#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003226.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_2003226 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 374 _journal_page_last 377 _publ_section_title ; Two-Dimensional Open-Frame Host Structure of the Inclusion Compound [Cd(tenH)~2~{Ni(CN)~4~}~2~].4C~6~H~5~NH~2~ (ten = 1,4-Diazabicyclo[2.2.2]octane) ; _chemical_formula_moiety 'C20 H26 Cd N12 Ni2 , 4C6 H7 N1' _chemical_formula_sum 'C44 H54 Cd N16 Ni2' _chemical_formula_weight 1036.82 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.537(2) _cell_length_b 10.615(3) _cell_length_c 21.101(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.24(2) _cell_angle_gamma 90.00 _cell_volume 2358.4(9) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_meas 1.47(1) _exptl_crystal_density_method 'flotation in mesitylene-bromoform' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.00 _cell_measurement_theta_max 17.45 _exptl_absorpt_coefficient_mu 1.287 _cell_measurement_temperature 293 _exptl_crystal_description plate _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_colour yellow _diffrn_measurement_device 'RIGAKU AFC-5R diffractometer' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _diffrn_reflns_number 7697 _reflns_number_total 5554 _reflns_number_observed 3654 _reflns_observed_criterion >4\s(F) _diffrn_reflns_av_R_equivalents 0.011 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 3.7 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0417 _refine_ls_wR_factor_obs 0.0338 _refine_ls_goodness_of_fit_obs 1.369 _refine_ls_number_reflns 3654 _refine_ls_number_parameters 397 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(F~o~)+0.00005F~o~^2^]' _refine_ls_shift/esd_max 0.013 _refine_diff_density_max 0.60 _refine_diff_density_min -0.46 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_source C 'SHELX-76 (Sheldrick, 1976)' H 'SHELX-76 (Sheldrick, 1976)' Cd 'International Tables Vol. IV Table 2.2B' N 'SHELX-76 (Sheldrick, 1976)' Ni 'International Tables Vol. IV Table 2.2B' ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1987) ; ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1987) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Cd .0 .0 .0 .0234(1) Ni1 .0 .5 .0 .0334(2) Ni2 .5 .0 .0 .0323(2) N1 -.0060(4) .2176(3) .0118(2) .040(1) N2 -.0864(4) .5334(4) .1334(2) .060(2) N3 .2190(3) .0019(5) .0214(2) .039(1) N4 .5626(4) .1063(5) .1303(2) .061(2) C1 -.0053(5) .3249(4) .0083(2) .034(1) C2 -.0534(4) .5193(4) .0828(2) .043(2) C3 .3260(3) .0012(5) .0147(2) .033(1) C4 .5366(4) .0669(4) .0811(2) .038(2) N11 -.0537(3) -.0314(3) .1106(2) .027(1) C11 .0644(5) -.0631(5) .1478(2) .040(2) C12 .0431(5) -.0591(6) .2189(3) .047(2) C13 -.1462(5) -.1342(5) .1202(2) .037(2) C14 -.1579(6) -.1638(5) .1908(2) .044(2) C15 -.1085(5) .0854(4) .1372(2) .034(2) C16 -.1499(5) .0639(5) .2051(3) .042(2) N12 -.0969(4) -.0583(4) .2279(2) .036(1) N21 -.0113(5) .3800(6) .2568(3) .066(2) C21 .0993(5) .3101(5) .2488(3) .045(2) C22 .1588(6) .2480(6) .2995(3) .059(2) C23 .2624(7) .1718(7) .2901(4) .076(3) C24 .3053(7) .1540(7) .2308(5) .082(3) C25 .2478(7) .2145(6) .1803(3) .066(3) C26 .1458(6) .2915(5) .1887(3) .052(2) N31 -.1329(5) -.0909(5) .3566(2) .053(2) C31 -.0492(5) -.0093(6) .3924(2) .047(2) C32 .0733(7) -.0448(7) .4075(3) .068(3) C33 .1547(8) .0364(9) .4416(4) .087(4) C34 .1134(9) .1528(8) .4600(3) .079(3) C35 -.0070(9) .1871(7) .4437(3) .081(3) C36 -.0892(6) .1093(6) .4102(3) .058(2) H1 .133(4) -.011(4) .135(2) .05(1) H2 .089(4) -.153(4) .133(2) .05(1) H3 .076(4) .006(4) .241(2) .06(2) H4 .075(5) -.130(5) .239(2) .06(2) H5 -.126(4) -.204(4) .098(2) .03(1) H6 -.225(4) -.111(5) .102(2) .06(2) H7 -.242(4) -.168(4) .204(2) .03(1) H8 -.115(5) -.244(5) .204(2) .07(2) H9 -.189(4) .106(4) .109(2) .05(1) H10 -.045(4) .150(4) .135(2) .05(1) H11 -.119(4) .122(4) .235(2) .04(1) H12 -.238(4) .059(4) .208(2) .04(1) H13 -.115(4) -.060(4) .272(2) .05(1) H20 -.010(6) .402(6) .293(2) .08(2) H21 -.026(5) .432(5) .223(2) .08(2) H22 .127(4) .266(4) .339(2) .05(2) H23 .290(6) .134(6) .324(3) .09(2) H24 .365(5) .113(5) .229(3) .07(2) H25 .272(5) .202(5) .138(2) .07(2) H26 .105(4) .334(4) .155(2) .03(1) H30 -.212(4) -.073(4) .362(2) .04(1) H31 -.118(5) -.160(5) .365(2) .06(2) H32 .104(5) -.121(5) .393(2) .06(2) H33 .229(6) .012(7) .444(3) .10(3) H34 .187(7) .206(6) .483(3) .13(3) H35 -.036(6) .262(6) .455(3) .11(3) H36 -.178(4) .129(4) .400(2) .05(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Cd .0186(2) -.0007(3) .0020(2) .0176(2) .0012(3) .0341(2) Ni1 .0377(4) .0002(6) .0027(3) .0166(3) .0033(5) .0459(4) Ni2 .0173(3) .0008(6) .0018(3) .0411(4) .0036(6) .0386(4) N1 .055(2) -.002(2) .016(2) .019(2) .000(2) .046(3) N2 .072(3) .009(2) .011(2) .051(3) .004(2) .055(3) N3 .022(1) .001(3) .002(1) .049(2) -.001(3) .047(2) N4 .040(3) .002(3) -.001(2) .093(4) -.012(3) .050(3) C1 .040(2) .003(3) .005(2) .025(2) -.001(2) .038(3) C2 .047(3) .002(2) -.003(2) .023(3) .001(2) .058(3) C3 .026(2) .004(4) -.002(1) .038(2) .000(3) .035(2) C4 .016(2) .005(2) .003(2) .050(3) .007(2) .047(3) N11 .027(2) -.003(1) .002(1) .019(2) .001(1) .034(2) C11 .034(3) .008(2) -.000(2) .049(3) .006(2) .036(3) C12 .038(3) .007(3) -.003(2) .060(4) .001(3) .040(3) C13 .045(3) -.014(2) .006(2) .030(3) -.005(2) .037(3) C14 .056(4) -.008(3) .013(3) .034(3) .003(2) .043(3) C15 .039(3) -.003(2) .002(2) .024(2) .001(2) .040(3) C16 .046(3) .009(3) .004(3) .040(3) -.008(2) .040(3) N12 .038(2) .001(2) .005(2) .038(2) -.002(2) .033(2) N21 .056(3) -.004(3) .009(3) .073(4) -.003(3) .069(4) C21 .041(3) -.013(2) .007(3) .038(3) -.002(2) .056(3) C22 .057(4) -.022(4) .002(3) .067(4) .002(4) .053(3) C23 .066(5) -.018(4) -.016(5) .064(5) .027(4) .097(6) C24 .051(4) -.006(4) .016(5) .049(4) -.002(5) .146(8) C25 .074(5) -.021(3) .028(4) .045(4) -.012(3) .080(5) C26 .058(4) -.015(3) .002(3) .043(3) .002(3) .055(3) N31 .062(4) .009(3) .012(3) .048(3) .003(2) .050(3) C31 .059(3) .005(4) .010(2) .049(3) .002(3) .032(2) C32 .067(4) .022(4) .010(4) .066(4) .005(3) .071(4) C33 .063(5) -.002(5) -.014(4) .118(8) .027(5) .079(5) C34 .101(6) -.022(5) .007(4) .081(6) .009(4) .056(4) C35 .113(7) -.010(5) .015(5) .055(5) -.013(4) .076(5) C36 .057(4) .007(3) .011(3) .048(3) -.004(3) .069(4) _cod_database_code 2003226