#------------------------------------------------------------------------------ #$Date: 2014-07-11 15:35:18 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500036.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1500036 loop_ _publ_author_name 'Carmen R. Maldonado' 'Miguel Quir\'os' 'Juan M. Salas' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_email mquiros@ugr.es _publ_contact_author_fax 34-58-248526 _publ_contact_author_name 'Miguel Quir\'os' _publ_contact_author_phone 34-58-240441 _journal_name_full Polyhedron _journal_page_first 911 _journal_page_last 916 _journal_volume 28 _journal_year 2009 _chemical_formula_moiety 'C10 H18 Cd N2 O4 2+, 2(C6 H6 N5 O2 1-)' _chemical_formula_sum 'C22 H30 Cd N12 O8' _chemical_formula_weight 702.98 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 87.250(1) _cell_angle_beta 87.410(1) _cell_angle_gamma 65.661(1) _cell_formula_units_Z 1 _cell_length_a 8.5015(4) _cell_length_b 9.1721(5) _cell_length_c 10.1821(5) _cell_measurement_reflns_used 7305 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.2 _cell_measurement_theta_min 2.4 _cell_volume 722.29(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.910 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8365 _diffrn_reflns_theta_full 26.90 _diffrn_reflns_theta_max 28.24 _diffrn_reflns_theta_min 2.00 _diffrn_standards_decay_% 0.3 _diffrn_standards_number 272 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_correction_T_min 0.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 358 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.37 _refine_diff_density_max 0.277 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 3259 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0229 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.0606 _reflns_number_gt 3243 _reflns_number_total 3259 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file dmaxpycompound6.cif _[local]_cod_data_source_block cdaxpyr _cod_database_code 1500036 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.5000 0.5000 0.5000 0.03921(7) Uani 1 2 d S . . O1W O 0.52928(18) 0.47827(19) 0.27267(13) 0.0513(3) Uani 1 1 d D . . H11W H 0.488(3) 0.432(3) 0.227(2) 0.062 Uiso 1 1 d D . . H12W H 0.6285(17) 0.462(3) 0.245(2) 0.062 Uiso 1 1 d D . . O2W O 0.27075(18) 0.4323(2) 0.48888(13) 0.0523(3) Uani 1 1 d D . . H21W H 0.198(3) 0.452(3) 0.5509(18) 0.063 Uiso 1 1 d D . . H22W H 0.213(3) 0.457(3) 0.4211(16) 0.063 Uiso 1 1 d D . . N1P N 0.3293(2) 0.77010(19) 0.46922(16) 0.0472(3) Uani 1 1 d . . . C2P C 0.2162(3) 0.8234(2) 0.3725(2) 0.0534(5) Uani 1 1 d . . . H2P H 0.2004 0.7478 0.3206 0.064 Uiso 1 1 d R . . C3P C 0.1226(3) 0.9834(3) 0.3440(2) 0.0616(5) Uani 1 1 d . . . H3P H 0.0435 1.0179 0.2755 0.074 Uiso 1 1 d R . . C4P C 0.1452(3) 1.0938(3) 0.4187(2) 0.0629(5) Uani 1 1 d . . . H4P H 0.0815 1.2060 0.4034 0.076 Uiso 1 1 d R . . C5P C 0.2596(4) 1.0405(3) 0.5197(3) 0.0687(6) Uani 1 1 d . . . H5P H 0.2766 1.1135 0.5738 0.082 Uiso 1 1 d R . . C6P C 0.3488(3) 0.8789(3) 0.5411(2) 0.0608(5) Uani 1 1 d . . . H6P H 0.4278 0.8418 0.6096 0.073 Uiso 1 1 d R . . N1 N 0.0995(2) 0.4621(2) 0.25453(14) 0.0444(3) Uani 1 1 d . . . N2 N -0.0624(2) 0.4914(2) 0.28682(15) 0.0466(3) Uani 1 1 d . . . N3 N -0.13069(19) 0.4225(2) 0.20266(14) 0.0447(3) Uani 1 1 d . . . C3A C -0.0041(2) 0.3485(2) 0.11657(15) 0.0383(3) Uani 1 1 d . . . N4 N -0.00762(19) 0.25973(19) 0.01265(14) 0.0433(3) Uani 1 1 d . . . C4 C -0.1646(3) 0.2389(3) -0.0131(2) 0.0580(5) Uani 1 1 d . . . H41 H -0.2019 0.2012 0.0645 0.070 Uiso 1 1 d R . . H42 H -0.1366 0.1587 -0.0806 0.070 Uiso 1 1 d R . . H43 H -0.2580 0.3410 -0.0415 0.070 Uiso 1 1 d R . . C5 C 0.1363(2) 0.1940(2) -0.06783(17) 0.0443(4) Uani 1 1 d . . . O5 O 0.1408(2) 0.1140(2) -0.16068(15) 0.0619(4) Uani 1 1 d . . . N6 N 0.28169(19) 0.22073(19) -0.03745(15) 0.0440(3) Uani 1 1 d . . . C6 C 0.4303(3) 0.1567(3) -0.1301(2) 0.0609(5) Uani 1 1 d . . . H61 H 0.4050 0.2282 -0.2049 0.073 Uiso 1 1 d R . . H62 H 0.4502 0.0490 -0.1575 0.073 Uiso 1 1 d R . . H63 H 0.5341 0.1503 -0.0885 0.073 Uiso 1 1 d R . . C7 C 0.2962(2) 0.3063(2) 0.06797(17) 0.0435(4) Uani 1 1 d . . . O7 O 0.43046(19) 0.3203(2) 0.08579(16) 0.0648(4) Uani 1 1 d . . . C7A C 0.1401(2) 0.3714(2) 0.14604(16) 0.0391(3) 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 Cd 0.03526(10) 0.04566(11) 0.03884(10) -0.00700(7) -0.00426(6) -0.01785(7) O1W 0.0454(7) 0.0741(9) 0.0416(7) -0.0152(6) 0.0019(5) -0.0309(7) O2W 0.0431(7) 0.0821(10) 0.0420(7) -0.0146(7) -0.0006(5) -0.0347(7) N1P 0.0464(8) 0.0470(8) 0.0478(8) -0.0075(6) -0.0078(6) -0.0175(7) C2P 0.0589(11) 0.0535(10) 0.0467(10) -0.0082(8) -0.0118(8) -0.0204(9) C3P 0.0664(13) 0.0605(12) 0.0519(11) 0.0044(9) -0.0148(10) -0.0193(10) C4P 0.0736(14) 0.0459(10) 0.0656(13) 0.0039(9) -0.0058(11) -0.0210(10) C5P 0.0845(17) 0.0516(11) 0.0763(15) -0.0098(11) -0.0157(13) -0.0320(12) C6P 0.0646(13) 0.0544(11) 0.0654(13) -0.0077(10) -0.0223(10) -0.0237(10) N1 0.0434(8) 0.0563(9) 0.0370(7) -0.0082(6) -0.0040(6) -0.0232(7) N2 0.0431(8) 0.0598(9) 0.0380(7) -0.0085(6) -0.0019(6) -0.0215(7) N3 0.0385(7) 0.0591(9) 0.0388(7) -0.0054(6) -0.0036(6) -0.0216(7) C3A 0.0395(8) 0.0471(9) 0.0316(7) 0.0002(6) -0.0062(6) -0.0208(7) N4 0.0429(8) 0.0562(9) 0.0387(7) -0.0076(6) -0.0049(6) -0.0274(7) C4 0.0519(11) 0.0792(14) 0.0580(12) -0.0114(10) -0.0085(9) -0.0404(11) C5 0.0503(10) 0.0485(9) 0.0390(9) -0.0049(7) -0.0040(7) -0.0245(8) O5 0.0691(9) 0.0744(10) 0.0532(8) -0.0259(7) 0.0030(7) -0.0384(8) N6 0.0415(8) 0.0526(8) 0.0406(7) -0.0091(6) 0.0021(6) -0.0216(7) C6 0.0561(12) 0.0731(14) 0.0544(12) -0.0198(10) 0.0132(9) -0.0270(11) C7 0.0408(9) 0.0524(10) 0.0416(9) -0.0067(7) -0.0025(7) -0.0229(8) O7 0.0437(7) 0.0965(12) 0.0663(9) -0.0302(8) 0.0068(6) -0.0389(8) C7A 0.0390(8) 0.0487(9) 0.0333(8) -0.0031(6) -0.0044(6) -0.0213(7) 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' 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 O2W Cd O2W 180.0 . 2_666 ? O2W Cd N1P 87.16(6) . 2_666 ? O2W Cd N1P 92.84(6) 2_666 2_666 ? O2W Cd N1P 92.84(6) . . ? O2W Cd N1P 87.16(6) 2_666 . ? N1P Cd N1P 180.0 2_666 . ? O2W Cd O1W 87.09(5) . . ? O2W Cd O1W 92.91(5) 2_666 . ? N1P Cd O1W 91.28(6) 2_666 . ? N1P Cd O1W 88.72(6) . . ? O2W Cd O1W 92.91(5) . 2_666 ? O2W Cd O1W 87.09(5) 2_666 2_666 ? N1P Cd O1W 88.72(6) 2_666 2_666 ? N1P Cd O1W 91.28(6) . 2_666 ? O1W Cd O1W 180.0 . 2_666 ? Cd O1W H11W 126.7(18) . . ? Cd O1W H12W 112.6(17) . . ? H11W O1W H12W 109(2) . . ? Cd O2W H21W 120.5(18) . . ? Cd O2W H22W 119.2(18) . . ? H21W O2W H22W 105(2) . . ? C6P N1P C2P 117.56(17) . . ? C6P N1P Cd 121.21(13) . . ? C2P N1P Cd 121.06(13) . . ? N1P C2P C3P 122.91(19) . . ? N1P C2P H2P 118.7 . . ? C3P C2P H2P 118.4 . . ? C2P C3P C4P 118.7(2) . . ? C2P C3P H3P 121.3 . . ? C4P C3P H3P 120.0 . . ? C3P C4P C5P 118.9(2) . . ? C3P C4P H4P 121.5 . . ? C5P C4P H4P 119.6 . . ? C6P C5P C4P 118.7(2) . . ? C6P C5P H5P 120.3 . . ? C4P C5P H5P 120.9 . . ? N1P C6P C5P 123.2(2) . . ? N1P C6P H6P 117.8 . . ? C5P C6P H6P 119.0 . . ? N2 N1 C7A 106.37(14) . . ? N1 N2 N3 111.65(14) . . ? C3A N3 N2 105.13(14) . . ? N3 C3A C7A 109.61(15) . . ? N3 C3A N4 127.66(15) . . ? C7A C3A N4 122.73(15) . . ? C5 N4 C3A 119.34(14) . . ? C5 N4 C4 120.53(15) . . ? C3A N4 C4 120.12(16) . . ? N4 C4 H41 109.2 . . ? N4 C4 H42 108.0 . . ? H41 C4 H42 109.0 . . ? N4 C4 H43 111.2 . . ? H41 C4 H43 108.4 . . ? H42 C4 H43 110.9 . . ? O5 C5 N4 122.21(17) . . ? O5 C5 N6 120.62(17) . . ? N4 C5 N6 117.16(15) . . ? C7 N6 C5 126.72(15) . . ? C7 N6 C6 117.47(16) . . ? C5 N6 C6 115.77(16) . . ? N6 C6 H61 107.1 . . ? N6 C6 H62 111.6 . . ? H61 C6 H62 109.6 . . ? N6 C6 H63 109.6 . . ? H61 C6 H63 110.6 . . ? H62 C6 H63 108.3 . . ? O7 C7 N6 121.04(17) . . ? O7 C7 C7A 126.63(17) . . ? N6 C7 C7A 112.33(15) . . ? N1 C7A C3A 107.23(15) . . ? N1 C7A C7 131.05(15) . . ? C3A C7A C7 121.71(15) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd O2W 2.2848(13) . ? Cd O2W 2.2848(13) 2_666 ? Cd N1P 2.3119(16) 2_666 ? Cd N1P 2.3119(16) . ? Cd O1W 2.3261(13) . ? Cd O1W 2.3261(13) 2_666 ? O1W H11W 0.828(10) . ? O1W H12W 0.832(10) . ? O2W H21W 0.836(10) . ? O2W H22W 0.834(10) . ? N1P C6P 1.332(3) . ? N1P C2P 1.336(2) . ? C2P C3P 1.375(3) . ? C2P H2P 0.9463 . ? C3P C4P 1.375(3) . ? C3P H3P 0.9408 . ? C4P C5P 1.376(3) . ? C4P H4P 0.9531 . ? C5P C6P 1.370(3) . ? C5P H5P 0.9460 . ? C6P H6P 0.9407 . ? N1 N2 1.318(2) . ? N1 C7A 1.360(2) . ? N2 N3 1.367(2) . ? N3 C3A 1.326(2) . ? C3A C7A 1.374(2) . ? C3A N4 1.374(2) . ? N4 C5 1.371(2) . ? N4 C4 1.461(2) . ? C4 H41 0.9410 . ? C4 H42 0.9796 . ? C4 H43 0.9864 . ? C5 O5 1.214(2) . ? C5 N6 1.406(2) . ? N6 C7 1.399(2) . ? N6 C6 1.471(2) . ? C6 H61 0.9530 . ? C6 H62 0.9827 . ? C6 H63 0.9753 . ? C7 O7 1.222(2) . ? C7 C7A 1.431(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W O7 0.828(10) 1.988(11) 2.800(2) 167(2) . O1W H12W N3 0.832(10) 1.958(10) 2.785(2) 173(2) 1_655 O2W H21W N2 0.836(10) 1.935(11) 2.758(2) 168(3) 2_566 O2W H22W N1 0.834(10) 1.977(11) 2.795(2) 167(2) . _journal_paper_doi 10.1016/j.poly.2009.01.037