# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Vadapalli Chandrasekhar' _publ_contact_author_email VC@IITK.AC.IN _publ_section_title ; Trapping Two Different CdCl2 1D-Layered Structures by a Cyclocarbophosphazene-based Ligand ; loop_ _publ_author_name 'Vadapalli Chandrasekhar' 'Tapas Senapati' # Attachment 'cif.cif' data_Ligand(L) _database_code_depnum_ccdc_archive 'CCDC 727814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H20 N7 O2 P' _chemical_formula_sum 'C16 H20 N7 O2 P' _chemical_formula_weight 373.36 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' P P 0.1023 0.0942 '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_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3777(16) _cell_length_b 10.187(2) _cell_length_c 12.570(3) _cell_angle_alpha 86.803(4) _cell_angle_beta 81.176(4) _cell_angle_gamma 74.745(4) _cell_volume 900.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2061 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.38 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9812 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5933 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.46 _reflns_number_total 4284 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0843P)^2^+0.6198P] 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 SHELXL _refine_ls_extinction_coef 0.068(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4284 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 P1 P 0.15985(11) 0.54424(8) 0.33977(6) 0.0453(3) Uani 1 1 d . . . O1 O 0.1587(3) 0.3878(2) 0.35007(16) 0.0522(5) Uani 1 1 d . . . O2 O 0.2109(3) 0.5439(2) 0.45766(16) 0.0527(5) Uani 1 1 d . . . N1 N 0.3265(3) 0.5662(3) 0.2513(2) 0.0484(6) Uani 1 1 d . . . N2 N -0.0399(4) 0.6411(3) 0.3271(2) 0.0524(6) Uani 1 1 d . . . N3 N 0.1011(3) 0.7473(2) 0.17076(19) 0.0468(6) Uani 1 1 d . . . N4 N -0.2117(4) 0.8255(3) 0.2415(2) 0.0522(6) Uani 1 1 d . . . N5 N 0.4135(4) 0.6800(3) 0.0975(2) 0.0533(6) Uani 1 1 d . . . N6 N 0.0960(5) 0.1411(4) 0.1135(3) 0.0780(10) Uani 1 1 d . . . N7 N 0.3174(5) 0.8562(3) 0.6178(3) 0.0705(8) Uani 1 1 d . . . C1 C 0.2743(4) 0.6642(3) 0.1758(2) 0.0423(6) Uani 1 1 d . . . C2 C -0.0446(4) 0.7349(3) 0.2470(2) 0.0444(6) Uani 1 1 d . . . C3 C -0.3777(5) 0.8230(4) 0.3200(3) 0.0649(9) Uani 1 1 d . . . H3A H -0.3396 0.7630 0.3788 0.097 Uiso 1 1 calc R . . H3B H -0.4664 0.7912 0.2865 0.097 Uiso 1 1 calc R . . H3C H -0.4365 0.9130 0.3465 0.097 Uiso 1 1 calc R . . C4 C -0.2382(5) 0.9323(3) 0.1595(3) 0.0583(8) Uani 1 1 d . . . H4A H -0.1186 0.9300 0.1159 0.088 Uiso 1 1 calc R . . H4B H -0.2875 1.0192 0.1934 0.088 Uiso 1 1 calc R . . H4C H -0.3261 0.9184 0.1150 0.088 Uiso 1 1 calc R . . C5 C 0.6056(5) 0.5947(4) 0.0928(3) 0.0645(9) Uani 1 1 d . . . H5A H 0.6090 0.5242 0.1469 0.097 Uiso 1 1 calc R . . H5B H 0.6885 0.6489 0.1052 0.097 Uiso 1 1 calc R . . H5C H 0.6464 0.5545 0.0230 0.097 Uiso 1 1 calc R . . C6 C 0.3785(5) 0.7827(4) 0.0123(3) 0.0638(9) Uani 1 1 d . . . H6A H 0.2524 0.8406 0.0284 0.096 Uiso 1 1 calc R . . H6B H 0.3911 0.7388 -0.0551 0.096 Uiso 1 1 calc R . . H6C H 0.4689 0.8362 0.0075 0.096 Uiso 1 1 calc R . . C7 C 0.1385(4) 0.3122(3) 0.2669(2) 0.0469(7) Uani 1 1 d . . . C8 C 0.0642(5) 0.3652(4) 0.1756(3) 0.0576(8) Uani 1 1 d . . . H8 H 0.0272 0.4588 0.1634 0.069 Uiso 1 1 calc R . . C9 C 0.0460(5) 0.2750(4) 0.1018(3) 0.0652(9) Uani 1 1 d . . . H9 H -0.0047 0.3110 0.0400 0.078 Uiso 1 1 calc R . . C10 C 0.1676(7) 0.0941(4) 0.2033(4) 0.0832(12) Uani 1 1 d . . . H10 H 0.2027 0.0002 0.2141 0.100 Uiso 1 1 calc R . . C11 C 0.1935(6) 0.1740(3) 0.2813(3) 0.0645(9) Uani 1 1 d . . . H11 H 0.2466 0.1354 0.3418 0.077 Uiso 1 1 calc R . . C12 C 0.2419(4) 0.6526(3) 0.5066(2) 0.0467(6) Uani 1 1 d . . . C13 C 0.1976(5) 0.7852(3) 0.4691(3) 0.0590(8) Uani 1 1 d . . . H13 H 0.1419 0.8089 0.4069 0.071 Uiso 1 1 calc R . . C14 C 0.2392(6) 0.8815(4) 0.5278(3) 0.0693(10) Uani 1 1 d . . . H14 H 0.2103 0.9710 0.5024 0.083 Uiso 1 1 calc R . . C15 C 0.3563(6) 0.7268(4) 0.6513(3) 0.0671(9) Uani 1 1 d . . . H15 H 0.4101 0.7056 0.7144 0.080 Uiso 1 1 calc R . . C16 C 0.3225(5) 0.6224(3) 0.5993(3) 0.0550(8) Uani 1 1 d . . . H16 H 0.3534 0.5336 0.6262 0.066 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 P1 0.0512(5) 0.0451(4) 0.0399(4) 0.0024(3) -0.0064(3) -0.0137(3) O1 0.0696(14) 0.0467(11) 0.0424(11) 0.0029(9) -0.0112(10) -0.0176(10) O2 0.0706(14) 0.0469(11) 0.0431(11) 0.0024(9) -0.0120(10) -0.0181(10) N1 0.0469(13) 0.0506(14) 0.0461(13) 0.0042(11) -0.0099(10) -0.0090(11) N2 0.0531(15) 0.0521(14) 0.0511(14) 0.0034(11) -0.0039(11) -0.0152(12) N3 0.0494(14) 0.0475(13) 0.0418(13) 0.0040(10) -0.0066(10) -0.0105(11) N4 0.0457(14) 0.0483(14) 0.0588(16) 0.0001(11) -0.0063(11) -0.0066(11) N5 0.0517(15) 0.0587(15) 0.0480(14) 0.0072(12) -0.0010(11) -0.0171(12) N6 0.107(3) 0.075(2) 0.062(2) -0.0125(16) -0.0073(18) -0.042(2) N7 0.083(2) 0.0669(19) 0.0668(19) -0.0107(15) -0.0137(16) -0.0247(16) C1 0.0453(15) 0.0470(15) 0.0369(13) -0.0048(11) -0.0058(11) -0.0154(12) C2 0.0503(16) 0.0409(14) 0.0442(15) -0.0044(11) -0.0082(12) -0.0138(12) C3 0.0498(18) 0.065(2) 0.075(2) -0.0081(17) 0.0005(16) -0.0099(15) C4 0.062(2) 0.0506(17) 0.0587(19) 0.0035(14) -0.0154(15) -0.0042(15) C5 0.0516(19) 0.076(2) 0.063(2) -0.0005(17) 0.0048(15) -0.0187(17) C6 0.070(2) 0.071(2) 0.0516(19) 0.0120(16) -0.0029(16) -0.0271(18) C7 0.0451(15) 0.0515(16) 0.0449(15) -0.0030(12) -0.0004(12) -0.0167(13) C8 0.065(2) 0.0564(18) 0.0520(18) 0.0013(14) -0.0114(15) -0.0151(15) C9 0.072(2) 0.083(3) 0.0474(18) -0.0031(17) -0.0125(16) -0.031(2) C10 0.124(4) 0.052(2) 0.075(3) -0.0074(18) -0.015(3) -0.024(2) C11 0.088(3) 0.0452(17) 0.061(2) 0.0015(15) -0.0169(18) -0.0151(17) C12 0.0495(16) 0.0489(16) 0.0413(15) -0.0023(12) -0.0023(12) -0.0138(13) C13 0.072(2) 0.0546(18) 0.0525(18) 0.0035(14) -0.0155(16) -0.0168(16) C14 0.086(3) 0.0513(19) 0.071(2) -0.0047(17) -0.010(2) -0.0188(18) C15 0.075(2) 0.073(2) 0.057(2) -0.0054(17) -0.0187(17) -0.0190(19) C16 0.0577(19) 0.0571(18) 0.0505(17) 0.0001(14) -0.0116(14) -0.0137(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 P1 N2 1.569(3) . ? P1 N1 1.580(3) . ? P1 O2 1.584(2) . ? P1 O1 1.594(2) . ? O1 C7 1.380(3) . ? O2 C12 1.382(3) . ? N1 C1 1.360(4) . ? N2 C2 1.347(4) . ? N3 C1 1.342(4) . ? N3 C2 1.354(4) . ? N4 C2 1.340(4) . ? N4 C4 1.452(4) . ? N4 C3 1.455(4) . ? N5 C1 1.345(4) . ? N5 C5 1.449(4) . ? N5 C6 1.458(4) . ? N6 C9 1.321(5) . ? N6 C10 1.332(5) . ? N7 C14 1.329(5) . ? N7 C15 1.332(5) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C11 1.369(4) . ? C7 C8 1.371(4) . ? C8 C9 1.386(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.374(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C16 1.371(4) . ? C12 C13 1.377(4) . ? C13 C14 1.383(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.374(5) . ? C15 H15 0.9300 . ? C16 H16 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 N2 P1 N1 114.41(13) . . ? N2 P1 O2 112.68(13) . . ? N1 P1 O2 111.83(13) . . ? N2 P1 O1 112.87(13) . . ? N1 P1 O1 110.97(13) . . ? O2 P1 O1 92.05(11) . . ? C7 O1 P1 124.41(19) . . ? C12 O2 P1 125.90(19) . . ? C1 N1 P1 115.3(2) . . ? C2 N2 P1 116.4(2) . . ? C1 N3 C2 118.9(2) . . ? C2 N4 C4 122.8(3) . . ? C2 N4 C3 121.0(3) . . ? C4 N4 C3 116.1(3) . . ? C1 N5 C5 121.7(3) . . ? C1 N5 C6 121.8(3) . . ? C5 N5 C6 116.6(3) . . ? C9 N6 C10 115.7(3) . . ? C14 N7 C15 115.5(3) . . ? N3 C1 N5 116.4(3) . . ? N3 C1 N1 127.7(3) . . ? N5 C1 N1 115.9(3) . . ? N4 C2 N2 116.7(3) . . ? N4 C2 N3 116.3(3) . . ? N2 C2 N3 127.0(3) . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N5 C5 H5A 109.5 . . ? N5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N5 C6 H6A 109.5 . . ? N5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 C7 C8 119.4(3) . . ? C11 C7 O1 115.5(3) . . ? C8 C7 O1 125.1(3) . . ? C7 C8 C9 117.8(3) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? N6 C9 C8 124.4(3) . . ? N6 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? N6 C10 C11 124.8(4) . . ? N6 C10 H10 117.6 . . ? C11 C10 H10 117.6 . . ? C7 C11 C10 117.9(3) . . ? C7 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C16 C12 C13 119.4(3) . . ? C16 C12 O2 115.8(3) . . ? C13 C12 O2 124.8(3) . . ? C12 C13 C14 117.3(3) . . ? C12 C13 H13 121.4 . . ? C14 C13 H13 121.4 . . ? N7 C14 C13 125.1(3) . . ? N7 C14 H14 117.5 . . ? C13 C14 H14 117.5 . . ? N7 C15 C16 124.5(3) . . ? N7 C15 H15 117.7 . . ? C16 C15 H15 117.7 . . ? C12 C16 C15 118.2(3) . . ? C12 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.345 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.077 #===END data_Complex-1 _database_code_depnum_ccdc_archive 'CCDC 727815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Cd3 Cl6 N14 O5 P2' _chemical_formula_sum 'C32 H40 Cd3 Cl6 N14 O5 P2' _chemical_formula_weight 1312.62 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.196(5) _cell_length_b 15.367(5) _cell_length_c 16.615(5) _cell_angle_alpha 76.167(5) _cell_angle_beta 87.919(5) _cell_angle_gamma 64.595(5) _cell_volume 3170.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5888 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8776 _exptl_absorpt_correction_T_max 0.9287 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17670 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12157 _reflns_number_gt 9532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1258P)^2^+8.1059P] 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 12157 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.2121 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.50034(4) 0.55956(3) 0.67841(3) 0.02550(16) Uani 1 1 d . . . Cd2 Cd 0.34554(4) 0.56286(4) 0.49053(3) 0.03107(17) Uani 1 1 d . . . Cd3 Cd 0.54314(4) 0.43134(3) 0.91202(3) 0.02022(15) Uani 1 1 d . . . Cl1 Cl 0.33746(17) 0.68460(14) 0.57748(11) 0.0420(5) Uani 1 1 d . . . Cl2 Cl 0.49053(14) 0.42764(12) 0.60377(10) 0.0263(4) Uani 1 1 d . . . Cl3 Cl 0.38282(13) 0.53067(12) 0.79887(10) 0.0261(3) Uani 1 1 d . . . Cl4 Cl 0.65481(13) 0.43122(12) 0.78339(10) 0.0264(4) Uani 1 1 d . . . Cl5 Cl 0.35394(17) 0.42842(14) 0.42229(11) 0.0372(4) Uani 1 1 d . . . Cl6 Cl 0.44319(14) 0.42149(12) 1.04694(10) 0.0260(4) Uani 1 1 d . . . P1 P 0.5530(2) 0.97352(15) 0.80079(12) 0.0386(5) Uani 1 1 d . . . P2 P -0.01430(15) 1.00451(14) 0.17103(12) 0.0319(4) Uani 1 1 d . . . O1 O 0.5250(6) 1.0250(4) 0.8768(3) 0.0522(17) Uani 1 1 d . . . O2 O 0.5079(5) 0.8959(4) 0.8437(3) 0.0423(14) Uani 1 1 d . . . O3 O 0.1101(4) 0.9439(4) 0.1838(3) 0.0321(11) Uani 1 1 d . . . O4 O -0.0112(4) 1.1000(4) 0.1097(3) 0.0330(12) Uani 1 1 d . . . O5 O 0.1970(5) 0.5554(6) 0.5496(5) 0.069(2) Uani 1 1 d . . . N1 N 0.4865(6) 1.0450(5) 0.7162(4) 0.0376(15) Uani 1 1 d . . . N2 N 0.6471(6) 1.0037(5) 0.6477(5) 0.0468(18) Uani 1 1 d . . . N3 N 0.6740(6) 0.9218(5) 0.7937(4) 0.0432(17) Uani 1 1 d . . . N4 N 0.4924(7) 1.1213(5) 0.5823(5) 0.052(2) Uani 1 1 d . . . N5 N 0.8089(7) 0.8920(7) 0.7086(6) 0.073(3) Uani 1 1 d . . . N6 N 0.5360(5) 1.2846(4) 0.8969(4) 0.0270(13) Uani 1 1 d . . . N7 N 0.5010(5) 0.6885(4) 0.7282(4) 0.0282(13) Uani 1 1 d . . . N8 N 0.2511(5) 0.7000(5) 0.3831(4) 0.0338(14) Uani 1 1 d . . . N9 N -0.0628(5) 1.0258(5) 0.2553(4) 0.0366(15) Uani 1 1 d . . . N10 N -0.1753(6) 0.9495(6) 0.2382(5) 0.0472(18) Uani 1 1 d . . . N11 N -0.0660(5) 0.9549(5) 0.1247(4) 0.0350(15) Uani 1 1 d . . . N12 N -0.1784(6) 1.0111(6) 0.3508(5) 0.0513(19) Uani 1 1 d . . . N13 N -0.1874(7) 0.8944(7) 0.1233(6) 0.066(3) Uani 1 1 d . . . N14 N 0.7061(5) 0.3143(4) 0.9856(3) 0.0274(13) Uani 1 1 d . . . C1 C 0.7065(8) 0.9419(7) 0.7165(6) 0.048(2) Uani 1 1 d . . . C2 C 0.5448(7) 1.0527(6) 0.6517(5) 0.0388(19) Uani 1 1 d . . . C3 C 0.8791(10) 0.8164(9) 0.7839(9) 0.089(4) Uani 1 1 d . . . H3A H 0.8461 0.8305 0.8337 0.134 Uiso 1 1 calc R . . H3B H 0.9449 0.8202 0.7841 0.134 Uiso 1 1 calc R . . H3C H 0.8907 0.7509 0.7814 0.134 Uiso 1 1 calc R . . C4 C 0.8542(11) 0.9076(11) 0.6253(9) 0.106(5) Uani 1 1 d . . . H4A H 0.8445 0.8673 0.5933 0.159 Uiso 1 1 calc R . . H4B H 0.9275 0.8890 0.6339 0.159 Uiso 1 1 calc R . . H4C H 0.8191 0.9763 0.5960 0.159 Uiso 1 1 calc R . . C5 C 0.5450(10) 1.1344(8) 0.5039(6) 0.073(3) Uani 1 1 d . . . H5A H 0.5079 1.2013 0.4708 0.110 Uiso 1 1 calc R . . H5B H 0.5451 1.0887 0.4733 0.110 Uiso 1 1 calc R . . H5C H 0.6157 1.1217 0.5171 0.110 Uiso 1 1 calc R . . C6 C 0.3791(9) 1.1832(9) 0.5759(8) 0.080(4) Uani 1 1 d . . . H6A H 0.3463 1.1699 0.5338 0.120 Uiso 1 1 calc R . . H6B H 0.3654 1.2521 0.5613 0.120 Uiso 1 1 calc R . . H6C H 0.3516 1.1681 0.6283 0.120 Uiso 1 1 calc R . . C7 C 0.5337(7) 1.1108(5) 0.8788(5) 0.0347(18) Uani 1 1 d . . . C8 C 0.5293(8) 1.1838(6) 0.8095(5) 0.044(2) Uani 1 1 d . . . H8 H 0.5261 1.1757 0.7561 0.053 Uiso 1 1 calc R . . C9 C 0.5299(7) 1.2690(5) 0.8226(5) 0.0362(18) Uani 1 1 d . . . H9 H 0.5257 1.3188 0.7762 0.043 Uiso 1 1 calc R . . C10 C 0.5407(7) 1.2132(6) 0.9624(5) 0.0397(19) Uani 1 1 d . . . H10 H 0.5451 1.2228 1.0151 0.048 Uiso 1 1 calc R . . C11 C 0.5393(7) 1.1258(6) 0.9566(4) 0.040(2) Uani 1 1 d . . . H11 H 0.5421 1.0780 1.0041 0.048 Uiso 1 1 calc R . . C12 C 0.5085(7) 0.8268(5) 0.8020(4) 0.0358(19) Uani 1 1 d . . . C13 C 0.5999(7) 0.7547(6) 0.7866(5) 0.0379(18) Uani 1 1 d . . . H13 H 0.6643 0.7514 0.8006 0.045 Uiso 1 1 calc R . . C14 C 0.5920(7) 0.6866(6) 0.7490(5) 0.0365(18) Uani 1 1 d . . . H14 H 0.6533 0.6368 0.7376 0.044 Uiso 1 1 calc R . . C15 C 0.4139(7) 0.7594(5) 0.7451(5) 0.0363(18) Uani 1 1 d . . . H15 H 0.3502 0.7612 0.7310 0.044 Uiso 1 1 calc R . . C16 C 0.4131(7) 0.8296(6) 0.7822(5) 0.0375(18) Uani 1 1 d . . . H16 H 0.3507 0.8779 0.7939 0.045 Uiso 1 1 calc R . . C17 C 0.2776(7) 0.7730(6) 0.3664(5) 0.042(2) Uani 1 1 d . . . H17 H 0.3309 0.7693 0.3999 0.050 Uiso 1 1 calc R . . C18 C 0.2305(7) 0.8556(6) 0.3015(5) 0.0423(19) Uani 1 1 d . . . H18 H 0.2505 0.9072 0.2925 0.051 Uiso 1 1 calc R . . C19 C 0.1541(6) 0.8609(5) 0.2504(4) 0.0318(16) Uani 1 1 d . . . C20 C 0.1261(6) 0.7842(6) 0.2653(5) 0.0383(18) Uani 1 1 d . . . H20 H 0.0750 0.7848 0.2314 0.046 Uiso 1 1 calc R . . C21 C 0.1772(6) 0.7053(6) 0.3331(5) 0.0394(18) Uani 1 1 d . . . H21 H 0.1585 0.6529 0.3443 0.047 Uiso 1 1 calc R . . C22 C -0.1078(6) 1.1725(5) 0.0684(4) 0.0302(16) Uani 1 1 d . . . C23 C -0.1748(6) 1.2430(6) 0.1073(5) 0.0351(17) Uani 1 1 d . . . H23 H -0.1580 1.2439 0.1606 0.042 Uiso 1 1 calc R . . C24 C -0.1303(6) 1.1739(6) -0.0112(5) 0.0368(18) Uani 1 1 d . . . H24 H -0.0840 1.1275 -0.0378 0.044 Uiso 1 1 calc R . . C25 C -0.1366(6) 0.9931(6) 0.2787(5) 0.0389(19) Uani 1 1 d . . . C26 C -0.1408(6) 0.9336(6) 0.1644(6) 0.043(2) Uani 1 1 d . . . C27 C -0.1440(8) 1.0601(7) 0.3991(6) 0.056(2) Uani 1 1 d . . . H27A H -0.0911 1.0111 0.4412 0.084 Uiso 1 1 calc R . . H27B H -0.2022 1.1012 0.4249 0.084 Uiso 1 1 calc R . . H27C H -0.1158 1.1006 0.3633 0.084 Uiso 1 1 calc R . . C28 C -0.2505(10) 0.9692(10) 0.3866(7) 0.078(4) Uani 1 1 d . . . H28A H -0.2857 0.9606 0.3429 0.117 Uiso 1 1 calc R . . H28B H -0.3011 1.0135 0.4154 0.117 Uiso 1 1 calc R . . H28C H -0.2119 0.9059 0.4248 0.117 Uiso 1 1 calc R . . C29 C -0.1544(9) 0.8761(10) 0.0426(7) 0.076(4) Uani 1 1 d . . . H29A H -0.1182 0.9153 0.0187 0.113 Uiso 1 1 calc R . . H29B H -0.2146 0.8940 0.0066 0.113 Uiso 1 1 calc R . . H29C H -0.1085 0.8069 0.0494 0.113 Uiso 1 1 calc R . . C30 C -0.2612(11) 0.8568(13) 0.1635(9) 0.101(5) Uani 1 1 d . . . H30A H -0.2235 0.7881 0.1924 0.151 Uiso 1 1 calc R . . H30B H -0.3106 0.8629 0.1221 0.151 Uiso 1 1 calc R . . H30C H -0.2978 0.8947 0.2024 0.151 Uiso 1 1 calc R . . C31 C 0.7753(6) 0.2469(5) 0.9495(4) 0.0323(17) Uani 1 1 d . . . H31 H 0.7590 0.2492 0.8951 0.039 Uiso 1 1 calc R . . C32 C 0.7315(6) 0.3126(5) 1.0630(4) 0.0320(16) Uani 1 1 d . . . H32 H 0.6843 0.3602 1.0882 0.038 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 0.0418(3) 0.0176(3) 0.0148(3) -0.00225(19) -0.0018(2) -0.0113(2) Cd2 0.0376(3) 0.0295(3) 0.0171(3) -0.0023(2) -0.0045(2) -0.0076(2) Cd3 0.0284(3) 0.0144(2) 0.0145(2) -0.00278(18) -0.00052(18) -0.00641(19) Cl1 0.0563(12) 0.0265(9) 0.0221(9) -0.0065(7) -0.0110(8) 0.0029(8) Cl2 0.0390(9) 0.0206(8) 0.0157(7) -0.0026(6) -0.0033(6) -0.0100(7) Cl3 0.0295(8) 0.0241(8) 0.0195(8) -0.0046(6) -0.0012(6) -0.0071(7) Cl4 0.0317(8) 0.0245(8) 0.0167(7) -0.0019(6) 0.0016(6) -0.0083(7) Cl5 0.0619(12) 0.0405(10) 0.0196(8) -0.0036(8) 0.0051(8) -0.0338(10) Cl6 0.0406(9) 0.0216(8) 0.0201(8) -0.0073(6) 0.0074(7) -0.0169(7) P1 0.0779(15) 0.0292(10) 0.0227(10) -0.0093(8) 0.0117(10) -0.0351(11) P2 0.0280(9) 0.0290(10) 0.0209(9) -0.0032(8) -0.0008(7) 0.0027(8) O1 0.113(5) 0.041(3) 0.027(3) -0.018(3) 0.022(3) -0.054(4) O2 0.090(4) 0.031(3) 0.027(3) -0.015(2) 0.022(3) -0.042(3) O3 0.028(3) 0.027(3) 0.023(3) 0.001(2) -0.003(2) 0.001(2) O4 0.028(3) 0.030(3) 0.025(3) 0.001(2) -0.003(2) -0.001(2) O5 0.041(4) 0.083(5) 0.073(5) -0.018(4) 0.010(3) -0.018(4) N1 0.065(4) 0.027(3) 0.030(3) -0.010(3) 0.010(3) -0.028(3) N2 0.065(5) 0.037(4) 0.037(4) -0.005(3) 0.016(4) -0.024(4) N3 0.069(5) 0.039(4) 0.035(4) -0.010(3) 0.001(3) -0.035(4) N4 0.078(6) 0.038(4) 0.035(4) 0.000(3) 0.011(4) -0.027(4) N5 0.061(6) 0.074(6) 0.075(7) -0.010(5) 0.012(5) -0.025(5) N6 0.038(3) 0.017(3) 0.025(3) -0.005(2) 0.004(3) -0.011(3) N7 0.044(4) 0.021(3) 0.021(3) -0.002(2) 0.001(3) -0.016(3) N8 0.035(3) 0.035(3) 0.022(3) -0.006(3) -0.004(3) -0.007(3) N9 0.036(3) 0.035(3) 0.023(3) -0.006(3) 0.000(3) -0.001(3) N10 0.052(4) 0.050(4) 0.049(4) -0.025(4) 0.022(4) -0.025(4) N11 0.029(3) 0.034(3) 0.031(3) -0.012(3) 0.000(3) -0.001(3) N12 0.061(5) 0.050(4) 0.037(4) -0.016(4) 0.021(4) -0.018(4) N13 0.064(5) 0.090(7) 0.070(6) -0.058(5) 0.033(5) -0.039(5) N14 0.034(3) 0.017(3) 0.019(3) -0.005(2) -0.001(2) 0.000(2) C1 0.057(6) 0.047(5) 0.048(5) -0.012(4) 0.006(4) -0.030(5) C2 0.071(6) 0.027(4) 0.028(4) -0.010(3) 0.014(4) -0.028(4) C3 0.076(8) 0.064(7) 0.114(12) 0.006(7) -0.024(8) -0.029(7) C4 0.079(9) 0.105(11) 0.101(11) 0.005(9) 0.029(8) -0.026(8) C5 0.115(10) 0.057(6) 0.031(5) 0.001(5) 0.018(6) -0.029(6) C6 0.071(8) 0.067(7) 0.076(8) 0.018(6) 0.006(6) -0.025(6) C7 0.067(5) 0.019(3) 0.028(4) -0.006(3) 0.009(4) -0.027(4) C8 0.087(7) 0.044(5) 0.015(3) -0.007(3) 0.009(4) -0.042(5) C9 0.066(5) 0.028(4) 0.019(4) -0.001(3) 0.008(3) -0.027(4) C10 0.071(6) 0.029(4) 0.024(4) -0.013(3) 0.010(4) -0.025(4) C11 0.084(6) 0.033(4) 0.014(3) -0.004(3) 0.013(4) -0.039(4) C12 0.077(6) 0.019(3) 0.021(3) -0.005(3) 0.013(4) -0.030(4) C13 0.060(5) 0.036(4) 0.032(4) -0.010(3) 0.011(4) -0.034(4) C14 0.060(5) 0.029(4) 0.022(4) -0.009(3) 0.010(3) -0.021(4) C15 0.055(5) 0.022(4) 0.028(4) -0.005(3) 0.001(3) -0.014(3) C16 0.052(5) 0.027(4) 0.030(4) -0.011(3) 0.010(4) -0.014(4) C17 0.044(5) 0.035(4) 0.037(5) 0.003(4) -0.016(4) -0.013(4) C18 0.045(5) 0.034(4) 0.040(5) 0.001(4) -0.005(4) -0.015(4) C19 0.029(4) 0.030(4) 0.021(3) -0.007(3) 0.000(3) 0.002(3) C20 0.031(4) 0.039(4) 0.027(4) -0.003(3) -0.008(3) -0.002(3) C21 0.039(4) 0.043(5) 0.030(4) -0.011(4) 0.002(3) -0.011(4) C22 0.029(4) 0.026(4) 0.023(4) -0.002(3) -0.001(3) -0.002(3) C23 0.036(4) 0.039(4) 0.021(4) -0.012(3) -0.006(3) -0.005(3) C24 0.034(4) 0.038(4) 0.022(4) -0.014(3) -0.002(3) 0.004(3) C25 0.041(4) 0.030(4) 0.031(4) -0.005(3) 0.010(3) -0.004(3) C26 0.039(4) 0.040(5) 0.047(5) -0.019(4) 0.011(4) -0.010(4) C27 0.066(6) 0.060(6) 0.036(5) -0.025(5) 0.014(4) -0.017(5) C28 0.095(9) 0.098(9) 0.058(7) -0.035(7) 0.050(7) -0.052(8) C29 0.068(7) 0.116(10) 0.072(8) -0.067(8) 0.030(6) -0.046(7) C30 0.099(10) 0.163(14) 0.105(11) -0.084(11) 0.058(9) -0.095(11) C31 0.038(4) 0.027(4) 0.017(3) -0.006(3) 0.000(3) 0.001(3) C32 0.040(4) 0.031(4) 0.023(4) -0.013(3) 0.003(3) -0.011(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 Cd1 N7 2.325(6) . ? Cd1 Cl4 2.5813(17) . ? Cd1 Cl1 2.6037(19) . ? Cd1 Cl3 2.6370(18) . ? Cd1 Cl5 2.653(2) 2_666 ? Cd1 Cl2 2.6690(18) . ? Cd2 N8 2.319(6) . ? Cd2 O5 2.330(7) . ? Cd2 Cl5 2.543(2) . ? Cd2 Cl1 2.588(2) . ? Cd2 Cl2 2.6145(17) . ? Cd2 Cl2 2.794(2) 2_666 ? Cd3 N6 2.373(5) 1_545 ? Cd3 N14 2.381(6) . ? Cd3 Cl6 2.5964(17) 2_667 ? Cd3 Cl4 2.6141(18) . ? Cd3 Cl6 2.6177(18) . ? Cd3 Cl3 2.6461(18) . ? Cl2 Cd2 2.794(2) 2_666 ? Cl5 Cd1 2.653(2) 2_666 ? Cl6 Cd3 2.5964(17) 2_667 ? P1 N3 1.567(8) . ? P1 N1 1.594(7) . ? P1 O1 1.597(5) . ? P1 O2 1.599(5) . ? P2 N9 1.581(6) . ? P2 N11 1.585(7) . ? P2 O4 1.591(5) . ? P2 O3 1.597(5) . ? O1 C7 1.384(8) . ? O2 C12 1.396(8) . ? O3 C19 1.391(8) . ? O4 C22 1.409(8) . ? N1 C2 1.344(10) . ? N2 C2 1.326(11) . ? N2 C1 1.337(12) . ? N3 C1 1.358(11) . ? N4 C2 1.342(11) . ? N4 C6 1.468(14) . ? N4 C5 1.493(12) . ? N5 C1 1.340(13) . ? N5 C4 1.515(16) . ? N5 C3 1.519(15) . ? N6 C9 1.325(9) . ? N6 C10 1.328(9) . ? N6 Cd3 2.373(5) 1_565 ? N7 C15 1.327(10) . ? N7 C14 1.336(10) . ? N8 C17 1.295(10) . ? N8 C21 1.324(10) . ? N9 C25 1.352(11) . ? N10 C25 1.328(11) . ? N10 C26 1.341(11) . ? N11 C26 1.348(11) . ? N12 C25 1.354(10) . ? N12 C27 1.442(12) . ? N12 C28 1.468(13) . ? N13 C26 1.356(12) . ? N13 C29 1.455(12) . ? N13 C30 1.471(14) . ? N14 C31 1.334(9) . ? N14 C32 1.339(9) . ? C7 C11 1.376(10) . ? C7 C8 1.383(10) . ? C8 C9 1.382(11) . ? C10 C11 1.378(10) . ? C12 C13 1.362(12) . ? C12 C16 1.384(12) . ? C13 C14 1.385(10) . ? C15 C16 1.361(10) . ? C17 C18 1.376(11) . ? C18 C19 1.364(11) . ? C19 C20 1.365(12) . ? C20 C21 1.384(11) . ? C22 C24 1.364(10) . ? C22 C23 1.379(10) . ? C23 C32 1.389(10) 1_464 ? C24 C31 1.380(10) 1_464 ? C31 C24 1.380(10) 1_646 ? C32 C23 1.388(10) 1_646 ? 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 N7 Cd1 Cl4 90.82(15) . . ? N7 Cd1 Cl1 90.40(15) . . ? Cl4 Cd1 Cl1 176.59(7) . . ? N7 Cd1 Cl3 88.59(15) . . ? Cl4 Cd1 Cl3 84.71(6) . . ? Cl1 Cd1 Cl3 92.13(7) . . ? N7 Cd1 Cl5 89.39(16) . 2_666 ? Cl4 Cd1 Cl5 85.47(6) . 2_666 ? Cl1 Cd1 Cl5 97.73(7) . 2_666 ? Cl3 Cd1 Cl5 169.95(6) . 2_666 ? N7 Cd1 Cl2 173.09(15) . . ? Cl4 Cd1 Cl2 95.23(6) . . ? Cl1 Cd1 Cl2 83.74(6) . . ? Cl3 Cd1 Cl2 95.26(6) . . ? Cl5 Cd1 Cl2 87.79(6) 2_666 . ? N8 Cd2 O5 94.0(3) . . ? N8 Cd2 Cl5 98.16(16) . . ? O5 Cd2 Cl5 86.4(2) . . ? N8 Cd2 Cl1 88.03(16) . . ? O5 Cd2 Cl1 89.6(2) . . ? Cl5 Cd2 Cl1 172.83(6) . . ? N8 Cd2 Cl2 164.12(17) . . ? O5 Cd2 Cl2 100.26(19) . . ? Cl5 Cd2 Cl2 89.73(6) . . ? Cl1 Cd2 Cl2 85.15(6) . . ? N8 Cd2 Cl2 80.41(17) . 2_666 ? O5 Cd2 Cl2 170.9(2) . 2_666 ? Cl5 Cd2 Cl2 87.34(6) . 2_666 ? Cl1 Cd2 Cl2 97.30(7) . 2_666 ? Cl2 Cd2 Cl2 86.24(6) . 2_666 ? N6 Cd3 N14 82.1(2) 1_545 . ? N6 Cd3 Cl6 171.09(14) 1_545 2_667 ? N14 Cd3 Cl6 92.35(15) . 2_667 ? N6 Cd3 Cl4 90.06(15) 1_545 . ? N14 Cd3 Cl4 84.09(15) . . ? Cl6 Cd3 Cl4 96.33(6) 2_667 . ? N6 Cd3 Cl6 89.03(15) 1_545 . ? N14 Cd3 Cl6 91.90(15) . . ? Cl6 Cd3 Cl6 84.17(6) 2_667 . ? Cl4 Cd3 Cl6 175.97(5) . . ? N6 Cd3 Cl3 86.84(15) 1_545 . ? N14 Cd3 Cl3 163.63(14) . . ? Cl6 Cd3 Cl3 99.97(6) 2_667 . ? Cl4 Cd3 Cl3 83.89(6) . . ? Cl6 Cd3 Cl3 99.97(6) . . ? Cd2 Cl1 Cd1 96.08(6) . . ? Cd2 Cl2 Cd1 93.87(6) . . ? Cd2 Cl2 Cd2 93.76(6) . 2_666 ? Cd1 Cl2 Cd2 89.31(6) . 2_666 ? Cd1 Cl3 Cd3 93.48(6) . . ? Cd1 Cl4 Cd3 95.56(6) . . ? Cd2 Cl5 Cd1 95.29(6) . 2_666 ? Cd3 Cl6 Cd3 95.83(5) 2_667 . ? N3 P1 N1 114.8(4) . . ? N3 P1 O1 111.7(4) . . ? N1 P1 O1 113.0(4) . . ? N3 P1 O2 112.3(4) . . ? N1 P1 O2 111.4(4) . . ? O1 P1 O2 91.6(3) . . ? N9 P2 N11 114.4(4) . . ? N9 P2 O4 112.6(3) . . ? N11 P2 O4 110.9(3) . . ? N9 P2 O3 111.2(3) . . ? N11 P2 O3 112.1(3) . . ? O4 P2 O3 94.0(3) . . ? C7 O1 P1 124.9(5) . . ? C12 O2 P1 119.2(5) . . ? C19 O3 P2 119.0(5) . . ? C22 O4 P2 115.7(5) . . ? C2 N1 P1 114.0(6) . . ? C2 N2 C1 119.3(8) . . ? C1 N3 P1 115.7(6) . . ? C2 N4 C6 123.0(8) . . ? C2 N4 C5 121.7(9) . . ? C6 N4 C5 115.2(8) . . ? C1 N5 C4 120.8(10) . . ? C1 N5 C3 119.1(10) . . ? C4 N5 C3 120.0(10) . . ? C9 N6 C10 117.0(6) . . ? C9 N6 Cd3 121.4(5) . 1_565 ? C10 N6 Cd3 121.6(5) . 1_565 ? C15 N7 C14 117.8(6) . . ? C15 N7 Cd1 122.3(5) . . ? C14 N7 Cd1 119.6(5) . . ? C17 N8 C21 117.5(7) . . ? C17 N8 Cd2 118.2(5) . . ? C21 N8 Cd2 124.0(6) . . ? C25 N9 P2 114.9(6) . . ? C25 N10 C26 119.8(8) . . ? C26 N11 P2 115.6(6) . . ? C25 N12 C27 121.4(8) . . ? C25 N12 C28 119.6(8) . . ? C27 N12 C28 118.5(8) . . ? C26 N13 C29 120.3(8) . . ? C26 N13 C30 121.0(9) . . ? C29 N13 C30 118.2(9) . . ? C31 N14 C32 118.0(6) . . ? C31 N14 Cd3 119.4(5) . . ? C32 N14 Cd3 122.5(5) . . ? N2 C1 N5 116.9(9) . . ? N2 C1 N3 127.0(9) . . ? N5 C1 N3 116.1(9) . . ? N2 C2 N4 115.5(8) . . ? N2 C2 N1 129.0(8) . . ? N4 C2 N1 115.4(8) . . ? C11 C7 C8 119.1(6) . . ? C11 C7 O1 115.8(6) . . ? C8 C7 O1 124.9(7) . . ? C9 C8 C7 117.5(7) . . ? N6 C9 C8 124.3(7) . . ? N6 C10 C11 123.5(7) . . ? C7 C11 C10 118.5(7) . . ? C13 C12 C16 121.0(7) . . ? C13 C12 O2 121.2(8) . . ? C16 C12 O2 117.6(7) . . ? C12 C13 C14 116.7(8) . . ? N7 C14 C13 123.5(8) . . ? N7 C15 C16 123.3(8) . . ? C15 C16 C12 117.7(7) . . ? N8 C17 C18 123.1(8) . . ? C19 C18 C17 119.1(8) . . ? C18 C19 C20 119.1(7) . . ? C18 C19 O3 117.9(7) . . ? C20 C19 O3 122.9(7) . . ? C19 C20 C21 117.0(7) . . ? N8 C21 C20 124.1(8) . . ? C24 C22 C23 121.6(7) . . ? C24 C22 O4 118.6(6) . . ? C23 C22 O4 119.7(6) . . ? C22 C23 C32 116.8(6) . 1_464 ? C22 C24 C31 117.3(6) . 1_464 ? N10 C25 N9 128.1(7) . . ? N10 C25 N12 116.7(8) . . ? N9 C25 N12 115.2(8) . . ? N10 C26 N11 127.1(8) . . ? N10 C26 N13 117.5(8) . . ? N11 C26 N13 115.5(8) . . ? N14 C31 C24 123.3(7) . 1_646 ? N14 C32 C23 123.0(6) . 1_646 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 3.275 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.240 #===end data_Complex-2 _database_code_depnum_ccdc_archive 'CCDC 727816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 Cd2 Cl4 N14 O4 P2, C H Cl3, 4(H2O)' _chemical_formula_sum 'C33 H49 Cd2 Cl7 N14 O8 P2' _chemical_formula_weight 1303.92 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' P P 0.1023 0.0942 '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 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.957 _cell_length_b 25.704 _cell_length_c 15.827 _cell_angle_alpha 90.000 _cell_angle_beta 93.362 _cell_angle_gamma 90.000 _cell_volume 5668(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3623 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 24.50 _exptl_crystal_description 'needle shape' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8055 _exptl_absorpt_correction_T_max 0.9150 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33910 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12305 _reflns_number_gt 5800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1707P)^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 12305 _refine_ls_number_parameters 570 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1538 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.3149 _refine_ls_wR_factor_gt 0.2490 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.037 _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 0.12721(4) 0.96540(2) 1.00422(4) 0.0362(2) Uani 1 1 d . . . Cd2 Cd 0.37534(4) 1.03140(2) 1.00595(4) 0.0373(2) Uani 1 1 d . . . Cl6 Cl 0.9398(5) -0.06233(18) 0.6865(4) 0.190(2) Uani 1 1 d . . . Cl5 Cl 0.8575(7) 0.0400(3) 0.6774(5) 0.275(5) Uani 1 1 d D . . Cl7 Cl 1.0684(8) 0.0206(3) 0.6615(8) 0.348(6) Uani 1 1 d . . . Cl2 Cl 0.28340(16) 0.95974(8) 0.92106(16) 0.0481(6) Uani 1 1 d . . . Cl3 Cl 0.23173(16) 1.03077(7) 1.10567(14) 0.0438(5) Uani 1 1 d . . . Cl1 Cl 0.03503(16) 1.03488(7) 0.91294(15) 0.0440(5) Uani 1 1 d . . . Cl4 Cl 0.48842(15) 0.97232(8) 1.10633(14) 0.0439(5) Uani 1 1 d . . . P1 P -0.09078(17) 0.75931(9) 0.69644(17) 0.0503(7) Uani 1 1 d . . . P2 P 0.33487(19) 0.73568(10) 1.2454(2) 0.0650(8) Uani 1 1 d D . . O5 O 0.5459(8) 0.9091(4) 0.3406(6) 0.149(4) Uani 1 1 d . . . O6 O 0.7167(15) 0.7549(10) 0.8680(13) 0.360(14) Uani 1 1 d . . . O7 O 0.3445(15) 0.0122(7) 0.6545(8) 0.248(9) Uani 1 1 d . . . O8 O 0.5802(15) 0.0176(6) 0.6448(13) 0.300(12) Uani 1 1 d . . . O2 O -0.0357(4) 0.7643(2) 0.7878(4) 0.0559(17) Uani 1 1 d . . . O3 O 0.1189(4) 1.2002(2) 0.7839(4) 0.0558(17) Uani 1 1 d . . . O4 O 0.6460(5) 1.2180(2) 1.1586(5) 0.083(2) Uani 1 1 d . . . O1 O 0.2761(5) 0.7842(2) 1.2705(5) 0.078(2) Uani 1 1 d . . . N7 N 0.0645(5) 0.8969(3) 0.9124(5) 0.0477(19) Uani 1 1 d . . . N6 N 0.1811(5) 0.8982(2) 1.0989(5) 0.0464(19) Uani 1 1 d . . . N14 N 0.4645(5) 1.1023(3) 1.0649(5) 0.053(2) Uani 1 1 d . . . N13 N 0.2847(5) 1.0962(2) 0.9266(5) 0.0437(18) Uani 1 1 d . . . N11 N -0.2563(8) 0.8626(4) 0.6128(8) 0.094(3) Uani 1 1 d D . . N12 N 0.0110(8) 0.7997(4) 0.4972(6) 0.083(3) Uani 1 1 d D . . N4 N 0.2530(13) 0.6354(6) 1.0826(8) 0.139(6) Uani 1 1 d D . . N5 N 0.5228(11) 0.7377(6) 1.0912(10) 0.186(7) Uiso 1 1 d D . . N10 N -0.0218(5) 0.7630(3) 0.6212(5) 0.056(2) Uani 1 1 d . . . N8 N -0.1803(5) 0.7958(3) 0.6880(5) 0.060(2) Uani 1 1 d . . . N9 N -0.1263(8) 0.8285(3) 0.5565(6) 0.078(3) Uani 1 1 d . . . N1 N 0.2729(5) 0.6949(3) 1.1925(6) 0.068(2) Uani 1 1 d D . . N3 N 0.4327(6) 0.7511(3) 1.2016(8) 0.107(5) Uani 1 1 d D . . N2 N 0.3935(9) 0.6897(4) 1.0863(7) 0.107(4) Uiso 1 1 d D . . C5 C 0.5827(13) 0.7737(7) 1.1320(12) 0.216(10) Uiso 1 1 d D . . H5A H 0.6353 0.7813 1.0976 0.325 Uiso 1 1 calc R . . H5B H 0.6070 0.7598 1.1853 0.325 Uiso 1 1 calc R . . H5C H 0.5475 0.8050 1.1415 0.325 Uiso 1 1 calc R . . C6 C 0.5379(14) 0.7151(8) 1.0139(11) 0.222(10) Uiso 1 1 d D . . H6A H 0.5920 0.7313 0.9899 0.332 Uiso 1 1 calc R . . H6B H 0.4819 0.7197 0.9765 0.332 Uiso 1 1 calc R . . H6C H 0.5503 0.6786 1.0216 0.332 Uiso 1 1 calc R . . C10 C 0.2690(7) 0.8962(4) 1.1258(8) 0.076(4) Uani 1 1 d . . . H10 H 0.3121 0.9199 1.1049 0.091 Uiso 1 1 calc R . . C25 C 0.1738(6) 1.1670(3) 0.8359(6) 0.044(2) Uani 1 1 d . . . C31 C 0.5717(7) 1.1709(3) 1.0449(6) 0.058(3) Uani 1 1 d . . . H31 H 0.6034 1.1922 1.0081 0.070 Uiso 1 1 calc R . . C14 C -0.0038(6) 0.8122(3) 0.8221(5) 0.045(2) Uani 1 1 d . . . C27 C 0.2480(6) 1.1360(3) 0.9627(6) 0.048(2) Uani 1 1 d . . . H27 H 0.2606 1.1400 1.0207 0.057 Uiso 1 1 calc R . . C23 C 0.2632(7) 1.0906(4) 0.8451(6) 0.063(3) Uani 1 1 d . . . H23 H 0.2866 1.0616 0.8179 0.076 Uiso 1 1 calc R . . C13 C 0.0887(7) 0.8255(3) 0.8203(7) 0.068(3) Uani 1 1 d . . . H13 H 0.1302 0.8062 0.7887 0.082 Uiso 1 1 calc R . . C7 C 0.2445(7) 0.8225(3) 1.2109(7) 0.059(3) Uani 1 1 d . . . C29 C 0.5391(9) 1.1448(4) 1.1851(7) 0.078(3) Uani 1 1 d . . . H29 H 0.5468 1.1474 1.2437 0.094 Uiso 1 1 calc R . . C24 C 0.2092(7) 1.1248(4) 0.7993(7) 0.067(3) Uani 1 1 d . . . H24 H 0.1963 1.1191 0.7418 0.080 Uiso 1 1 calc R . . C8 C 0.1511(7) 0.8221(4) 1.1799(8) 0.078(4) Uani 1 1 d . . . H8 H 0.1081 0.7967 1.1956 0.094 Uiso 1 1 calc R . . C32 C 0.5123(7) 1.1335(3) 1.0151(7) 0.057(3) Uani 1 1 d . . . H32 H 0.5040 1.1291 0.9568 0.069 Uiso 1 1 calc R . . C15 C -0.0666(7) 0.8412(4) 0.8656(7) 0.066(3) Uani 1 1 d . . . H15 H -0.1314 0.8328 0.8654 0.079 Uiso 1 1 calc R . . C16 C -0.0285(6) 0.8841(4) 0.9104(7) 0.061(3) Uani 1 1 d . . . H16 H -0.0698 0.9046 0.9401 0.073 Uiso 1 1 calc R . . C17 C -0.1851(8) 0.8280(4) 0.6204(9) 0.069(3) Uani 1 1 d . . . C18 C -0.0482(8) 0.7980(4) 0.5596(6) 0.061(3) Uani 1 1 d D . . C30 C 0.5856(7) 1.1776(3) 1.1339(7) 0.060(3) Uani 1 1 d . . . C12 C 0.1213(7) 0.8677(4) 0.8654(7) 0.068(3) Uani 1 1 d . . . H12 H 0.1856 0.8768 0.8636 0.082 Uiso 1 1 calc R . . C26 C 0.1911(6) 1.1733(3) 0.9208(6) 0.052(2) Uani 1 1 d . . . H26 H 0.1659 1.2013 0.9493 0.063 Uiso 1 1 calc R . . C11 C 0.3034(7) 0.8588(4) 1.1873(8) 0.083(4) Uani 1 1 d . . . H11 H 0.3663 0.8602 1.2101 0.100 Uiso 1 1 calc R . . C9 C 0.1238(7) 0.8617(4) 1.1239(7) 0.070(3) Uani 1 1 d . . . H9 H 0.0603 0.8623 1.1026 0.084 Uiso 1 1 calc R . . C28 C 0.4804(7) 1.1080(4) 1.1470(7) 0.063(3) Uani 1 1 d . . . H28 H 0.4494 1.0852 1.1819 0.075 Uiso 1 1 calc R . . C21 C -0.3191(11) 0.8683(5) 0.6824(10) 0.127(6) Uani 1 1 d D . . H21A H -0.3659 0.8949 0.6688 0.191 Uiso 1 1 calc R . . H21B H -0.2817 0.8780 0.7329 0.191 Uiso 1 1 calc R . . H21C H -0.3512 0.8360 0.6916 0.191 Uiso 1 1 calc R . . C22 C -0.2667(11) 0.8996(5) 0.5447(10) 0.121(5) Uani 1 1 d . . . H22A H -0.3215 0.9213 0.5525 0.182 Uiso 1 1 calc R . . H22B H -0.2753 0.8815 0.4918 0.182 Uiso 1 1 calc R . . H22C H -0.2101 0.9209 0.5444 0.182 Uiso 1 1 calc R . . C19 C 0.0962(10) 0.7691(5) 0.4938(8) 0.098(4) Uani 1 1 d D . . H19A H 0.1278 0.7774 0.4433 0.147 Uiso 1 1 calc R . . H19B H 0.0795 0.7329 0.4934 0.147 Uiso 1 1 calc R . . H19C H 0.1383 0.7765 0.5425 0.147 Uiso 1 1 calc R . . C20 C -0.0011(13) 0.8384(5) 0.4296(8) 0.141(7) Uani 1 1 d . . . H20A H 0.0486 0.8341 0.3908 0.211 Uiso 1 1 calc R . . H20B H 0.0026 0.8727 0.4536 0.211 Uiso 1 1 calc R . . H20C H -0.0626 0.8337 0.4001 0.211 Uiso 1 1 calc R . . C33 C 0.9454(16) 0.0015(7) 0.7127(12) 0.268(17) Uani 1 1 d D . . H33 H 0.9536 0.0048 0.7744 0.322 Uiso 1 1 calc R . . C1 C 0.3096(10) 0.6749(6) 1.1189(9) 0.094(4) Uani 1 1 d . . . C2 C 0.4388(10) 0.7243(6) 1.1300(8) 0.109(5) Uiso 1 1 d D . . C4 C 0.2860(16) 0.6138(9) 1.0035(11) 0.251(15) Uani 1 1 d D . . H4A H 0.2415 0.5878 0.9822 0.376 Uiso 1 1 calc R . . H4B H 0.3482 0.5984 1.0140 0.376 Uiso 1 1 calc R . . H4C H 0.2899 0.6412 0.9625 0.376 Uiso 1 1 calc R . . C3 C 0.1666(15) 0.6160(8) 1.1162(14) 0.187(10) Uani 1 1 d D . . H3A H 0.1383 0.5902 1.0786 0.281 Uiso 1 1 calc R . . H3B H 0.1222 0.6442 1.1217 0.281 Uiso 1 1 calc R . . H3C H 0.1814 0.6007 1.1707 0.281 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 0.0280(4) 0.0264(3) 0.0530(4) 0.0003(3) -0.0085(3) 0.0011(2) Cd2 0.0274(4) 0.0268(3) 0.0560(5) -0.0005(3) -0.0110(3) -0.0002(2) Cl6 0.229(6) 0.105(3) 0.233(6) 0.018(4) -0.019(5) -0.024(4) Cl5 0.414(13) 0.198(7) 0.214(8) 0.052(5) 0.023(8) 0.139(8) Cl7 0.350(12) 0.211(8) 0.492(17) -0.043(9) 0.087(11) -0.129(8) Cl2 0.0365(12) 0.0388(11) 0.0687(16) -0.0158(10) -0.0001(11) -0.0081(9) Cl3 0.0389(12) 0.0404(11) 0.0515(13) -0.0049(9) -0.0027(10) -0.0012(9) Cl1 0.0388(12) 0.0392(11) 0.0536(13) 0.0074(9) -0.0003(10) 0.0081(9) Cl4 0.0332(11) 0.0440(11) 0.0536(13) 0.0037(10) -0.0059(10) 0.0022(9) P1 0.0487(14) 0.0376(12) 0.0629(17) -0.0107(11) -0.0101(12) -0.0108(11) P2 0.0522(16) 0.0466(14) 0.093(2) 0.0294(14) -0.0197(15) 0.0034(12) O5 0.156(9) 0.190(10) 0.098(7) 0.059(7) -0.025(6) 0.086(8) O6 0.30(3) 0.53(4) 0.27(2) -0.12(2) 0.21(2) -0.03(2) O7 0.36(2) 0.270(18) 0.109(10) -0.057(11) 0.012(12) -0.140(17) O8 0.38(2) 0.195(14) 0.36(2) 0.078(15) 0.28(2) 0.152(16) O2 0.057(4) 0.042(3) 0.067(4) -0.013(3) -0.014(3) -0.012(3) O3 0.060(4) 0.048(3) 0.058(4) 0.012(3) -0.013(3) 0.016(3) O4 0.102(6) 0.057(4) 0.085(5) -0.019(4) -0.036(4) -0.030(4) O1 0.100(6) 0.039(3) 0.092(6) 0.023(3) -0.031(5) 0.012(3) N7 0.040(4) 0.037(4) 0.065(5) -0.014(4) -0.009(4) -0.001(3) N6 0.031(4) 0.031(3) 0.075(5) 0.020(3) -0.013(4) -0.004(3) N14 0.052(5) 0.033(4) 0.070(6) -0.009(4) -0.017(4) -0.002(3) N13 0.042(4) 0.028(3) 0.059(5) 0.004(3) -0.009(4) 0.007(3) N11 0.084(7) 0.074(7) 0.121(10) -0.013(7) -0.017(7) 0.029(6) N12 0.112(8) 0.069(6) 0.068(7) 0.001(5) 0.010(6) -0.019(6) N4 0.181(15) 0.113(11) 0.116(12) -0.050(9) -0.052(11) 0.063(11) N10 0.057(5) 0.051(4) 0.060(5) 0.002(4) 0.002(4) 0.000(4) N8 0.051(5) 0.056(5) 0.073(6) -0.009(4) -0.011(4) 0.010(4) N9 0.082(7) 0.067(6) 0.082(7) 0.007(5) -0.008(6) 0.013(5) N1 0.045(5) 0.065(5) 0.092(7) 0.021(5) -0.006(5) 0.005(4) N3 0.043(5) 0.070(6) 0.202(13) 0.081(8) -0.039(6) -0.007(4) C10 0.039(6) 0.063(6) 0.123(10) 0.044(6) -0.026(6) -0.004(5) C25 0.038(5) 0.028(4) 0.063(6) 0.002(4) -0.013(4) 0.007(4) C31 0.075(7) 0.038(5) 0.060(6) 0.001(5) -0.013(5) -0.014(5) C14 0.055(6) 0.035(4) 0.045(5) -0.013(4) -0.005(4) -0.011(4) C27 0.045(5) 0.048(5) 0.049(6) 0.008(4) -0.008(4) 0.012(4) C23 0.083(7) 0.055(6) 0.051(6) 0.005(5) -0.006(5) 0.029(5) C13 0.045(6) 0.055(6) 0.106(9) -0.047(6) 0.020(6) -0.016(5) C7 0.051(6) 0.041(5) 0.082(7) 0.015(5) -0.014(5) 0.006(4) C29 0.106(9) 0.060(7) 0.067(7) -0.021(6) -0.001(7) -0.030(6) C24 0.079(7) 0.053(6) 0.066(7) 0.005(5) -0.015(6) 0.031(5) C8 0.041(6) 0.062(6) 0.129(10) 0.052(6) -0.014(6) -0.007(5) C32 0.061(6) 0.040(5) 0.068(7) 0.000(5) -0.021(5) -0.005(4) C15 0.036(5) 0.060(6) 0.099(9) -0.031(6) -0.015(5) 0.003(5) C16 0.035(5) 0.058(6) 0.091(8) -0.034(6) 0.000(5) -0.003(4) C17 0.056(7) 0.057(6) 0.091(9) -0.022(6) -0.017(6) 0.004(5) C18 0.083(8) 0.052(6) 0.048(6) -0.009(5) 0.002(6) -0.024(6) C30 0.060(6) 0.029(4) 0.088(8) -0.010(5) -0.017(6) -0.008(4) C12 0.037(5) 0.063(6) 0.105(9) -0.037(6) 0.013(5) -0.005(5) C26 0.053(6) 0.038(5) 0.066(7) -0.003(4) -0.004(5) 0.011(4) C11 0.041(6) 0.068(7) 0.135(11) 0.028(7) -0.035(6) -0.003(5) C9 0.046(6) 0.056(6) 0.105(9) 0.036(6) -0.022(6) -0.005(5) C28 0.065(7) 0.050(6) 0.071(8) -0.006(5) -0.008(6) -0.016(5) C21 0.114(12) 0.085(10) 0.180(17) -0.035(10) -0.004(12) 0.030(9) C22 0.146(14) 0.091(10) 0.121(13) 0.017(9) -0.038(10) 0.023(9) C19 0.111(10) 0.094(9) 0.092(10) -0.020(7) 0.033(8) -0.001(8) C20 0.25(2) 0.098(10) 0.073(10) 0.014(8) 0.017(11) -0.039(12) C33 0.53(5) 0.18(2) 0.094(15) -0.018(14) 0.00(2) -0.19(3) C1 0.089(10) 0.107(11) 0.084(10) 0.018(9) -0.012(8) 0.043(9) C4 0.31(3) 0.26(3) 0.17(2) -0.12(2) -0.10(2) 0.17(2) C3 0.16(2) 0.137(16) 0.26(3) -0.019(16) -0.042(19) -0.049(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 Cd1 N6 2.380(6) . ? Cd1 N7 2.414(7) . ? Cd1 Cl1 2.591(2) . ? Cd1 Cl2 2.616(3) . ? Cd1 Cl1 2.682(2) 3_577 ? Cd1 Cl3 2.693(2) . ? Cd2 N14 2.367(7) . ? Cd2 N13 2.401(6) . ? Cd2 Cl2 2.577(2) . ? Cd2 Cl3 2.623(3) . ? Cd2 Cl4 2.651(2) . ? Cd2 Cl4 2.679(2) 3_677 ? Cl6 C33 1.693(17) . ? Cl5 C33 1.648(18) . ? Cl7 C33 2.00(2) . ? Cl1 Cd1 2.682(2) 3_577 ? Cl4 Cd2 2.679(2) 3_677 ? P1 N8 1.563(8) . ? P1 N10 1.578(8) . ? P1 O2 1.602(6) . ? P1 O3 1.605(6) 2_546 ? P2 O1 1.557(7) . ? P2 N1 1.570(8) . ? P2 O4 1.594(7) 2_647 ? P2 N3 1.616(9) . ? O2 C14 1.407(9) . ? O3 C25 1.385(9) . ? O3 P1 1.605(6) 2_556 ? O4 C30 1.380(10) . ? O4 P2 1.594(7) 2_657 ? O1 C7 1.416(10) . ? N7 C16 1.339(10) . ? N7 C12 1.346(11) . ? N6 C10 1.276(10) . ? N6 C9 1.309(11) . ? N14 C28 1.313(12) . ? N14 C32 1.331(12) . ? N13 C27 1.294(10) . ? N13 C23 1.314(11) . ? N11 C17 1.333(13) . ? N11 C22 1.440(15) . ? N11 C21 1.455(13) . ? N12 C18 1.326(11) . ? N12 C19 1.428(12) . ? N12 C20 1.462(14) . ? N4 C1 1.389(19) . ? N4 C3 1.436(15) . ? N4 C4 1.468(12) . ? N5 C6 1.381(12) . ? N5 C5 1.383(12) . ? N5 C2 1.398(11) . ? N10 C18 1.362(12) . ? N8 C17 1.351(14) . ? N9 C17 1.340(14) . ? N9 C18 1.341(13) . ? N1 C1 1.398(15) . ? N3 C2 1.334(9) . ? N2 C2 1.272(10) . ? N2 C1 1.361(16) . ? C10 C11 1.432(13) . ? C25 C24 1.337(12) . ? C25 C26 1.361(12) . ? C31 C32 1.338(11) . ? C31 C30 1.421(13) . ? C14 C13 1.337(12) . ? C14 C15 1.366(12) . ? C27 C26 1.388(11) . ? C23 C24 1.342(12) . ? C13 C12 1.362(11) . ? C7 C11 1.310(13) . ? C7 C8 1.366(12) . ? C29 C30 1.359(14) . ? C29 C28 1.369(12) . ? C8 C9 1.387(12) . ? C15 C16 1.399(12) . ? 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 N6 Cd1 N7 86.5(3) . . ? N6 Cd1 Cl1 168.43(18) . . ? N7 Cd1 Cl1 90.97(18) . . ? N6 Cd1 Cl2 91.97(19) . . ? N7 Cd1 Cl2 86.55(19) . . ? Cl1 Cd1 Cl2 99.15(8) . . ? N6 Cd1 Cl1 86.28(19) . 3_577 ? N7 Cd1 Cl1 90.32(19) . 3_577 ? Cl1 Cd1 Cl1 82.45(8) . 3_577 ? Cl2 Cd1 Cl1 176.51(7) . 3_577 ? N6 Cd1 Cl3 86.42(17) . . ? N7 Cd1 Cl3 168.03(18) . . ? Cl1 Cd1 Cl3 97.83(7) . . ? Cl2 Cd1 Cl3 84.05(7) . . ? Cl1 Cd1 Cl3 98.84(7) 3_577 . ? N14 Cd2 N13 85.4(3) . . ? N14 Cd2 Cl2 171.8(2) . . ? N13 Cd2 Cl2 89.55(18) . . ? N14 Cd2 Cl3 99.8(2) . . ? N13 Cd2 Cl3 85.50(19) . . ? Cl2 Cd2 Cl3 86.25(7) . . ? N14 Cd2 Cl4 85.67(18) . . ? N13 Cd2 Cl4 171.03(17) . . ? Cl2 Cd2 Cl4 99.42(7) . . ? Cl3 Cd2 Cl4 94.88(7) . . ? N14 Cd2 Cl4 84.9(2) . 3_677 ? N13 Cd2 Cl4 92.88(19) . 3_677 ? Cl2 Cd2 Cl4 88.84(7) . 3_677 ? Cl3 Cd2 Cl4 174.84(6) . 3_677 ? Cl4 Cd2 Cl4 87.49(8) . 3_677 ? Cd2 Cl2 Cd1 95.86(8) . . ? Cd2 Cl3 Cd1 92.95(7) . . ? Cd1 Cl1 Cd1 97.55(8) . 3_577 ? Cd2 Cl4 Cd2 92.51(7) . 3_677 ? N8 P1 N10 114.8(5) . . ? N8 P1 O2 111.5(4) . . ? N10 P1 O2 113.3(4) . . ? N8 P1 O3 112.4(4) . 2_546 ? N10 P1 O3 111.7(4) . 2_546 ? O2 P1 O3 90.6(3) . 2_546 ? O1 P2 N1 112.9(4) . . ? O1 P2 O4 92.6(4) . 2_647 ? N1 P2 O4 112.0(4) . 2_647 ? O1 P2 N3 112.5(5) . . ? N1 P2 N3 112.9(6) . . ? O4 P2 N3 112.3(5) 2_647 . ? C14 O2 P1 122.9(5) . . ? C25 O3 P1 127.0(5) . 2_556 ? C30 O4 P2 123.3(7) . 2_657 ? C7 O1 P2 122.4(7) . . ? C16 N7 C12 116.8(7) . . ? C16 N7 Cd1 120.7(6) . . ? C12 N7 Cd1 122.3(6) . . ? C10 N6 C9 117.6(8) . . ? C10 N6 Cd1 120.0(6) . . ? C9 N6 Cd1 122.3(5) . . ? C28 N14 C32 117.2(8) . . ? C28 N14 Cd2 122.0(7) . . ? C32 N14 Cd2 120.0(6) . . ? C27 N13 C23 116.5(7) . . ? C27 N13 Cd2 121.9(6) . . ? C23 N13 Cd2 121.4(6) . . ? C17 N11 C22 123.4(13) . . ? C17 N11 C21 118.6(12) . . ? C22 N11 C21 117.5(11) . . ? C18 N12 C19 124.4(10) . . ? C18 N12 C20 121.1(12) . . ? C19 N12 C20 114.1(11) . . ? C1 N4 C3 124.8(14) . . ? C1 N4 C4 115.4(19) . . ? C3 N4 C4 119.8(19) . . ? C6 N5 C5 125.1(11) . . ? C6 N5 C2 117.5(10) . . ? C5 N5 C2 117.4(10) . . ? C18 N10 P1 115.4(7) . . ? C17 N8 P1 116.0(8) . . ? C17 N9 C18 120.0(10) . . ? C1 N1 P2 118.2(9) . . ? C2 N3 P2 109.5(8) . . ? C2 N2 C1 113.7(14) . . ? N6 C10 C11 122.0(9) . . ? C24 C25 C26 118.4(8) . . ? C24 C25 O3 116.6(8) . . ? C26 C25 O3 124.9(8) . . ? C32 C31 C30 118.9(9) . . ? C13 C14 C15 121.3(8) . . ? C13 C14 O2 120.0(8) . . ? C15 C14 O2 118.2(8) . . ? N13 C27 C26 124.4(8) . . ? N13 C23 C24 123.2(9) . . ? C14 C13 C12 119.1(9) . . ? C11 C7 C8 120.3(9) . . ? C11 C7 O1 120.6(8) . . ? C8 C7 O1 119.1(9) . . ? C30 C29 C28 117.4(10) . . ? C25 C24 C23 120.5(10) . . ? C7 C8 C9 116.4(9) . . ? N14 C32 C31 123.1(10) . . ? C14 C15 C16 116.7(9) . . ? N7 C16 C15 123.1(9) . . ? N11 C17 N9 114.3(12) . . ? N11 C17 N8 118.8(12) . . ? N9 C17 N8 126.8(10) . . ? N12 C18 N9 119.6(11) . . ? N12 C18 N10 113.6(10) . . ? N9 C18 N10 126.7(10) . . ? C29 C30 O4 127.1(10) . . ? C29 C30 C31 118.3(8) . . ? O4 C30 C31 114.6(9) . . ? N7 C12 C13 122.9(8) . . ? C25 C26 C27 116.9(8) . . ? C7 C11 C10 118.8(9) . . ? N6 C9 C8 124.6(8) . . ? N14 C28 C29 125.1(10) . . ? Cl5 C33 Cl6 118.4(12) . . ? Cl5 C33 Cl7 110.7(11) . . ? Cl6 C33 Cl7 99.6(11) . . ? N2 C1 N4 121.9(15) . . ? N2 C1 N1 125.3(14) . . ? N4 C1 N1 112.7(13) . . ? N2 C2 N3 140.3(14) . . ? N2 C2 N5 109.6(12) . . ? N3 C2 N5 110.1(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.128 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.202 #===END