# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex01 _database_code_depnum_ccdc_archive 'CCDC 903001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H87 Cd3 Cl9 N24 O36' _chemical_formula_weight 2088.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' '-x, -x+y, -z' 'x-y, -y, -z' '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' 'y+2/3, x+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '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' 'y+1/3, x+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' 'x, x-y, z' '-x+y, y, z' '-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' '-y+2/3, -x+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' '-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' '-y+1/3, -x+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' _cell_length_a 20.073(4) _cell_length_b 20.073(4) _cell_length_c 15.195(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5302(3) _cell_formula_units_Z 3 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 1.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7386 _exptl_absorpt_correction_T_max 0.8137 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21633 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.87 _reflns_number_total 1530 _reflns_number_gt 1254 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1242P)^2^+38.0637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1530 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2214 _refine_ls_wR_factor_gt 0.2116 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.26092(11) 0.3333 -0.1667 0.1045(12) Uani 1 2 d S . . Cd1 Cd 0.20749(3) 0.41499(7) -0.18555(6) 0.0487(4) Uani 0.50 2 d SP . . Cl2 Cl 0.21103(12) 0.4221(2) -0.3504(2) 0.0701(12) Uani 0.50 2 d SP . . O1W O 0.3195(5) 0.5242(4) -0.1836(3) 0.161(4) Uani 1 1 d . . . C1 C 0.22252(17) 0.4450(3) 0.0452(3) 0.0354(12) Uani 1 2 d S . . C2 C 0.2274(2) 0.3771(2) 0.1674(2) 0.0310(8) Uani 1 1 d . . . H2 H 0.2192 0.3244 0.1628 0.037 Uiso 1 1 calc R . . C3 C 0.21586(16) 0.4317(3) 0.2991(3) 0.0327(11) Uani 1 2 d S . . C4 C 0.3344(2) 0.4242(2) 0.2821(2) 0.0339(8) Uani 1 1 d . . . H4A H 0.3373 0.3778 0.2698 0.041 Uiso 1 1 calc R . . H4B H 0.3372 0.4315 0.3460 0.041 Uiso 1 1 calc R . . N1 N 0.26666(19) 0.4230(2) 0.0913(2) 0.0341(7) Uani 1 1 d . . . N2 N 0.26107(19) 0.4123(2) 0.2515(2) 0.0347(7) Uani 1 1 d . . . O1 O 0.23866(17) 0.4773(3) -0.0259(3) 0.0547(13) Uani 1 2 d S . . O2 O 0.22972(15) 0.4594(3) 0.3733(3) 0.0462(11) 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 Cl1 0.0657(9) 0.134(2) 0.137(2) -0.085(2) -0.0427(10) 0.0668(12) Cd1 0.0518(5) 0.0720(7) 0.0290(5) -0.0080(4) -0.0040(2) 0.0360(4) Cl2 0.109(3) 0.063(2) 0.0229(14) -0.0062(13) -0.0031(7) 0.0317(11) O1W 0.239(9) 0.100(4) 0.037(2) 0.014(2) 0.026(3) 0.004(5) C1 0.040(2) 0.040(3) 0.027(2) 0.002(2) 0.0011(11) 0.0198(14) C2 0.0363(19) 0.0282(17) 0.0268(17) -0.0016(13) -0.0014(14) 0.0149(15) C3 0.039(2) 0.033(3) 0.024(2) 0.0016(19) 0.0008(10) 0.0163(13) C4 0.038(2) 0.039(2) 0.0238(16) 0.0064(14) 0.0007(14) 0.0185(17) N1 0.0367(17) 0.0419(18) 0.0262(15) 0.0035(13) 0.0018(12) 0.0215(15) N2 0.0377(17) 0.0426(18) 0.0240(14) 0.0007(13) -0.0003(12) 0.0201(15) O1 0.057(2) 0.078(3) 0.036(2) 0.022(2) 0.0110(11) 0.0392(17) O2 0.0514(18) 0.067(3) 0.0254(18) -0.0086(19) -0.0043(9) 0.0335(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 Cl1 Cd1 2.3825(19) 31_554 ? Cl1 Cd1 2.3826(19) . ? Cd1 O1W 2.220(7) . ? Cd1 O1W 2.220(7) 24 ? Cd1 Cl1 2.3825(19) 31_554 ? Cd1 Cl2 2.507(3) . ? Cd1 Cd1 2.896(2) 31_554 ? C1 O1 1.217(7) . ? C1 N1 1.366(4) 24 ? C1 N1 1.366(4) . ? C2 N1 1.442(5) . ? C2 N2 1.453(5) . ? C2 C2 1.557(8) 24 ? C2 H2 0.9900 . ? C3 O2 1.226(7) . ? C3 N2 1.360(4) . ? C3 N2 1.360(4) 24 ? C4 N2 1.445(5) . ? C4 N1 1.449(5) 11 ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? N1 C4 1.449(5) 11 ? 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 Cd1 Cl1 Cd1 74.87(8) 31_554 . ? O1W Cd1 O1W 62.5(5) . 24 ? O1W Cd1 Cl1 156.9(2) . 31_554 ? O1W Cd1 Cl1 95.5(3) 24 31_554 ? O1W Cd1 Cl1 95.5(3) . . ? O1W Cd1 Cl1 156.9(2) 24 . ? Cl1 Cd1 Cl1 105.13(8) 31_554 . ? O1W Cd1 Cl2 88.36(14) . . ? O1W Cd1 Cl2 88.36(14) 24 . ? Cl1 Cd1 Cl2 98.60(6) 31_554 . ? Cl1 Cd1 Cl2 98.60(6) . . ? O1W Cd1 Cd1 146.6(2) . 31_554 ? O1W Cd1 Cd1 146.7(2) 24 31_554 ? Cl1 Cd1 Cd1 52.57(4) 31_554 31_554 ? Cl1 Cd1 Cd1 52.57(4) . 31_554 ? Cl2 Cd1 Cd1 104.24(10) . 31_554 ? O1 C1 N1 125.8(2) . 24 ? O1 C1 N1 125.8(2) . . ? N1 C1 N1 108.4(5) 24 . ? N1 C2 N2 114.9(3) . . ? N1 C2 C2 103.2(2) . 24 ? N2 C2 C2 102.9(2) . 24 ? N1 C2 H2 111.7 . . ? N2 C2 H2 111.7 . . ? C2 C2 H2 111.7 24 . ? O2 C3 N2 125.9(2) . . ? O2 C3 N2 125.9(2) . 24 ? N2 C3 N2 108.2(5) . 24 ? N2 C4 N1 113.8(3) . 11 ? N2 C4 H4A 108.8 . . ? N1 C4 H4A 108.8 11 . ? N2 C4 H4B 108.8 . . ? N1 C4 H4B 108.8 11 . ? H4A C4 H4B 107.7 . . ? C1 N1 C2 112.4(3) . . ? C1 N1 C4 121.3(3) . 11 ? C2 N1 C4 123.0(3) . 11 ? C3 N2 C4 123.5(3) . . ? C3 N2 C2 113.0(3) . . ? C4 N2 C2 123.5(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.264 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.125 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.060 206 83 ' ' 2 0.333 0.667 0.047 205 83 ' ' 3 0.667 0.333 -0.051 205 83 ' ' _platon_squeeze_details ; ; data_complex02 _database_code_depnum_ccdc_archive 'CCDC 903002' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H90 Cd3 Cl6 N24 O39' _chemical_formula_weight 2033.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.60(3) _cell_length_b 12.647(14) _cell_length_c 12.733(13) _cell_angle_alpha 106.08(3) _cell_angle_beta 105.57(5) _cell_angle_gamma 104.49(5) _cell_volume 1759(4) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7807 _exptl_absorpt_correction_T_max 0.8358 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15544 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5828 _reflns_number_gt 4036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5828 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.1062 _refine_ls_wR_factor_ref 0.3672 _refine_ls_wR_factor_gt 0.3150 _refine_ls_goodness_of_fit_ref 1.429 _refine_ls_restrained_S_all 1.429 _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 O1W O 0.3587(5) -0.6419(5) 0.7266(4) 0.0535(17) Uani 1 1 d . . . O2W O 1.6409(4) 0.2730(4) 1.6410(5) 0.0512(18) Uani 1 1 d . . . O3W O 0.7264(4) -0.6420(4) 0.3590(5) 0.0510(18) Uani 1 1 d . . . O4W O 0.7949(7) -0.3536(8) 0.5197(10) 0.122(4) Uani 1 1 d . . . O5W O 0.7945(7) -0.4865(11) 0.6451(9) 0.131(5) Uani 1 1 d . . . O6W O 1.3509(8) 0.2023(8) 1.4835(11) 0.124(5) Uani 1 1 d . . . O7W O 0.6477(8) -0.4827(11) 0.7967(8) 0.128(5) Uani 1 1 d . . . O8W O 1.4852(11) 0.2041(8) 1.3533(9) 0.133(5) Uani 1 1 d . . . O9W O 0.5191(11) -0.3540(10) 0.7975(8) 0.133(5) Uani 1 1 d . . . Cl1 Cl 0.4057(3) -0.4058(3) 0.9993(5) 0.1065(15) Uani 1 1 d . . . Cl2 Cl 1.5941(3) -0.0014(5) 1.4051(3) 0.1098(15) Uani 1 1 d . . . Cl3 Cl 1.0026(5) -0.5929(3) 0.5942(3) 0.1107(15) Uani 1 1 d . . . Cd1 Cd 0.52088(10) -0.47903(10) 0.89806(12) 0.0542(5) Uani 0.50 1 d P . . Cd2 Cd 1.47919(10) 0.10180(12) 1.47893(11) 0.0555(5) Uani 0.50 1 d P . . Cd3 Cd 0.89833(11) -0.47909(11) 0.52094(11) 0.0556(5) Uani 0.50 1 d P . . C1 C 1.1014(6) -0.2329(6) 0.7671(7) 0.040(2) Uani 1 1 d . . . C2 C 1.2909(6) -0.1045(6) 0.8161(7) 0.041(2) Uani 1 1 d . . . H2 H 1.3389 -0.1174 0.7669 0.049 Uiso 1 1 calc R . . C3 C 1.2901(6) -0.1836(6) 0.8957(6) 0.0357(18) Uani 1 1 d . . . H3 H 1.3379 -0.2339 0.8836 0.043 Uiso 1 1 calc R . . C4 C 1.3669(6) 0.0156(6) 1.0146(7) 0.043(2) Uani 1 1 d . . . C5 C 1.1280(6) -0.3558(6) 0.8827(7) 0.043(2) Uani 1 1 d . . . H5A H 1.1907 -0.3892 0.8927 0.051 Uiso 1 1 calc R . . H5B H 1.0597 -0.4137 0.8146 0.051 Uiso 1 1 calc R . . C6 C 1.3580(6) -0.1274(7) 1.1156(7) 0.044(2) Uani 1 1 d . . . H6A H 1.4160 -0.0587 1.1833 0.052 Uiso 1 1 calc R . . H6B H 1.3918 -0.1897 1.1049 0.052 Uiso 1 1 calc R . . C7 C 0.9852(6) -0.3664(6) 0.9856(6) 0.039(2) Uani 1 1 d . . . C8 C 1.1820(6) -0.2901(6) 1.1062(6) 0.040(2) Uani 1 1 d . . . H8 H 1.2317 -0.3385 1.1176 0.048 Uiso 1 1 calc R . . C9 C 1.1040(6) -0.2914(6) 1.1839(7) 0.047(2) Uani 1 1 d . . . H9 H 1.1169 -0.3395 1.2324 0.056 Uiso 1 1 calc R . . C10 C 1.2333(7) -0.0993(6) 1.2321(7) 0.047(2) Uani 1 1 d . . . C11 C 0.8843(6) -0.3565(6) 1.1254(7) 0.042(2) Uani 1 1 d . . . H11A H 0.8933 -0.3921 1.1851 0.050 Uiso 1 1 calc R . . H11B H 0.8171 -0.4129 1.0554 0.050 Uiso 1 1 calc R . . C12 C 1.1156(6) -0.1284(6) 1.3574(6) 0.041(2) Uani 1 1 d . . . H12A H 1.1032 -0.1915 1.3883 0.050 Uiso 1 1 calc R . . H12B H 1.1834 -0.0611 1.4170 0.050 Uiso 1 1 calc R . . C13 C 0.7670(6) -0.2334(6) 1.0999(6) 0.040(2) Uani 1 1 d . . . C14 C 0.8955(5) -0.1829(6) 1.2912(6) 0.0322(16) Uani 1 1 d . . . H14 H 0.8848 -0.2311 1.3396 0.039 Uiso 1 1 calc R . . C15 C 0.8166(6) -0.1048(6) 1.2902(7) 0.040(2) Uani 1 1 d . . . H15 H 0.7669 -0.1158 1.3375 0.049 Uiso 1 1 calc R . . C16 C 1.0154(5) 0.0153(6) 1.3660(6) 0.0338(17) Uani 1 1 d . . . C17 C 1.3576(6) 0.1168(7) 0.8726(7) 0.044(2) Uani 1 1 d . . . H17A H 1.4152 0.1848 0.9413 0.053 Uiso 1 1 calc R . . H17B H 1.3912 0.1054 0.8110 0.053 Uiso 1 1 calc R . . C18 C 1.1284(7) -0.1151(7) 0.6417(6) 0.043(2) Uani 1 1 d . . . H18A H 1.1915 -0.1045 0.6102 0.052 Uiso 1 1 calc R . . H18B H 1.0603 -0.1824 0.5824 0.052 Uiso 1 1 calc R . . N1 N 1.1679(5) -0.1419(6) 0.7484(5) 0.0434(18) Uani 1 1 d . . . N2 N 1.1670(5) -0.2521(5) 0.8583(6) 0.0436(18) Uani 1 1 d . . . N3 N 1.3379(5) 0.0128(5) 0.9040(6) 0.0434(18) Uani 1 1 d . . . N4 N 1.3388(5) -0.0968(5) 1.0134(5) 0.0421(17) Uani 1 1 d . . . N5 N 1.0963(5) -0.3380(5) 0.9853(5) 0.0412(17) Uani 1 1 d . . . N6 N 0.9860(5) -0.3386(5) 1.0969(5) 0.0411(17) Uani 1 1 d . . . N7 N 1.2530(5) -0.1670(5) 1.1419(6) 0.0454(19) Uani 1 1 d . . . N8 N 1.1417(5) -0.1678(5) 1.2534(5) 0.0402(16) Uani 1 1 d . . . N9 N 0.8577(5) -0.2532(5) 1.1681(5) 0.0442(19) Uani 1 1 d . . . N10 N 0.7481(5) -0.1415(5) 1.1680(5) 0.0382(16) Uani 1 1 d . . . N11 N 1.0149(5) -0.0951(5) 1.3377(5) 0.0389(16) Uani 1 1 d . . . N12 N 0.9028(5) 0.0136(5) 1.3383(6) 0.0423(18) Uani 1 1 d . . . O1 O 0.9955(5) -0.2897(5) 0.7109(5) 0.0573(18) Uani 1 1 d . . . O2 O 0.8957(5) -0.4154(5) 0.8966(5) 0.0531(17) Uani 1 1 d . . . O3 O 0.7108(5) -0.2894(5) 0.9977(5) 0.061(2) Uani 1 1 d . . . O4 O 1.4132(5) 0.1034(4) 1.1042(5) 0.0475(15) Uani 1 1 d . . . O5 O 1.2895(5) 0.0046(5) 1.2899(6) 0.0614(19) Uani 1 1 d . . . O6 O 1.1042(5) 0.1041(5) 1.4152(6) 0.0570(19) 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 O1W 0.046(3) 0.039(3) 0.021(2) -0.012(2) -0.014(2) -0.021(2) O2W 0.042(3) 0.025(2) 0.036(3) -0.009(2) -0.033(2) 0.0040(19) O3W 0.027(2) 0.041(3) 0.035(3) -0.034(2) -0.006(2) 0.0036(19) O4W 0.062(4) 0.089(6) 0.148(9) -0.009(6) -0.003(5) 0.023(4) O5W 0.061(4) 0.175(11) 0.082(6) -0.008(7) 0.006(4) 0.002(5) O6W 0.079(5) 0.062(5) 0.166(10) -0.006(6) 0.003(6) 0.020(4) O7W 0.082(5) 0.171(10) 0.056(5) -0.006(6) 0.007(4) -0.006(6) O8W 0.169(10) 0.072(6) 0.082(7) 0.006(5) -0.001(7) -0.002(6) O9W 0.161(10) 0.102(7) 0.066(6) 0.007(5) -0.002(6) 0.006(7) Cl1 0.0673(15) 0.0667(16) 0.209(5) 0.060(2) 0.060(2) 0.0410(13) Cl2 0.0662(15) 0.218(5) 0.0660(18) 0.053(2) 0.0314(14) 0.075(2) Cl3 0.215(4) 0.0688(18) 0.0713(19) 0.0285(15) 0.059(2) 0.076(2) Cd1 0.0422(7) 0.0394(7) 0.0558(8) -0.0016(6) 0.0005(6) 0.0133(5) Cd2 0.0417(7) 0.0578(8) 0.0407(7) -0.0032(6) 0.0006(5) 0.0140(6) Cd3 0.0611(8) 0.0394(7) 0.0407(8) -0.0006(6) -0.0008(6) 0.0138(6) C1 0.033(3) 0.027(3) 0.044(4) 0.002(3) 0.003(3) 0.008(3) C2 0.033(3) 0.039(4) 0.036(4) -0.004(3) 0.005(3) 0.017(3) C3 0.036(3) 0.030(3) 0.034(4) -0.003(3) 0.010(3) 0.020(3) C4 0.035(3) 0.030(4) 0.044(4) -0.003(3) -0.003(3) 0.015(3) C5 0.044(4) 0.029(3) 0.038(4) -0.006(3) 0.003(3) 0.017(3) C6 0.030(3) 0.042(4) 0.039(4) -0.001(3) -0.003(3) 0.015(3) C7 0.034(3) 0.034(3) 0.038(4) -0.001(3) 0.005(3) 0.019(3) C8 0.040(3) 0.031(3) 0.033(4) 0.000(3) -0.007(3) 0.019(3) C9 0.034(3) 0.035(4) 0.047(4) -0.008(3) -0.007(3) 0.021(3) C10 0.046(4) 0.028(3) 0.038(4) -0.008(3) -0.009(3) 0.014(3) C11 0.041(4) 0.029(3) 0.041(4) 0.000(3) 0.004(3) 0.016(3) C12 0.041(3) 0.036(3) 0.028(3) -0.005(3) -0.001(3) 0.016(3) C13 0.031(3) 0.038(4) 0.028(4) -0.007(3) -0.001(3) 0.008(3) C14 0.029(3) 0.025(3) 0.031(4) 0.004(3) 0.007(3) 0.003(2) C15 0.036(3) 0.032(3) 0.033(4) -0.002(3) -0.001(3) 0.010(3) C16 0.030(3) 0.037(4) 0.026(3) 0.004(3) 0.005(3) 0.012(3) C17 0.032(3) 0.044(4) 0.041(4) 0.000(3) 0.004(3) 0.016(3) C18 0.052(4) 0.039(4) 0.029(4) 0.002(3) 0.002(3) 0.024(3) N1 0.039(3) 0.044(3) 0.032(3) 0.003(3) -0.003(3) 0.020(3) N2 0.033(3) 0.035(3) 0.043(4) -0.002(3) -0.001(3) 0.014(2) N3 0.048(3) 0.029(3) 0.035(3) -0.001(3) -0.001(3) 0.014(2) N4 0.042(3) 0.036(3) 0.028(3) 0.000(3) -0.001(3) 0.009(2) N5 0.040(3) 0.037(3) 0.028(3) -0.004(3) 0.002(3) 0.011(2) N6 0.039(3) 0.039(3) 0.029(3) -0.002(3) 0.002(3) 0.014(2) N7 0.041(3) 0.037(3) 0.040(3) -0.003(3) 0.000(3) 0.018(3) N8 0.036(3) 0.038(3) 0.032(3) -0.001(3) 0.008(2) 0.009(2) N9 0.046(3) 0.033(3) 0.033(3) -0.008(3) -0.004(3) 0.022(3) N10 0.036(3) 0.038(3) 0.031(3) 0.004(3) 0.004(2) 0.017(2) N11 0.031(3) 0.045(3) 0.028(3) 0.002(3) 0.004(2) 0.015(2) N12 0.036(3) 0.030(3) 0.043(4) -0.003(3) 0.005(3) 0.011(2) O1 0.042(3) 0.061(4) 0.052(4) 0.017(3) 0.001(3) 0.012(3) O2 0.043(3) 0.052(3) 0.036(3) -0.003(2) -0.001(2) 0.010(2) O3 0.061(3) 0.058(4) 0.044(3) 0.000(3) 0.001(3) 0.029(3) O4 0.059(3) 0.031(3) 0.032(3) 0.002(2) 0.002(2) 0.009(2) O5 0.067(4) 0.040(3) 0.054(4) -0.005(3) 0.013(3) 0.017(3) O6 0.042(3) 0.039(3) 0.060(4) -0.003(3) -0.003(3) 0.012(2) _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 O1W Cd1 2.489(5) . ? O2W Cd2 2.482(5) . ? O3W Cd3 2.491(5) . ? O4W Cd3 2.293(10) . ? O5W Cd3 2.314(12) . ? O6W Cd2 2.296(10) . ? O7W Cd1 2.310(12) . ? O8W Cd2 2.325(13) . ? O9W Cd1 2.295(13) . ? Cl1 Cd1 2.376(5) . ? Cl1 Cd1 2.401(4) 2_647 ? Cl2 Cd2 2.384(5) . ? Cl2 Cd2 2.415(5) 2_858 ? Cl3 Cd3 2.385(6) 2_746 ? Cl3 Cd3 2.388(4) . ? Cd1 Cl1 2.401(4) 2_647 ? Cd1 O3 2.627(7) . ? Cd1 Cd1 2.942(4) 2_647 ? Cd2 Cl2 2.415(5) 2_858 ? Cd2 O5 2.612(7) . ? Cd2 Cd2 2.913(4) 2_858 ? Cd3 Cl3 2.385(6) 2_746 ? Cd3 O1 2.611(6) . ? Cd3 Cd3 2.896(6) 2_746 ? C1 O1 1.237(9) . ? C1 N2 1.354(10) . ? C1 N1 1.364(12) . ? C2 N1 1.436(9) . ? C2 N3 1.445(8) . ? C2 C3 1.609(13) . ? C2 H2 0.9900 . ? C3 N2 1.444(10) . ? C3 N4 1.444(8) . ? C3 H3 0.9900 . ? C4 O4 1.221(8) . ? C4 N3 1.345(12) . ? C4 N4 1.371(11) . ? C5 N2 1.429(12) . ? C5 N5 1.443(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.435(12) . ? C6 N7 1.454(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.231(8) . ? C7 N5 1.357(11) . ? C7 N6 1.358(11) . ? C8 N7 1.457(10) . ? C8 N5 1.472(8) . ? C8 C9 1.571(13) . ? C8 H8 0.9900 . ? C9 N8 1.446(9) . ? C9 N6 1.448(8) . ? C9 H9 0.9900 . ? C10 O5 1.221(9) . ? C10 N7 1.352(11) . ? C10 N8 1.398(12) . ? C11 N6 1.406(11) . ? C11 N9 1.427(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.416(9) . ? C12 N8 1.435(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.201(9) . ? C13 N10 1.360(9) . ? C13 N9 1.362(9) . ? C14 N9 1.446(9) . ? C14 N11 1.473(9) . ? C14 C15 1.568(10) . ? C14 H14 0.9900 . ? C15 N10 1.435(9) . ? C15 N12 1.456(9) . ? C15 H15 0.9900 . ? C16 O6 1.228(9) . ? C16 N11 1.340(9) . ? C16 N12 1.360(9) . ? C17 N10 1.438(9) 2_757 ? C17 N3 1.461(12) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.412(9) 2_757 ? C18 N1 1.477(11) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? N10 C17 1.438(9) 2_757 ? N12 C18 1.412(9) 2_757 ? 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 Cd1 Cl1 Cd1 76.02(13) . 2_647 ? Cd2 Cl2 Cd2 74.72(14) . 2_858 ? Cd3 Cl3 Cd3 74.71(16) 2_746 . ? O9W Cd1 O7W 67.8(5) . . ? O9W Cd1 Cl1 93.2(4) . . ? O7W Cd1 Cl1 159.0(4) . . ? O9W Cd1 Cl1 158.8(4) . 2_647 ? O7W Cd1 Cl1 93.0(4) . 2_647 ? Cl1 Cd1 Cl1 103.98(13) . 2_647 ? O9W Cd1 O1W 91.1(3) . . ? O7W Cd1 O1W 90.9(3) . . ? Cl1 Cd1 O1W 98.5(2) . . ? Cl1 Cd1 O1W 98.5(2) 2_647 . ? O9W Cd1 O3 67.5(3) . . ? O7W Cd1 O3 67.7(3) . . ? Cl1 Cd1 O3 97.5(2) . . ? Cl1 Cd1 O3 97.4(2) 2_647 . ? O1W Cd1 O3 153.8(2) . . ? O9W Cd1 Cd1 143.6(4) . 2_647 ? O7W Cd1 Cd1 142.8(3) . 2_647 ? Cl1 Cd1 Cd1 52.38(12) . 2_647 ? Cl1 Cd1 Cd1 51.60(13) 2_647 2_647 ? O1W Cd1 Cd1 103.97(19) . 2_647 ? O3 Cd1 Cd1 102.19(19) . 2_647 ? O6W Cd2 O8W 70.5(6) . . ? O6W Cd2 Cl2 159.4(4) . . ? O8W Cd2 Cl2 91.2(4) . . ? O6W Cd2 Cl2 91.0(4) . 2_858 ? O8W Cd2 Cl2 159.9(4) . 2_858 ? Cl2 Cd2 Cl2 105.28(14) . 2_858 ? O6W Cd2 O2W 90.9(3) . . ? O8W Cd2 O2W 89.9(3) . . ? Cl2 Cd2 O2W 98.9(2) . . ? Cl2 Cd2 O2W 98.6(2) 2_858 . ? O6W Cd2 O5 67.6(3) . . ? O8W Cd2 O5 68.6(3) . . ? Cl2 Cd2 O5 97.3(2) . . ? Cl2 Cd2 O5 97.5(2) 2_858 . ? O2W Cd2 O5 153.3(2) . . ? O6W Cd2 Cd2 141.3(4) . 2_858 ? O8W Cd2 Cd2 142.8(4) . 2_858 ? Cl2 Cd2 Cd2 53.13(13) . 2_858 ? Cl2 Cd2 Cd2 52.14(12) 2_858 2_858 ? O2W Cd2 Cd2 104.46(15) . 2_858 ? O5 Cd2 Cd2 102.22(17) . 2_858 ? O4W Cd3 O5W 69.3(5) . . ? O4W Cd3 Cl3 92.3(4) . 2_746 ? O5W Cd3 Cl3 160.2(4) . 2_746 ? O4W Cd3 Cl3 158.3(4) . . ? O5W Cd3 Cl3 91.3(4) . . ? Cl3 Cd3 Cl3 105.29(16) 2_746 . ? O4W Cd3 O3W 90.6(3) . . ? O5W Cd3 O3W 89.1(3) . . ? Cl3 Cd3 O3W 98.7(2) 2_746 . ? Cl3 Cd3 O3W 99.0(2) . . ? O4W Cd3 O1 67.8(3) . . ? O5W Cd3 O1 69.1(3) . . ? Cl3 Cd3 O1 97.7(2) 2_746 . ? Cl3 Cd3 O1 96.83(18) . . ? O3W Cd3 O1 153.3(2) . . ? O4W Cd3 Cd3 143.0(4) . 2_746 ? O5W Cd3 Cd3 142.5(3) . 2_746 ? Cl3 Cd3 Cd3 52.69(12) 2_746 2_746 ? Cl3 Cd3 Cd3 52.60(14) . 2_746 ? O3W Cd3 Cd3 104.67(17) . 2_746 ? O1 Cd3 Cd3 101.99(18) . 2_746 ? O1 C1 N2 123.9(8) . . ? O1 C1 N1 125.7(8) . . ? N2 C1 N1 110.5(6) . . ? N1 C2 N3 113.7(5) . . ? N1 C2 C3 101.5(7) . . ? N3 C2 C3 101.6(6) . . ? N1 C2 H2 113.0 . . ? N3 C2 H2 113.0 . . ? C3 C2 H2 113.0 . . ? N2 C3 N4 114.1(6) . . ? N2 C3 C2 103.5(5) . . ? N4 C3 C2 102.8(6) . . ? N2 C3 H3 111.9 . . ? N4 C3 H3 111.9 . . ? C2 C3 H3 111.9 . . ? O4 C4 N3 126.5(8) . . ? O4 C4 N4 123.8(8) . . ? N3 C4 N4 109.7(6) . . ? N2 C5 N5 114.8(6) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 114.6(6) . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? N7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 124.3(8) . . ? O2 C7 N6 124.6(8) . . ? N5 C7 N6 111.0(6) . . ? N7 C8 N5 112.2(6) . . ? N7 C8 C9 105.5(6) . . ? N5 C8 C9 104.1(6) . . ? N7 C8 H8 111.5 . . ? N5 C8 H8 111.5 . . ? C9 C8 H8 111.5 . . ? N8 C9 N6 113.8(5) . . ? N8 C9 C8 101.5(7) . . ? N6 C9 C8 102.3(6) . . ? N8 C9 H9 112.7 . . ? N6 C9 H9 112.7 . . ? C8 C9 H9 112.7 . . ? O5 C10 N7 125.7(9) . . ? O5 C10 N8 124.5(8) . . ? N7 C10 N8 109.7(6) . . ? N6 C11 N9 115.1(7) . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? N9 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N11 C12 N8 113.1(6) . . ? N11 C12 H12A 109.0 . . ? N8 C12 H12A 109.0 . . ? N11 C12 H12B 109.0 . . ? N8 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N10 125.5(7) . . ? O3 C13 N9 126.0(7) . . ? N10 C13 N9 108.5(5) . . ? N9 C14 N11 112.9(7) . . ? N9 C14 C15 102.3(5) . . ? N11 C14 C15 102.4(5) . . ? N9 C14 H14 112.8 . . ? N11 C14 H14 112.8 . . ? C15 C14 H14 112.8 . . ? N10 C15 N12 113.0(7) . . ? N10 C15 C14 103.4(6) . . ? N12 C15 C14 102.6(5) . . ? N10 C15 H15 112.3 . . ? N12 C15 H15 112.3 . . ? C14 C15 H15 112.3 . . ? O6 C16 N11 125.1(6) . . ? O6 C16 N12 125.5(7) . . ? N11 C16 N12 109.4(6) . . ? N10 C17 N3 113.0(7) 2_757 . ? N10 C17 H17A 109.0 2_757 . ? N3 C17 H17A 109.0 . . ? N10 C17 H17B 109.0 2_757 . ? N3 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N12 C18 N1 113.4(6) 2_757 . ? N12 C18 H18A 108.9 2_757 . ? N1 C18 H18A 108.9 . . ? N12 C18 H18B 108.9 2_757 . ? N1 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C1 N1 C2 112.6(7) . . ? C1 N1 C18 123.0(6) . . ? C2 N1 C18 120.5(8) . . ? C1 N2 C5 122.6(5) . . ? C1 N2 C3 111.1(7) . . ? C5 N2 C3 122.3(6) . . ? C4 N3 C2 113.7(7) . . ? C4 N3 C17 124.5(6) . . ? C2 N3 C17 121.8(7) . . ? C4 N4 C6 125.1(6) . . ? C4 N4 C3 112.1(7) . . ? C6 N4 C3 122.7(6) . . ? C7 N5 C5 125.9(6) . . ? C7 N5 C8 110.0(7) . . ? C5 N5 C8 124.0(6) . . ? C7 N6 C11 124.2(6) . . ? C7 N6 C9 112.5(7) . . ? C11 N6 C9 123.3(7) . . ? C10 N7 C6 122.2(6) . . ? C10 N7 C8 110.5(8) . . ? C6 N7 C8 124.0(6) . . ? C10 N8 C12 123.1(6) . . ? C10 N8 C9 112.4(7) . . ? C12 N8 C9 121.3(8) . . ? C13 N9 C11 120.9(5) . . ? C13 N9 C14 112.7(5) . . ? C11 N9 C14 123.6(6) . . ? C13 N10 C15 112.5(6) . . ? C13 N10 C17 121.0(5) . 2_757 ? C15 N10 C17 122.6(6) . 2_757 ? C16 N11 C12 125.8(6) . . ? C16 N11 C14 112.7(6) . . ? C12 N11 C14 121.3(6) . . ? C16 N12 C18 124.2(6) . 2_757 ? C16 N12 C15 112.8(6) . . ? C18 N12 C15 122.9(6) 2_757 . ? C1 O1 Cd3 128.4(6) . . ? C13 O3 Cd1 129.5(7) . . ? C10 O5 Cd2 129.3(5) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.218 _refine_diff_density_min -1.432 _refine_diff_density_rms 0.180 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.051 -0.051 -0.051 221 87 ' ' _platon_squeeze_details ; ; data_complex03 _database_code_depnum_ccdc_archive 'CCDC 903003' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H75 Cd2 Cl8 N24 Na3 O31' _chemical_formula_weight 1917.57 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' 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 23.6197(15) _cell_length_b 10.7230(6) _cell_length_c 29.6064(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.713(3) _cell_angle_gamma 90.00 _cell_volume 6917.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7585 _exptl_absorpt_correction_T_max 0.7951 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32018 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6731 _reflns_number_gt 5352 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+10.5871P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6731 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 O1W O 0.97546(13) 0.2372(3) 0.16250(12) 0.0402(7) Uani 1 1 d . A . O2W O 0.89007(15) 0.2373(3) 0.22631(12) 0.0430(7) Uani 1 1 d . A . O3W O 1.0000 0.0235(6) 0.2500 0.160(5) Uani 1 2 d S . . O4W O 1.0273(3) 0.4535(6) 0.2514(2) 0.0540(16) Uani 0.50 1 d P . . Cl1 Cl 0.75630(4) 0.26965(9) -0.10800(4) 0.0381(2) Uani 1 1 d . . . Cl2 Cl 0.84255(7) 0.23635(12) 0.03747(4) 0.0602(4) Uani 1 1 d . A . Cl3 Cl 0.74699(7) 0.56006(12) -0.00524(6) 0.0798(5) Uani 1 1 d . A . Cl4 Cl 0.8901(5) 0.4806(4) -0.0383(3) 0.0677(19) Uani 0.61(3) 1 d P A 1 Cl4' Cl 0.8638(12) 0.518(3) -0.0465(3) 0.115(7) Uani 0.39(3) 1 d P A 2 Cd1 Cd 0.79040(2) 0.38209(3) -0.029831(13) 0.06423(18) Uani 1 1 d . . . Na1 Na 0.86937(6) 0.23894(12) 0.14081(6) 0.0312(3) Uani 1 1 d . . . Na2 Na 1.0000 0.2345(2) 0.2500 0.0437(6) Uani 1 2 d S . . C1 C 0.85911(15) 0.5580(3) 0.13255(12) 0.0242(7) Uani 1 1 d . . . C2 C 0.80032(14) 0.7381(3) 0.10689(13) 0.0224(7) Uani 1 1 d . . . H2 H 0.7585 0.7391 0.0810 0.027 Uiso 1 1 calc R A . C3 C 0.84955(15) 0.7361(3) 0.08503(13) 0.0231(7) Uani 1 1 d . A . H3 H 0.8310 0.7344 0.0488 0.028 Uiso 1 1 calc R . . C4 C 0.86044(16) 0.9190(3) 0.13050(13) 0.0258(7) Uani 1 1 d . . . C5 C 0.92581(15) 0.5685(3) 0.08606(13) 0.0260(7) Uani 1 1 d . . . H5A H 0.9090 0.5780 0.0504 0.031 Uiso 1 1 calc R A . H5B H 0.9291 0.4790 0.0933 0.031 Uiso 1 1 calc R . . C6 C 0.92453(15) 0.9016(3) 0.08198(14) 0.0273(7) Uani 1 1 d . . . H6A H 0.9266 0.9922 0.0868 0.033 Uiso 1 1 calc R A . H6B H 0.9070 0.8859 0.0466 0.033 Uiso 1 1 calc R . . C7 C 1.03760(15) 0.5581(3) 0.13525(13) 0.0251(7) Uani 1 1 d . . . C8 C 1.00288(15) 0.7344(3) 0.08585(13) 0.0242(7) Uani 1 1 d . . . H8 H 0.9879 0.7308 0.0497 0.029 Uiso 1 1 calc R A . C9 C 1.07433(15) 0.7352(3) 0.11001(13) 0.0234(7) Uani 1 1 d . A . H9 H 1.0928 0.7321 0.0852 0.028 Uiso 1 1 calc R . . C10 C 1.03688(15) 0.9192(3) 0.13013(13) 0.0245(7) Uani 1 1 d . . . C11 C 1.15028(14) 0.5755(3) 0.16435(13) 0.0238(7) Uani 1 1 d . . . H11A H 1.1481 0.4843 0.1653 0.029 Uiso 1 1 calc R A . H11B H 1.1741 0.5971 0.1447 0.029 Uiso 1 1 calc R . . C12 C 1.15011(15) 0.8975(3) 0.16290(13) 0.0248(7) Uani 1 1 d . . . H12A H 1.1752 0.8740 0.1445 0.030 Uiso 1 1 calc R A . H12B H 1.1491 0.9888 0.1641 0.030 Uiso 1 1 calc R . . C13 C 1.18556(15) 0.5546(3) 0.25344(14) 0.0265(7) Uani 1 1 d . . . C14 C 1.21541(15) 0.7378(3) 0.22611(13) 0.0229(7) Uani 1 1 d . . . H14 H 1.2496 0.7397 0.2146 0.028 Uiso 1 1 calc R A . C15 C 1.23988(16) 0.7395(3) 0.28284(14) 0.0251(7) Uani 1 1 d . A . H15 H 1.2853 0.7426 0.2976 0.030 Uiso 1 1 calc R . . C16 C 1.18031(15) 0.9183(3) 0.25151(14) 0.0273(7) Uani 1 1 d . . . C17 C 0.77466(16) 0.9015(3) 0.15853(13) 0.0271(7) Uani 1 1 d . . . H17A H 0.7319 0.8833 0.1376 0.033 Uiso 1 1 calc R A . H17B H 0.7793 0.9924 0.1609 0.033 Uiso 1 1 calc R . . C18 C 0.77098(15) 0.5771(3) 0.15726(13) 0.0261(7) Uani 1 1 d . . . H18A H 0.7288 0.5992 0.1361 0.031 Uiso 1 1 calc R A . H18B H 0.7738 0.4859 0.1585 0.031 Uiso 1 1 calc R . . N1 N 0.81179(13) 0.6245(2) 0.13557(12) 0.0253(6) Uani 1 1 d . A . N2 N 0.88368(12) 0.6231(2) 0.10487(11) 0.0239(6) Uani 1 1 d . A . N3 N 0.81361(13) 0.8529(3) 0.13555(11) 0.0270(6) Uani 1 1 d . A . N4 N 0.88406(12) 0.8499(3) 0.10320(11) 0.0242(6) Uani 1 1 d . A . N5 N 0.98681(13) 0.6227(2) 0.10595(12) 0.0259(6) Uani 1 1 d . A . N6 N 1.08882(13) 0.6245(2) 0.14048(11) 0.0254(6) Uani 1 1 d . A . N7 N 0.98651(13) 0.8512(3) 0.10240(12) 0.0268(6) Uani 1 1 d . A . N8 N 1.08820(13) 0.8517(3) 0.13711(11) 0.0254(6) Uani 1 1 d . A . N9 N 1.18188(14) 0.6209(2) 0.21315(12) 0.0277(6) Uani 1 1 d . A . N10 N 1.21668(14) 0.6231(3) 0.29407(11) 0.0272(6) Uani 1 1 d . . . N11 N 1.17863(14) 0.8504(3) 0.21197(11) 0.0281(6) Uani 1 1 d . A . N12 N 1.21291(14) 0.8522(3) 0.29320(11) 0.0285(6) Uani 1 1 d . . . O1 O 0.87650(12) 0.4544(2) 0.15102(10) 0.0314(6) Uani 1 1 d . A . O2 O 1.03723(12) 0.4547(2) 0.15374(11) 0.0388(6) Uani 1 1 d . A . O3 O 1.16621(13) 0.4481(2) 0.25245(11) 0.0377(6) Uani 1 1 d . A . O4 O 0.87804(12) 1.0228(2) 0.14760(10) 0.0341(6) Uani 1 1 d . . . O5 O 1.03559(12) 1.0262(2) 0.14504(11) 0.0400(7) Uani 1 1 d . A . O6 O 1.15903(14) 1.0220(2) 0.24945(11) 0.0417(7) Uani 1 1 d . A . 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 O1W 0.0329(14) 0.0353(15) 0.0521(18) 0.0001(12) 0.0159(13) -0.0001(11) O2W 0.0539(18) 0.0360(15) 0.0457(18) 0.0021(12) 0.0264(15) 0.0016(12) O3W 0.295(14) 0.043(4) 0.097(6) 0.000 0.024(7) 0.000 O4W 0.070(4) 0.041(3) 0.049(4) 0.000(3) 0.020(4) 0.006(3) Cl1 0.0339(5) 0.0437(5) 0.0374(6) -0.0059(4) 0.0144(4) -0.0033(4) Cl2 0.0860(9) 0.0592(7) 0.0327(6) 0.0100(5) 0.0200(6) 0.0186(6) Cl3 0.0856(10) 0.0399(6) 0.0694(9) -0.0131(6) -0.0191(7) 0.0133(6) Cl4 0.099(4) 0.064(2) 0.048(3) -0.0234(15) 0.037(2) -0.0204(19) Cl4' 0.131(11) 0.161(12) 0.034(2) 0.000(4) 0.012(4) -0.083(10) Cd1 0.1097(4) 0.0426(2) 0.0299(2) 0.00180(14) 0.0155(2) 0.00321(18) Na1 0.0312(7) 0.0209(7) 0.0387(9) 0.0000(6) 0.0104(6) -0.0006(5) Na2 0.0407(12) 0.0443(13) 0.0421(14) 0.000 0.0115(10) 0.000 C1 0.0284(17) 0.0186(15) 0.0228(17) -0.0037(13) 0.0069(13) -0.0040(12) C2 0.0188(15) 0.0190(15) 0.0268(18) 0.0008(13) 0.0061(13) -0.0010(11) C3 0.0251(16) 0.0191(15) 0.0229(17) -0.0007(12) 0.0069(13) -0.0013(12) C4 0.0302(17) 0.0200(16) 0.0232(18) 0.0046(13) 0.0061(14) 0.0040(13) C5 0.0276(17) 0.0192(15) 0.0313(19) -0.0072(14) 0.0115(14) -0.0016(13) C6 0.0236(16) 0.0239(16) 0.034(2) 0.0089(14) 0.0108(14) 0.0016(13) C7 0.0286(17) 0.0198(16) 0.0300(19) -0.0020(14) 0.0149(14) -0.0012(13) C8 0.0280(17) 0.0232(16) 0.0242(18) 0.0016(13) 0.0131(14) 0.0013(13) C9 0.0278(17) 0.0194(15) 0.0259(18) 0.0007(13) 0.0137(14) -0.0020(12) C10 0.0288(17) 0.0179(16) 0.0291(19) -0.0009(13) 0.0137(14) -0.0027(12) C11 0.0223(15) 0.0177(15) 0.0336(19) -0.0030(13) 0.0132(14) 0.0006(12) C12 0.0245(16) 0.0207(15) 0.0321(19) 0.0059(13) 0.0141(14) -0.0022(12) C13 0.0245(16) 0.0225(16) 0.037(2) 0.0021(14) 0.0164(15) 0.0028(13) C14 0.0195(15) 0.0186(15) 0.0324(19) 0.0002(13) 0.0118(14) -0.0013(11) C15 0.0245(16) 0.0215(16) 0.032(2) 0.0004(13) 0.0134(14) -0.0011(12) C16 0.0243(16) 0.0270(18) 0.033(2) -0.0010(15) 0.0134(15) -0.0021(13) C17 0.0322(18) 0.0199(16) 0.030(2) 0.0038(14) 0.0129(15) 0.0059(13) C18 0.0259(16) 0.0198(15) 0.034(2) -0.0039(14) 0.0135(15) -0.0078(12) N1 0.0255(14) 0.0194(14) 0.0326(17) 0.0003(11) 0.0128(12) -0.0002(10) N2 0.0220(13) 0.0196(14) 0.0307(16) -0.0003(11) 0.0107(12) 0.0015(10) N3 0.0306(15) 0.0181(13) 0.0341(17) -0.0018(12) 0.0146(13) -0.0020(11) N4 0.0229(13) 0.0166(13) 0.0323(16) -0.0014(11) 0.0099(12) -0.0031(10) N5 0.0249(14) 0.0186(14) 0.0332(17) -0.0005(11) 0.0103(12) -0.0031(10) N6 0.0240(14) 0.0186(14) 0.0337(17) 0.0053(11) 0.0111(12) 0.0002(10) N7 0.0245(14) 0.0187(13) 0.0361(17) 0.0001(12) 0.0105(12) 0.0023(11) N8 0.0254(14) 0.0195(13) 0.0315(16) -0.0021(12) 0.0112(12) -0.0002(11) N9 0.0350(16) 0.0188(14) 0.0293(17) -0.0011(11) 0.0122(13) -0.0040(11) N10 0.0328(15) 0.0211(14) 0.0302(17) 0.0008(11) 0.0149(13) -0.0015(11) N11 0.0329(15) 0.0200(14) 0.0314(17) 0.0005(12) 0.0124(13) 0.0049(11) N12 0.0362(16) 0.0200(14) 0.0310(17) -0.0010(12) 0.0149(13) 0.0019(12) O1 0.0385(14) 0.0194(12) 0.0384(15) 0.0029(10) 0.0173(12) 0.0014(10) O2 0.0341(14) 0.0253(13) 0.0547(18) 0.0110(12) 0.0147(13) -0.0033(10) O3 0.0497(16) 0.0233(13) 0.0438(17) -0.0008(11) 0.0222(13) -0.0087(11) O4 0.0413(14) 0.0176(12) 0.0427(16) -0.0038(11) 0.0154(12) -0.0032(10) O5 0.0339(14) 0.0234(13) 0.0596(19) -0.0075(12) 0.0145(13) 0.0014(10) O6 0.0591(18) 0.0238(13) 0.0426(17) -0.0007(12) 0.0202(14) 0.0148(12) _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 O1W Na1 2.334(3) . ? O1W Na2 2.427(3) . ? O2W Na1 2.386(4) . ? O2W Na2 2.414(3) . ? O3W Na2 2.263(7) . ? O4W O4W 1.257(14) 2_755 ? O4W Na2 2.431(7) . ? Cl1 Cd1 2.4533(10) . ? Cl1 Na1 2.7452(17) 7_655 ? Cl2 Cd1 2.4566(12) . ? Cl2 Na1 2.875(2) . ? Cl3 Cd1 2.4084(15) . ? Cl4 Cd1 2.679(7) . ? Cl4' Cd1 2.458(10) . ? Na1 O4 2.329(3) 1_545 ? Na1 O1 2.328(3) . ? Na1 Cl1 2.7452(17) 7_655 ? Na1 Na2 3.5029(15) . ? Na2 O2W 2.414(3) 2_755 ? Na2 O1W 2.427(3) 2_755 ? Na2 O4W 2.431(7) 2_755 ? Na2 Na1 3.5029(15) 2_755 ? C1 O1 1.236(4) . ? C1 N1 1.357(4) . ? C1 N2 1.365(4) . ? C2 N1 1.449(4) . ? C2 N3 1.459(4) . ? C2 C3 1.534(5) . ? C2 H2 0.9900 . ? C3 N2 1.448(4) . ? C3 N4 1.450(4) . ? C3 H3 0.9900 . ? C4 O4 1.226(4) . ? C4 N4 1.365(5) . ? C4 N3 1.370(5) . ? C5 N2 1.439(4) . ? C5 N5 1.451(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.442(4) . ? C6 N7 1.455(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.238(4) . ? C7 N6 1.360(4) . ? C7 N5 1.367(5) . ? C8 N5 1.452(4) . ? C8 N7 1.451(4) . ? C8 C9 1.558(5) . ? C8 H8 0.9900 . ? C9 N6 1.449(4) . ? C9 N8 1.452(4) . ? C9 H9 0.9900 . ? C10 O5 1.233(4) . ? C10 N8 1.358(4) . ? C10 N7 1.366(4) . ? C11 N9 1.431(5) . ? C11 N6 1.446(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.436(5) . ? C12 N8 1.449(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.226(4) . ? C13 N9 1.362(5) . ? C13 N10 1.358(5) . ? C14 N11 1.452(4) . ? C14 N9 1.453(4) . ? C14 C15 1.551(5) . ? C14 H14 0.9900 . ? C15 N10 1.452(4) . ? C15 N12 1.453(4) . ? C15 H15 0.9900 . ? C16 O6 1.212(4) . ? C16 N11 1.366(5) . ? C16 N12 1.373(5) . ? C17 N3 1.437(5) . ? C17 N12 1.444(5) 2_755 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N10 1.442(5) 2_755 ? C18 N1 1.441(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? N10 C18 1.442(5) 2_755 ? N12 C17 1.444(5) 2_755 ? O4 Na1 2.329(3) 1_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 Na1 O1W Na2 94.72(11) . . ? Na1 O2W Na2 93.74(11) . . ? O4W O4W Na2 75.01(16) 2_755 . ? Cd1 Cl1 Na1 105.46(5) . 7_655 ? Cd1 Cl2 Na1 133.83(6) . . ? Cl3 Cd1 Cl4' 90.3(9) . . ? Cl3 Cd1 Cl1 130.66(4) . . ? Cl4' Cd1 Cl1 95.9(4) . . ? Cl3 Cd1 Cl2 113.42(5) . . ? Cl4' Cd1 Cl2 111.7(7) . . ? Cl1 Cd1 Cl2 109.37(4) . . ? Cl3 Cd1 Cl4 102.00(10) . . ? Cl4' Cd1 Cl4 14.9(7) . . ? Cl1 Cd1 Cl4 94.92(14) . . ? Cl2 Cd1 Cl4 98.2(2) . . ? O4 Na1 O1 167.73(12) 1_545 . ? O4 Na1 O1W 85.35(10) 1_545 . ? O1 Na1 O1W 87.50(10) . . ? O4 Na1 O2W 85.76(11) 1_545 . ? O1 Na1 O2W 83.95(11) . . ? O1W Na1 O2W 87.11(12) . . ? O4 Na1 Cl1 92.53(8) 1_545 7_655 ? O1 Na1 Cl1 95.35(8) . 7_655 ? O1W Na1 Cl1 175.03(11) . 7_655 ? O2W Na1 Cl1 97.22(9) . 7_655 ? O4 Na1 Cl2 93.33(9) 1_545 . ? O1 Na1 Cl2 97.06(9) . . ? O1W Na1 Cl2 93.71(10) . . ? O2W Na1 Cl2 178.72(10) . . ? Cl1 Na1 Cl2 81.91(5) 7_655 . ? O4 Na1 Na2 83.69(9) 1_545 . ? O1 Na1 Na2 84.26(9) . . ? O1W Na1 Na2 43.66(8) . . ? O2W Na1 Na2 43.45(8) . . ? Cl1 Na1 Na2 140.61(6) 7_655 . ? Cl2 Na1 Na2 137.36(6) . . ? O3W Na2 O2W 90.72(9) . 2_755 ? O3W Na2 O2W 90.72(9) . . ? O2W Na2 O2W 178.56(17) 2_755 . ? O3W Na2 O1W 90.68(8) . . ? O2W Na2 O1W 95.56(10) 2_755 . ? O2W Na2 O1W 84.42(10) . . ? O3W Na2 O1W 90.68(8) . 2_755 ? O2W Na2 O1W 84.42(10) 2_755 2_755 ? O2W Na2 O1W 95.56(10) . 2_755 ? O1W Na2 O1W 178.65(17) . 2_755 ? O3W Na2 O4W 165.01(16) . . ? O2W Na2 O4W 74.62(18) 2_755 . ? O2W Na2 O4W 103.94(18) . . ? O1W Na2 O4W 87.69(18) . . ? O1W Na2 O4W 91.00(18) 2_755 . ? O3W Na2 O4W 165.01(16) . 2_755 ? O2W Na2 O4W 103.94(18) 2_755 2_755 ? O2W Na2 O4W 74.62(18) . 2_755 ? O1W Na2 O4W 91.00(18) . 2_755 ? O1W Na2 O4W 87.69(18) 2_755 2_755 ? O4W Na2 O4W 30.0(3) . 2_755 ? O3W Na2 Na1 90.78(4) . 2_755 ? O2W Na2 Na1 42.81(8) 2_755 2_755 ? O2W Na2 Na1 137.16(8) . 2_755 ? O1W Na2 Na1 138.36(7) . 2_755 ? O1W Na2 Na1 41.61(7) 2_755 2_755 ? O4W Na2 Na1 80.66(16) . 2_755 ? O4W Na2 Na1 97.81(17) 2_755 2_755 ? O3W Na2 Na1 90.78(4) . . ? O2W Na2 Na1 137.16(8) 2_755 . ? O2W Na2 Na1 42.81(8) . . ? O1W Na2 Na1 41.61(7) . . ? O1W Na2 Na1 138.36(7) 2_755 . ? O4W Na2 Na1 97.81(17) . . ? O4W Na2 Na1 80.66(16) 2_755 . ? Na1 Na2 Na1 178.44(9) 2_755 . ? O1 C1 N1 125.8(3) . . ? O1 C1 N2 125.4(3) . . ? N1 C1 N2 108.8(3) . . ? N1 C2 N3 114.8(3) . . ? N1 C2 C3 103.6(2) . . ? N3 C2 C3 103.3(2) . . ? N1 C2 H2 111.5 . . ? N3 C2 H2 111.5 . . ? C3 C2 H2 111.5 . . ? N2 C3 N4 114.1(3) . . ? N2 C3 C2 103.6(3) . . ? N4 C3 C2 103.9(3) . . ? N2 C3 H3 111.6 . . ? N4 C3 H3 111.6 . . ? C2 C3 H3 111.6 . . ? O4 C4 N4 125.9(3) . . ? O4 C4 N3 125.7(3) . . ? N4 C4 N3 108.4(3) . . ? N2 C5 N5 114.0(3) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 113.9(3) . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6B 108.8 . . ? N7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.2(3) . . ? O2 C7 N5 125.5(3) . . ? N6 C7 N5 109.3(3) . . ? N5 C8 N7 115.3(3) . . ? N5 C8 C9 103.0(3) . . ? N7 C8 C9 102.9(3) . . ? N5 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N6 C9 N8 114.3(3) . . ? N6 C9 C8 103.6(3) . . ? N8 C9 C8 103.4(3) . . ? N6 C9 H9 111.6 . . ? N8 C9 H9 111.6 . . ? C8 C9 H9 111.6 . . ? O5 C10 N8 125.8(3) . . ? O5 C10 N7 125.1(3) . . ? N8 C10 N7 109.0(3) . . ? N9 C11 N6 113.8(3) . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11B 108.8 . . ? N6 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.4(3) . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? N8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 124.6(3) . . ? O3 C13 N10 126.5(3) . . ? N9 C13 N10 108.8(3) . . ? N11 C14 N9 115.9(3) . . ? N11 C14 C15 103.5(3) . . ? N9 C14 C15 103.5(3) . . ? N11 C14 H14 111.1 . . ? N9 C14 H14 111.1 . . ? C15 C14 H14 111.1 . . ? N10 C15 N12 115.6(3) . . ? N10 C15 C14 102.8(3) . . ? N12 C15 C14 103.2(3) . . ? N10 C15 H15 111.5 . . ? N12 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O6 C16 N11 124.9(4) . . ? O6 C16 N12 126.6(3) . . ? N11 C16 N12 108.4(3) . . ? N3 C17 N12 114.4(3) . 2_755 ? N3 C17 H17A 108.7 . . ? N12 C17 H17A 108.7 2_755 . ? N3 C17 H17B 108.7 . . ? N12 C17 H17B 108.7 2_755 . ? H17A C17 H17B 107.6 . . ? N10 C18 N1 114.4(3) 2_755 . ? N10 C18 H18A 108.7 2_755 . ? N1 C18 H18A 108.7 . . ? N10 C18 H18B 108.7 2_755 . ? N1 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C1 N1 C18 123.6(3) . . ? C1 N1 C2 112.0(3) . . ? C18 N1 C2 123.5(3) . . ? C1 N2 C5 122.8(3) . . ? C1 N2 C3 111.9(3) . . ? C5 N2 C3 122.9(3) . . ? C4 N3 C17 123.7(3) . . ? C4 N3 C2 112.0(3) . . ? C17 N3 C2 123.3(3) . . ? C4 N4 C6 122.7(3) . . ? C4 N4 C3 112.2(3) . . ? C6 N4 C3 122.3(3) . . ? C7 N5 C5 123.0(3) . . ? C7 N5 C8 112.0(3) . . ? C5 N5 C8 122.7(3) . . ? C7 N6 C11 123.1(3) . . ? C7 N6 C9 111.9(3) . . ? C11 N6 C9 123.6(3) . . ? C10 N7 C6 123.7(3) . . ? C10 N7 C8 112.3(3) . . ? C6 N7 C8 122.5(3) . . ? C10 N8 C12 124.0(3) . . ? C10 N8 C9 112.2(3) . . ? C12 N8 C9 123.3(3) . . ? C13 N9 C11 122.6(3) . . ? C13 N9 C14 112.0(3) . . ? C11 N9 C14 125.3(3) . . ? C13 N10 C18 122.1(3) . 2_755 ? C13 N10 C15 112.7(3) . . ? C18 N10 C15 125.0(3) 2_755 . ? C16 N11 C12 121.8(3) . . ? C16 N11 C14 112.3(3) . . ? C12 N11 C14 125.4(3) . . ? C16 N12 C17 122.0(3) . 2_755 ? C16 N12 C15 112.3(3) . . ? C17 N12 C15 125.1(3) 2_755 . ? C1 O1 Na1 147.1(2) . . ? C4 O4 Na1 149.6(2) . 1_565 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.411 _refine_diff_density_min -1.455 _refine_diff_density_rms 0.103 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 253 96 ' ' 2 1.000 0.000 0.500 253 96 ' ' 3 0.500 0.500 0.500 253 96 ' ' 4 0.500 0.500 1.000 253 96 ' ' 5 0.500 0.244 0.250 82 32 ' ' 6 1.000 0.255 0.750 82 32 ' ' 7 1.000 0.744 0.250 82 32 ' ' 8 0.500 0.755 0.750 82 32 ' ' _platon_squeeze_details ; ; data_complex04 _database_code_depnum_ccdc_archive 'CCDC 903004' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 Cd2 Cl4 N24 O29' _chemical_formula_weight 1669.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0180(5) _cell_length_b 12.4823(10) _cell_length_c 12.7410(6) _cell_angle_alpha 107.495(2) _cell_angle_beta 108.0150(10) _cell_angle_gamma 97.391(2) _cell_volume 1541.11(16) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7531 _exptl_absorpt_correction_T_max 0.8078 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16917 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5370 _reflns_number_gt 4868 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+1.7225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5370 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 O1W O 0.2492(3) 0.1426(3) 0.3163(3) 0.0523(8) Uani 1 1 d . . . O2W O 0.2513(3) 0.3040(3) 0.1634(4) 0.0637(10) Uani 1 1 d . . . Cl1 Cl -0.01055(9) 0.08661(7) -0.09067(7) 0.0301(2) Uani 1 1 d . . . Cl2 Cl 0.33807(9) 0.05067(9) 0.06616(8) 0.0377(2) Uani 1 1 d . . . Cd1 Cd 0.15141(2) 0.11319(2) 0.11811(2) 0.02921(11) Uani 1 1 d . . . C1 C 0.0008(3) 0.1305(3) 0.4725(3) 0.0246(7) Uani 1 1 d . . . C2 C -0.1374(3) 0.1362(3) 0.5807(3) 0.0245(7) Uani 1 1 d . . . H2 H -0.1590 0.0751 0.6113 0.029 Uiso 1 1 calc R . . C3 C -0.2223(3) 0.1025(3) 0.4488(3) 0.0245(7) Uani 1 1 d . . . H3 H -0.2831 0.0249 0.4171 0.029 Uiso 1 1 calc R . . C4 C -0.2661(3) 0.2685(3) 0.5592(3) 0.0268(7) Uani 1 1 d . . . C5 C -0.1561(3) 0.0679(3) 0.2668(3) 0.0253(7) Uani 1 1 d . . . H5A H -0.0797 0.0472 0.2496 0.030 Uiso 1 1 calc R . . H5B H -0.2292 -0.0015 0.2264 0.030 Uiso 1 1 calc R . . C6 C -0.4043(3) 0.1849(3) 0.3471(3) 0.0275(7) Uani 1 1 d . . . H6A H -0.4640 0.2267 0.3756 0.033 Uiso 1 1 calc R . . H6B H -0.4522 0.1036 0.3031 0.033 Uiso 1 1 calc R . . C7 C -0.1139(3) 0.2129(3) 0.1773(3) 0.0228(7) Uani 1 1 d . . . C8 C -0.3264(3) 0.1646(3) 0.1771(3) 0.0228(7) Uani 1 1 d . . . H8 H -0.3880 0.0874 0.1308 0.027 Uiso 1 1 calc R . . C9 C -0.3261(3) 0.2386(3) 0.0996(3) 0.0232(7) Uani 1 1 d . . . H9 H -0.3828 0.1944 0.0158 0.028 Uiso 1 1 calc R . . C10 C -0.4085(3) 0.3240(3) 0.2445(3) 0.0250(7) Uani 1 1 d . . . C11 C -0.1454(3) 0.3208(3) 0.0411(3) 0.0247(7) Uani 1 1 d . . . H11A H -0.2166 0.2955 -0.0364 0.030 Uiso 1 1 calc R . . H11B H -0.0699 0.2929 0.0288 0.030 Uiso 1 1 calc R . . C12 C -0.4030(3) 0.4233(3) 0.1025(3) 0.0285(7) Uani 1 1 d . . . H12A H -0.4380 0.3877 0.0160 0.034 Uiso 1 1 calc R . . H12B H -0.4710 0.4554 0.1263 0.034 Uiso 1 1 calc R . . C13 C 0.0198(3) 0.5092(3) 0.1401(3) 0.0240(7) Uani 1 1 d . . . C14 C -0.2016(3) 0.5186(3) 0.0750(3) 0.0257(7) Uani 1 1 d . . . H14 H -0.2503 0.5036 -0.0096 0.031 Uiso 1 1 calc R . . C15 C -0.1097(3) 0.6434(3) 0.1408(3) 0.0229(7) Uani 1 1 d . . . H15 H -0.1259 0.6914 0.0909 0.027 Uiso 1 1 calc R . . C16 C -0.2560(3) 0.6158(3) 0.2354(3) 0.0275(7) Uani 1 1 d . . . C17 C 0.1410(3) 0.7143(3) 0.2365(3) 0.0261(7) Uani 1 1 d . . . H17A H 0.2151 0.6845 0.2229 0.031 Uiso 1 1 calc R . . H17B H 0.1353 0.7791 0.2084 0.031 Uiso 1 1 calc R . . C18 C -0.1115(3) 0.8117(3) 0.3122(3) 0.0258(7) Uani 1 1 d . . . H18A H -0.0978 0.8546 0.2621 0.031 Uiso 1 1 calc R . . H18B H -0.1862 0.8309 0.3337 0.031 Uiso 1 1 calc R . . N1 N -0.0042(3) 0.1510(2) 0.5818(2) 0.0253(6) Uani 1 1 d . . . N2 N -0.1253(3) 0.1030(3) 0.3931(2) 0.0267(6) Uani 1 1 d . . . N3 N -0.1694(3) 0.2421(2) 0.6374(2) 0.0256(6) Uani 1 1 d . . . N4 N -0.2936(3) 0.1916(3) 0.4474(2) 0.0270(6) Uani 1 1 d . . . N5 N -0.1915(3) 0.1556(2) 0.2195(2) 0.0235(6) Uani 1 1 d . . . N6 N -0.1880(3) 0.2683(2) 0.1144(2) 0.0245(6) Uani 1 1 d . . . N7 N -0.3678(3) 0.2322(2) 0.2679(2) 0.0247(6) Uani 1 1 d . . . N8 N -0.3763(3) 0.3340(3) 0.1517(3) 0.0271(6) Uani 1 1 d . . . N9 N -0.1085(3) 0.4464(2) 0.0906(3) 0.0261(6) Uani 1 1 d . . . N10 N 0.0221(3) 0.6243(2) 0.1667(2) 0.0248(6) Uani 1 1 d . . . N11 N -0.2885(3) 0.5172(2) 0.1394(3) 0.0273(6) Uani 1 1 d . . . N12 N -0.1440(3) 0.6878(2) 0.2445(2) 0.0247(6) Uani 1 1 d . . . O1 O 0.1008(2) 0.1322(2) 0.4494(2) 0.0343(6) Uani 1 1 d . . . O2 O 0.0013(2) 0.2135(2) 0.1936(2) 0.0295(5) Uani 1 1 d . . . O3 O 0.1169(2) 0.4699(2) 0.1544(2) 0.0353(6) Uani 1 1 d . . . O4 O -0.3214(3) 0.3461(2) 0.5846(2) 0.0374(6) Uani 1 1 d . . . O5 O -0.4657(3) 0.3852(2) 0.2958(2) 0.0344(6) Uani 1 1 d . . . O6 O -0.3151(3) 0.6380(2) 0.3025(2) 0.0393(6) 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 O1W 0.0419(17) 0.082(2) 0.0391(15) 0.0228(16) 0.0197(13) 0.0215(16) O2W 0.0352(16) 0.0312(16) 0.118(3) 0.0224(18) 0.0226(18) 0.0118(13) Cl1 0.0356(5) 0.0277(4) 0.0326(4) 0.0149(3) 0.0147(4) 0.0109(4) Cl2 0.0274(5) 0.0458(5) 0.0374(5) 0.0079(4) 0.0136(4) 0.0142(4) Cd1 0.02478(16) 0.03060(17) 0.03415(16) 0.01142(11) 0.01285(12) 0.00872(11) C1 0.0305(18) 0.0190(16) 0.0284(17) 0.0099(13) 0.0138(15) 0.0093(14) C2 0.0268(17) 0.0225(16) 0.0301(17) 0.0116(13) 0.0153(14) 0.0085(14) C3 0.0270(17) 0.0238(17) 0.0256(16) 0.0097(13) 0.0120(14) 0.0086(14) C4 0.0233(17) 0.0320(19) 0.0280(17) 0.0129(14) 0.0118(14) 0.0056(15) C5 0.0315(18) 0.0200(16) 0.0265(16) 0.0073(13) 0.0126(14) 0.0104(14) C6 0.0229(17) 0.0349(19) 0.0298(17) 0.0140(15) 0.0136(14) 0.0087(14) C7 0.0251(17) 0.0170(15) 0.0242(15) 0.0028(12) 0.0106(13) 0.0051(13) C8 0.0208(16) 0.0253(17) 0.0228(15) 0.0083(13) 0.0087(13) 0.0067(13) C9 0.0179(16) 0.0250(17) 0.0234(15) 0.0062(13) 0.0060(13) 0.0047(13) C10 0.0193(16) 0.0272(17) 0.0264(16) 0.0080(14) 0.0073(13) 0.0056(14) C11 0.0304(18) 0.0224(16) 0.0265(16) 0.0086(13) 0.0173(14) 0.0067(14) C12 0.0221(17) 0.0295(18) 0.0351(18) 0.0137(15) 0.0095(14) 0.0084(14) C13 0.0306(18) 0.0267(17) 0.0222(15) 0.0120(13) 0.0141(14) 0.0127(14) C14 0.0273(17) 0.0306(18) 0.0230(15) 0.0128(14) 0.0101(14) 0.0106(15) C15 0.0219(16) 0.0270(17) 0.0237(15) 0.0141(13) 0.0083(13) 0.0071(13) C16 0.0268(17) 0.0313(19) 0.0276(17) 0.0124(14) 0.0107(14) 0.0119(15) C17 0.0293(18) 0.0294(18) 0.0251(16) 0.0118(14) 0.0151(14) 0.0076(14) C18 0.0252(17) 0.0247(17) 0.0288(17) 0.0100(14) 0.0096(14) 0.0107(14) N1 0.0237(14) 0.0284(15) 0.0263(14) 0.0099(12) 0.0121(12) 0.0071(12) N2 0.0274(15) 0.0341(16) 0.0249(14) 0.0119(12) 0.0143(12) 0.0136(13) N3 0.0288(15) 0.0297(15) 0.0214(13) 0.0094(12) 0.0114(12) 0.0119(12) N4 0.0269(15) 0.0330(16) 0.0249(14) 0.0111(12) 0.0119(12) 0.0127(12) N5 0.0255(14) 0.0265(15) 0.0238(13) 0.0133(11) 0.0104(11) 0.0108(12) N6 0.0242(14) 0.0261(14) 0.0302(14) 0.0140(12) 0.0148(12) 0.0082(12) N7 0.0251(14) 0.0259(15) 0.0260(14) 0.0087(11) 0.0132(12) 0.0071(12) N8 0.0279(15) 0.0264(15) 0.0324(15) 0.0129(12) 0.0145(13) 0.0106(12) N9 0.0264(15) 0.0219(14) 0.0365(16) 0.0113(12) 0.0180(13) 0.0098(12) N10 0.0214(14) 0.0253(15) 0.0268(14) 0.0072(11) 0.0103(11) 0.0042(11) N11 0.0257(15) 0.0257(15) 0.0340(15) 0.0095(12) 0.0162(13) 0.0075(12) N12 0.0251(14) 0.0205(14) 0.0289(14) 0.0079(11) 0.0118(12) 0.0049(11) O1 0.0288(13) 0.0485(16) 0.0336(13) 0.0170(12) 0.0175(11) 0.0153(12) O2 0.0238(13) 0.0331(13) 0.0351(13) 0.0115(11) 0.0145(10) 0.0115(10) O3 0.0287(13) 0.0303(14) 0.0530(16) 0.0171(12) 0.0189(12) 0.0125(11) O4 0.0446(16) 0.0396(15) 0.0356(13) 0.0127(12) 0.0190(12) 0.0263(13) O5 0.0326(14) 0.0359(14) 0.0396(14) 0.0107(11) 0.0195(12) 0.0161(12) O6 0.0355(14) 0.0383(15) 0.0455(15) 0.0065(12) 0.0266(13) 0.0047(12) _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 O1W Cd1 2.308(3) . ? O2W Cd1 2.307(3) . ? Cl1 Cd1 2.5983(9) . ? Cl1 Cd1 2.6259(9) 2 ? Cl2 Cd1 2.4943(9) . ? Cd1 O2 2.454(2) . ? Cd1 Cl1 2.6259(9) 2 ? C1 O1 1.223(4) . ? C1 N1 1.359(4) . ? C1 N2 1.368(5) . ? C2 N1 1.451(4) . ? C2 N3 1.448(4) . ? C2 C3 1.542(5) . ? C2 H2 0.9900 . ? C3 N4 1.443(4) . ? C3 N2 1.455(4) . ? C3 H3 0.9900 . ? C4 O4 1.226(4) . ? C4 N4 1.371(4) . ? C4 N3 1.367(5) . ? C5 N5 1.441(4) . ? C5 N2 1.448(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(4) . ? C6 N7 1.441(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.220(4) . ? C7 N6 1.364(4) . ? C7 N5 1.374(4) . ? C8 N5 1.448(4) . ? C8 N7 1.448(4) . ? C8 C9 1.542(5) . ? C8 H8 0.9900 . ? C9 N8 1.444(4) . ? C9 N6 1.457(4) . ? C9 H9 0.9900 . ? C10 O5 1.219(4) . ? C10 N7 1.363(5) . ? C10 N8 1.370(4) . ? C11 N6 1.442(4) . ? C11 N9 1.450(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.452(4) . ? C12 N8 1.453(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.220(4) . ? C13 N10 1.368(4) . ? C13 N9 1.370(5) . ? C14 N11 1.442(4) . ? C14 N9 1.457(4) . ? C14 C15 1.562(5) . ? C14 H14 0.9900 . ? C15 N10 1.454(4) . ? C15 N12 1.455(4) . ? C15 H15 0.9900 . ? C16 O6 1.217(4) . ? C16 N11 1.361(4) . ? C16 N12 1.381(4) . ? C17 N3 1.446(4) 2_566 ? C17 N10 1.439(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.439(4) 2_566 ? C18 N12 1.460(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? N1 C18 1.439(4) 2_566 ? N3 C17 1.446(4) 2_566 ? 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 Cd1 Cl1 Cd1 93.27(3) . 2 ? O2W Cd1 O1W 87.71(14) . . ? O2W Cd1 O2 78.71(10) . . ? O1W Cd1 O2 80.58(10) . . ? O2W Cd1 Cl2 90.29(8) . . ? O1W Cd1 Cl2 94.50(8) . . ? O2 Cd1 Cl2 168.07(6) . . ? O2W Cd1 Cl1 94.88(10) . . ? O1W Cd1 Cl1 165.42(8) . . ? O2 Cd1 Cl1 85.85(6) . . ? Cl2 Cd1 Cl1 99.82(3) . . ? O2W Cd1 Cl1 168.76(9) . 2 ? O1W Cd1 Cl1 88.03(9) . 2 ? O2 Cd1 Cl1 90.33(6) . 2 ? Cl2 Cd1 Cl1 100.41(3) . 2 ? Cl1 Cd1 Cl1 86.73(3) . 2 ? O1 C1 N1 125.5(3) . . ? O1 C1 N2 126.4(3) . . ? N1 C1 N2 108.0(3) . . ? N1 C2 N3 114.6(3) . . ? N1 C2 C3 103.2(3) . . ? N3 C2 C3 103.4(3) . . ? N1 C2 H2 111.7 . . ? N3 C2 H2 111.7 . . ? C3 C2 H2 111.7 . . ? N4 C3 N2 115.4(3) . . ? N4 C3 C2 103.9(3) . . ? N2 C3 C2 103.2(3) . . ? N4 C3 H3 111.2 . . ? N2 C3 H3 111.2 . . ? C2 C3 H3 111.2 . . ? O4 C4 N4 125.4(3) . . ? O4 C4 N3 125.9(3) . . ? N4 C4 N3 108.7(3) . . ? N5 C5 N2 113.8(3) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 113.5(3) . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? N7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 126.3(3) . . ? O2 C7 N5 125.5(3) . . ? N6 C7 N5 108.2(3) . . ? N5 C8 N7 114.5(3) . . ? N5 C8 C9 103.9(2) . . ? N7 C8 C9 103.5(3) . . ? N5 C8 H8 111.4 . . ? N7 C8 H8 111.4 . . ? C9 C8 H8 111.4 . . ? N8 C9 N6 115.4(3) . . ? N8 C9 C8 103.2(3) . . ? N6 C9 C8 102.9(3) . . ? N8 C9 H9 111.6 . . ? N6 C9 H9 111.6 . . ? C8 C9 H9 111.6 . . ? O5 C10 N7 126.0(3) . . ? O5 C10 N8 126.0(3) . . ? N7 C10 N8 108.0(3) . . ? N6 C11 N9 113.7(3) . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? N9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 113.9(3) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N10 125.0(3) . . ? O3 C13 N9 126.1(3) . . ? N10 C13 N9 108.9(3) . . ? N11 C14 N9 115.1(3) . . ? N11 C14 C15 102.9(3) . . ? N9 C14 C15 102.2(3) . . ? N11 C14 H14 111.9 . . ? N9 C14 H14 111.9 . . ? C15 C14 H14 111.9 . . ? N10 C15 N12 114.4(3) . . ? N10 C15 C14 103.8(3) . . ? N12 C15 C14 103.1(2) . . ? N10 C15 H15 111.6 . . ? N12 C15 H15 111.6 . . ? C14 C15 H15 111.6 . . ? O6 C16 N11 126.2(3) . . ? O6 C16 N12 125.2(3) . . ? N11 C16 N12 108.6(3) . . ? N3 C17 N10 115.3(3) 2_566 . ? N3 C17 H17A 108.5 2_566 . ? N10 C17 H17A 108.5 . . ? N3 C17 H17B 108.5 2_566 . ? N10 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? N1 C18 N12 113.2(3) 2_566 . ? N1 C18 H18A 108.9 2_566 . ? N12 C18 H18A 108.9 . . ? N1 C18 H18B 108.9 2_566 . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C1 N1 C18 123.1(3) . 2_566 ? C1 N1 C2 113.0(3) . . ? C18 N1 C2 123.8(3) 2_566 . ? C1 N2 C5 122.4(3) . . ? C1 N2 C3 112.6(3) . . ? C5 N2 C3 124.8(3) . . ? C4 N3 C17 122.5(3) . 2_566 ? C4 N3 C2 111.9(3) . . ? C17 N3 C2 121.4(3) 2_566 . ? C4 N4 C6 122.3(3) . . ? C4 N4 C3 111.8(3) . . ? C6 N4 C3 124.1(3) . . ? C7 N5 C8 112.0(3) . . ? C7 N5 C5 123.4(3) . . ? C8 N5 C5 121.8(3) . . ? C7 N6 C11 123.2(3) . . ? C7 N6 C9 112.4(3) . . ? C11 N6 C9 121.9(3) . . ? C10 N7 C6 123.0(3) . . ? C10 N7 C8 112.0(3) . . ? C6 N7 C8 121.7(3) . . ? C10 N8 C9 112.5(3) . . ? C10 N8 C12 123.9(3) . . ? C9 N8 C12 123.4(3) . . ? C13 N9 C14 112.5(3) . . ? C13 N9 C11 122.8(3) . . ? C14 N9 C11 123.9(3) . . ? C13 N10 C17 122.5(3) . . ? C13 N10 C15 111.7(3) . . ? C17 N10 C15 124.3(3) . . ? C16 N11 C14 113.0(3) . . ? C16 N11 C12 123.2(3) . . ? C14 N11 C12 123.8(3) . . ? C16 N12 C15 111.2(3) . . ? C16 N12 C18 120.3(3) . . ? C15 N12 C18 121.4(3) . . ? C7 O2 Cd1 144.8(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.633 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.091 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.015 0.500 0.500 187 50 ' ' 2 0.500 0.000 0.500 226 83 ' ' _platon_squeeze_details ; ;