556 ? N2 O1 1.182(9) . ? N2 O2 1.188(10) 4_556 ? N2 O2 1.188(11) . ? N2 O2 1.188(11) 6_556 ? N2 O2 1.188(11) 3 ? N2 O2 1.188(11) 5_556 ? N2 O2 1.188(10) 2 ? C6 C5 1.381(5) . ? C6 C1 1.383(4) . ? N1 C1 1.421(4) . ? N1 C7 5.743(3) . ? N1 N1 10.032(4) 16 ? C1 C2 1.385(3) . ? C4 C5 1.383(4) . ? C4 C3 1.387(4) . ? C4 C7 1.513(3) . ? C2 C3 1.376(4) . ? C7 C4 1.513(3) 16 ? C7 N1 5.743(3) 16 ? O1 O2 1.34(2) 4_556 ? O1 O2 1.34(2) 6_556 ? O1 O2 1.34(2) 5_556 ? O2 O1 1.34(2) 4_556 ? O2 O2 1.39(3) 6_556 ? O2 O2 1.41(3) 4_556 ? 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 N1 Ag N1 89.97(8) 19_556 2 ? N1 Ag N1 90.03(8) 19_556 20_556 ? N1 Ag N1 180.0 2 20_556 ? N1 Ag N1 180.0 19_556 . ? N1 Ag N1 90.03(8) 2 . ? N1 Ag N1 89.97(8) 20_556 . ? N1 Ag N1 90.03(8) 19_556 21_556 ? N1 Ag N1 89.97(8) 2 21_556 ? N1 Ag N1 90.03(8) 20_556 21_556 ? N1 Ag N1 89.97(8) . 21_556 ? N1 Ag N1 89.97(8) 19_556 3 ? N1 Ag N1 90.03(8) 2 3 ? N1 Ag N1 89.97(8) 20_556 3 ? N1 Ag N1 90.03(8) . 3 ? N1 Ag N1 180.00(11) 21_556 3 ? O1 N2 O1 180.000(2) 4_556 . ? O1 N2 O2 111.2(10) 4_556 4_556 ? O1 N2 O2 68.8(10) . 4_556 ? O1 N2 O2 68.8(10) 4_556 . ? O1 N2 O2 111.2(10) . . ? O2 N2 O2 72.9(13) 4_556 . ? O1 N2 O2 111.2(10) 4_556 6_556 ? O1 N2 O2 68.8(10) . 6_556 ? O2 N2 O2 107.7(11) 4_556 6_556 ? O2 N2 O2 71.7(18) . 6_556 ? O1 N2 O2 68.8(10) 4_556 3 ? O1 N2 O2 111.2(10) . 3 ? O2 N2 O2 71.7(18) 4_556 3 ? O2 N2 O2 107.7(11) . 3 ? O2 N2 O2 179.3(14) 6_556 3 ? O1 N2 O2 111.2(10) 4_556 5_556 ? O1 N2 O2 68.8(10) . 5_556 ? O2 N2 O2 107.7(11) 4_556 5_556 ? O2 N2 O2 179.3(14) . 5_556 ? O2 N2 O2 107.7(11) 6_556 5_556 ? O2 N2 O2 72.9(13) 3 5_556 ? O1 N2 O2 68.8(10) 4_556 2 ? O1 N2 O2 111.2(10) . 2 ? O2 N2 O2 179.3(15) 4_556 2 ? O2 N2 O2 107.7(11) . 2 ? O2 N2 O2 72.9(13) 6_556 2 ? O2 N2 O2 107.7(11) 3 2 ? O2 N2 O2 71.7(18) 5_556 2 ? C5 C6 C1 120.5(3) . . ? C1 N1 Ag 117.78(15) . . ? C1 N1 C7 0.64(13) . . ? Ag N1 C7 118.41(7) . . ? C1 N1 N1 28.57(13) . 16 ? Ag N1 N1 95.26(5) . 16 ? C7 N1 N1 29.13(4) . 16 ? C6 C1 C2 118.4(3) . . ? C6 C1 N1 120.7(2) . . ? C2 C1 N1 120.9(3) . . ? C5 C4 C3 116.9(2) . . ? C5 C4 C7 121.5(2) . . ? C3 C4 C7 121.5(2) . . ? C3 C2 C1 120.4(2) . . ? C2 C3 C4 122.1(2) . . ? C6 C5 C4 121.8(3) . . ? C4 C7 C4 116.6(3) . 16 ? C4 C7 N1 3.33(12) . . ? C4 C7 N1 119.12(19) 16 . ? C4 C7 N1 119.12(18) . 16 ? C4 C7 N1 3.33(12) 16 16 ? N1 C7 N1 121.74(8) . 16 ? N2 O1 O2 55.8(6) . 4_556 ? N2 O1 O2 55.8(6) . 6_556 ? O2 O1 O2 91.5(8) 4_556 6_556 ? N2 O1 O2 55.8(6) . 5_556 ? O2 O1 O2 91.5(8) 4_556 5_556 ? O2 O1 O2 91.5(8) 6_556 5_556 ? N2 O2 O1 55.4(6) . 4_556 ? N2 O2 O2 54.1(9) . 6_556 ? O1 O2 O2 91.4(9) 4_556 6_556 ? N2 O2 O2 53.6(7) . 4_556 ? O1 O2 O2 90.6(12) 4_556 4_556 ? O2 O2 O2 86(2) 6_556 4_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag N1 C7 N1 40.83(7) . . . 16 ? N1 C7 N1 Ag 40.83(7) . . 16 16 ? Ag N1 N1 Ag 70.55(11) . . 16 16 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.514 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.064 # * END