data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 Cd N9, C9 H22 P' _chemical_formula_sum 'C15 H22 Cd N9 P' _chemical_formula_weight 471.79 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' 'Cd' 'Cd' -0.8075 1.2024 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/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 10.498(8) _cell_length_b 16.500(3) _cell_length_c 15.763(9) _cell_angle_alpha 90.00 _cell_angle_beta 128.040(2) _cell_angle_gamma 90.00 _cell_volume 2150(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2800 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7927 _exptl_absorpt_correction_T_max 0.8089 _exptl_absorpt_process_details ? _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 'Saturn724+ (4x4 bin mode)' _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7807 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3049 _reflns_number_gt 2800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1318P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.061(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3049 _refine_ls_number_parameters 230 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.14553 _refine_ls_R_factor_gt 0.13489 _refine_ls_wR_factor_ref 0.3447 _refine_ls_wR_factor_gt 0.3423 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.00 _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 C5 C 0.5248(13) 0.6464(8) 0.6763(9) 0.0480(19) Uani 1 1 d U . . Cd1 Cd 0.56481(11) 0.82341(5) 0.80771(6) 0.0378(3) Uani 1 1 d U . . N9 N 0.4052(3) 0.44502(8) 0.6107(4) 0.050(2) Uani 1 1 d DU . . N7 N 0.5260(13) 0.7051(7) 0.7168(9) 0.0563(19) Uani 1 1 d U . . N8 N 0.5060(11) 0.5792(7) 0.6165(8) 0.0510(19) Uani 1 1 d U . . C6 C 0.4513(3) 0.51316(10) 0.6148(5) 0.050(2) Uani 1 1 d DU . . N4 N 0.8469(12) 0.8006(10) 0.9201(9) 0.065(2) Uani 1 1 d U . . C3 C 0.9493(15) 0.7610(13) 0.9606(11) 0.066(2) Uani 1 1 d U . . N1 N 0.5190(12) 0.7493(10) 0.9151(8) 0.0584(15) Uani 1 1 d U . . N2 N 0.4375(11) 0.6487(10) 0.9846(8) 0.0564(16) Uani 1 1 d U . . C1 C 0.4918(14) 0.7067(12) 0.9565(10) 0.0559(16) Uani 1 1 d U . . N6 N 1.2818(14) 0.6530(11) 1.1794(10) 0.072(3) Uani 1 1 d U . . N5 N 1.0736(13) 0.7138(11) 0.9846(10) 0.070(2) Uani 1 1 d U . . C4 C 1.1885(17) 0.6814(14) 1.1012(13) 0.073(2) Uani 1 1 d U . . N3 N 0.5790(12) 0.6109(10) 1.1776(8) 0.061(2) Uani 1 1 d U . . C2 C 0.5130(15) 0.6307(12) 1.0890(10) 0.0589(19) Uani 1 1 d U . . P1 P 0.9998(3) 0.4787(2) 1.2622(2) 0.0347(8) Uani 1 1 d U . . C13 C 0.8374(16) 0.5180(10) 1.1268(10) 0.0562(18) Uani 1 1 d U . . H13A H 0.7384 0.4870 1.0968 0.067 Uiso 1 1 calc R . . H13B H 0.8159 0.5746 1.1331 0.067 Uiso 1 1 calc R . . C9 C 1.0615(13) 0.3752(2) 1.24096(19) 0.0436(19) Uani 1 1 d DU . . H9A H 0.9643 0.3454 1.1839 0.052 Uiso 1 1 calc R . . H9B H 1.1283 0.3837 1.2178 0.052 Uiso 1 1 calc R . . C7 C 1.1758(14) 0.5459(10) 1.3280(11) 0.059(2) Uani 1 1 d U . . H7A H 1.2672 0.5206 1.3950 0.071 Uiso 1 1 calc R . . H7B H 1.2061 0.5530 1.2808 0.071 Uiso 1 1 calc R . . C11 C 0.9316(14) 0.4652(13) 1.3496(11) 0.070(2) Uani 1 1 d U . . H11A H 1.0254 0.4475 1.4212 0.084 Uiso 1 1 calc R . . H11B H 0.8994 0.5184 1.3581 0.084 Uiso 1 1 calc R . . C8 C 1.1416(18) 0.6297(10) 1.3539(14) 0.071(4) Uani 1 1 d U . . H8A H 1.2377 0.6632 1.3893 0.106 Uiso 1 1 calc R . . H8B H 1.1124 0.6229 1.4011 0.106 Uiso 1 1 calc R . . H8C H 1.0533 0.6556 1.2876 0.106 Uiso 1 1 calc R . . C12 C 0.7955(16) 0.4070(14) 1.3107(12) 0.078(3) Uani 1 1 d U . . H12A H 0.7722 0.4060 1.3614 0.116 Uiso 1 1 calc R . . H12B H 0.8266 0.3532 1.3049 0.116 Uiso 1 1 calc R . . H12C H 0.7000 0.4242 1.2407 0.116 Uiso 1 1 calc R . . C10 C 1.1554(12) 0.3253(2) 1.3439(2) 0.0436(19) Uani 1 1 d DU . . H10A H 1.1853 0.2737 1.3311 0.065 Uiso 1 1 calc R . . H10B H 1.0886 0.3159 1.3661 0.065 Uiso 1 1 calc R . . H10C H 1.2524 0.3543 1.4002 0.065 Uiso 1 1 calc R . . C15 C 0.742(2) 0.5574(11) 0.9428(13) 0.068(4) Uani 1 1 d U . . H15A H 0.7703 0.5555 0.8947 0.102 Uiso 1 1 calc R . . H15B H 0.7339 0.6135 0.9575 0.102 Uiso 1 1 calc R . . H15C H 0.6394 0.5305 0.9094 0.102 Uiso 1 1 calc R . . C14 C 0.8763(16) 0.5137(10) 1.0509(10) 0.055(2) Uani 1 1 d U . . H14A H 0.8839 0.4569 1.0364 0.066 Uiso 1 1 calc R . . H14B H 0.9811 0.5395 1.0834 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 C5 0.070(2) 0.0355(18) 0.086(2) -0.0065(15) 0.0721(17) 0.004(2) Cd1 0.0483(4) 0.0221(4) 0.0334(3) -0.0006(3) 0.0203(2) 0.0029(4) N9 0.060(3) 0.041(2) 0.084(3) -0.004(3) 0.062(2) -0.002(2) N7 0.078(3) 0.037(2) 0.0875(18) -0.0093(16) 0.0677(15) 0.006(2) N8 0.070(2) 0.0388(18) 0.087(2) -0.0071(15) 0.0697(16) 0.0009(17) C6 0.062(2) 0.0379(18) 0.087(2) -0.008(2) 0.0643(19) 0.0021(19) N4 0.0427(15) 0.101(3) 0.077(3) 0.007(3) 0.0487(15) 0.0081(18) C3 0.0432(17) 0.101(2) 0.076(2) 0.008(2) 0.0477(18) 0.0094(17) N1 0.0421(16) 0.091(3) 0.0573(15) 0.0043(16) 0.0384(10) -0.0075(19) N2 0.0458(19) 0.094(2) 0.0524(15) 0.0051(16) 0.0420(14) -0.0027(18) C1 0.0411(19) 0.092(2) 0.0557(16) 0.0034(15) 0.0405(12) -0.0038(17) N6 0.050(3) 0.103(3) 0.076(3) 0.004(3) 0.045(2) 0.018(3) N5 0.0460(18) 0.104(2) 0.077(2) 0.006(2) 0.0465(18) 0.0134(18) C4 0.048(2) 0.104(3) 0.077(2) 0.006(2) 0.044(2) 0.014(2) N3 0.056(3) 0.100(4) 0.0482(17) -0.002(3) 0.042(2) 0.009(3) C2 0.051(2) 0.096(3) 0.0508(15) 0.0027(19) 0.0419(17) 0.004(2) P1 0.0343(9) 0.0350(14) 0.0478(9) -0.0033(10) 0.0318(6) -0.0007(10) C13 0.052(2) 0.060(3) 0.0549(14) -0.002(2) 0.0318(12) 0.027(2) C9 0.033(2) 0.038(2) 0.077(2) 0.005(2) 0.0423(15) 0.0002(19) C7 0.045(2) 0.062(3) 0.095(4) -0.032(3) 0.0554(17) -0.016(2) C11 0.0590(17) 0.099(5) 0.0954(16) 0.014(3) 0.0699(11) 0.013(2) C8 0.051(4) 0.059(3) 0.105(5) -0.037(3) 0.049(4) -0.015(3) C12 0.066(2) 0.103(6) 0.106(3) 0.020(4) 0.0741(18) 0.008(3) C10 0.033(2) 0.038(2) 0.077(2) 0.005(2) 0.0423(15) 0.0002(19) C15 0.053(5) 0.066(6) 0.058(2) 0.012(3) 0.021(3) 0.007(5) C14 0.048(2) 0.062(3) 0.0525(16) 0.005(3) 0.0308(14) 0.022(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 C5 N7 1.156(19) . ? C5 N8 1.389(19) . ? Cd1 N9 2.298(3) 2_656 ? Cd1 N7 2.305(13) . ? Cd1 N4 2.363(11) . ? Cd1 N1 2.366(16) . ? Cd1 N6 2.379(11) 4_475 ? Cd1 N3 2.404(15) 4_575 ? N9 C6 1.210(2) . ? N9 Cd1 2.298(3) 2_646 ? N8 C6 1.223(12) . ? N4 C3 1.07(2) . ? C3 N5 1.36(2) . ? N1 C1 1.11(2) . ? N2 C1 1.32(2) . ? N2 C2 1.347(18) . ? N6 C4 1.10(2) . ? N6 Cd1 2.379(11) 4_676 ? N5 C4 1.54(2) . ? N3 C2 1.160(18) . ? N3 Cd1 2.404(15) 4_576 ? P1 C7 1.832(14) . ? P1 C13 1.844(12) . ? P1 C11 1.92(2) . ? P1 C9 1.929(8) . ? C13 C14 1.48(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C9 C10 1.520(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C7 C8 1.55(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C11 C12 1.50(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C15 C14 1.564(19) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? 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 C5 N8 173.2(11) . . ? N9 Cd1 N7 176.9(3) 2_656 . ? N9 Cd1 N4 92.5(4) 2_656 . ? N7 Cd1 N4 89.5(5) . . ? N9 Cd1 N1 94.0(4) 2_656 . ? N7 Cd1 N1 88.3(5) . . ? N4 Cd1 N1 95.4(5) . . ? N9 Cd1 N6 90.1(4) 2_656 4_475 ? N7 Cd1 N6 87.7(5) . 4_475 ? N4 Cd1 N6 174.1(6) . 4_475 ? N1 Cd1 N6 89.7(5) . 4_475 ? N9 Cd1 N3 91.4(4) 2_656 4_575 ? N7 Cd1 N3 86.1(5) . 4_575 ? N4 Cd1 N3 90.2(5) . 4_575 ? N1 Cd1 N3 172.0(4) . 4_575 ? N6 Cd1 N3 84.4(5) 4_475 4_575 ? C6 N9 Cd1 150.3(3) . 2_646 ? C5 N7 Cd1 172.2(11) . . ? C6 N8 C5 126.5(14) . . ? N9 C6 N8 174.3(9) . . ? C3 N4 Cd1 151.6(16) . . ? N4 C3 N5 163(2) . . ? C1 N1 Cd1 171.2(14) . . ? C1 N2 C2 121.1(12) . . ? N1 C1 N2 167.3(15) . . ? C4 N6 Cd1 131.7(17) . 4_676 ? C3 N5 C4 116.2(16) . . ? N6 C4 N5 170(2) . . ? C2 N3 Cd1 126.5(14) . 4_576 ? N3 C2 N2 176(2) . . ? C7 P1 C13 109.5(7) . . ? C7 P1 C11 110.9(8) . . ? C13 P1 C11 112.6(7) . . ? C7 P1 C9 107.7(6) . . ? C13 P1 C9 106.3(6) . . ? C11 P1 C9 109.6(7) . . ? C14 C13 P1 113.5(10) . . ? C14 C13 H13A 108.9 . . ? P1 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? P1 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C10 C9 P1 111.2(5) . . ? C10 C9 H9A 109.4 . . ? P1 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? P1 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C8 C7 P1 111.9(11) . . ? C8 C7 H7A 109.2 . . ? P1 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? P1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C12 C11 P1 117.6(13) . . ? C12 C11 H11A 107.9 . . ? P1 C11 H11A 107.9 . . ? C12 C11 H11B 107.9 . . ? P1 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C14 C15 110.2(15) . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.392 _refine_diff_density_min -2.069 _refine_diff_density_rms 0.484