#------------------------------------------------------------------------------ #$Date: 2014-07-12 04:47:43 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120105 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/32/40/4324033.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_4324033 loop_ _publ_author_name 'Hidetaka Yuge' 'Yohsuke Noda' 'Toschitake Iwamoto' _publ_section_title ; Variations in Catenation Behavior in Aromatic Guest Clathrates Containing Rigid Host Entitiesp-Xylylenediamine (p-xda) and Tetracyanonickelate(II) Linking Octahedral Cadmium(II) in [Cd(p-xda)nNi(CN)4] Host (n= 1, 1.5, or 2) and the Related Complex [Cd(C6H5NH2)2(p-xda)Ni(CN)4] ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1842 _journal_page_last 1848 _journal_volume 35 _journal_year 1996 _chemical_formula_moiety 'C20 H24 Cd N8 Ni, (C9 H7 N)' _chemical_formula_structural 'Cd (C4 N4 Ni) (C8 H12 N2)2 (C9 H7 N)' _chemical_formula_sum 'C29 H31 Cd N10' _chemical_formula_weight 676.73 _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _cell_angle_alpha 90.00 _cell_angle_beta 102.64(1) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.505(1) _cell_length_b 17.737(1) _cell_length_c 10.106(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 17.41 _cell_measurement_theta_min 16.40 _cell_volume 1487.6(3) _diffrn_measurement_device 'RIGAKU AFC5R diffractometer' _diffrn_measurement_method '2\q-\w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70926 _diffrn_reflns_av_R_equivalents 0.005 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4842 _diffrn_reflns_theta_max 30.00 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_meas 1.50(1) _exptl_crystal_density_method 'flotation in mesitylene-bromoform' _exptl_crystal_description plate-like _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.93 _refine_diff_density_min -0.39 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.379 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 199 _refine_ls_number_reflns 3430 _refine_ls_R_factor_obs 0.0422 _refine_ls_shift/esd_max 0.009 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'calc w=1/(\s^2^(Fo)+0.0003Fo^2^)' _refine_ls_wR_factor_obs 0.0474 _reflns_number_observed 3430 _reflns_number_total 4150 _reflns_observed_criterion >4sigma(F) _[local]_cod_data_source_file ic950382n_4.cif _[local]_cod_data_source_block compound_(3b) _[local]_cod_chemical_formula_sum_orig 'C29 H31 Cd N9 N' _cod_original_cell_volume 1487.5(3) _cod_database_code 4324033 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y+1/2,-z -x,-y,-z +x,-y+1/2,+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd .0275(2) .0259(2) .0315(2) -.0027(2) .0091(2) -.0018(2) Ni .0301(4) .0207(3) .0369(4) .0 .0100(3) .0 N(1) .045(2) .031(2) .061(3) -.009(2) .004(2) .000(2) N(2) .053(3) .048(3) .077(3) .014(2) .025(2) -.007(2) N(3) .037(2) .041(2) .035(2) .009(2) .003(2) -.005(2) N(4) .050(2) .045(2) .035(2) .003(2) .022(2) .001(2) C(1) .032(2) .027(2) .039(2) .003(2) .004(2) -.002(2) C(2) .038(2) .034(2) .048(2) .001(2) .017(2) -.003(2) C(3) .034(2) .075(4) .031(2) -.008(2) .010(2) -.007(2) C(4) .029(2) .047(3) .031(2) -.004(2) .003(2) -.001(2) C(5) .061(3) .038(3) .041(3) -.001(2) .012(2) .005(2) C(6) .061(3) .034(2) .046(3) .001(2) .018(2) .001(2) C(7) .037(2) .038(2) .037(2) -.002(2) .013(2) -.000(2) C(8) .073(4) .038(3) .044(3) -.000(3) .029(3) -.001(2) C(9) .071(4) .037(3) .043(3) .000(3) .021(3) -.002(2) C(10) .068(3) .043(3) .046(3) -.006(2) .034(3) -.006(2) N(11) .087(6) .053(5) .097(7) .0 -.003(6) .0 C(12) .106(9) .049(5) .098(8) .0 .017(7) .0 C(13) .115(9) .047(5) .075(7) .0 -.005(7) .0 C(14) .106(8) .045(5) .068(6) .0 .001(6) .0 C(15) .107(9) .043(5) .094(8) .0 .021(7) .0 C(16) .149(12) .048(5) .077(7) .0 .019(8) .0 C(17) .184(15) .036(5) .070(7) .0 .016(9) .0 C(18) .148(11) .036(4) .058(6) .0 -.014(7) .0 C(19) .088(7) .033(4) .067(6) .0 -.007(5) .0 C(20) .084(6) .027(3) .064(5) .0 -.005(5) .0 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Cd .0 .0 .0 .0279(1) Uani d . Ni .33512(9) .25 .04288(8) .0288(2) Uani d . N(1) .0936(5) .1258(2) .0328(4) .047(1) Uani d . N(2) .5862(5) .1283(3) .0593(5) .058(2) Uani d . N(3) .2330(4) -.0532(2) .1317(3) .038(1) Uani d . N(4) .1093(5) -.0202(2) .8049(4) .041(1) Uani d . C(1) .1825(5) .1744(2) .0373(4) .033(1) Uani d . C(2) .4910(5) .1748(3) .0512(5) .039(2) Uani d . C(3) .3574(5) -.0072(3) .2279(4) .046(2) Uani d . C(4) .3040(5) .0074(3) .3584(4) .036(1) Uani d . C(5) .2756(7) .0795(3) .4005(5) .046(2) Uani d . C(6) .2300(7) .0911(3) .5239(5) .046(2) Uani d . C(7) .2134(5) .0307(3) .6062(4) .036(1) Uani d . C(8) .2432(7) -.0426(3) .5647(5) .049(2) Uani d . C(9) .2905(7) -.0534(3) .4420(5) .049(2) Uani d . C(10) .1662(7) .0468(3) .7408(5) .049(2) Uani d . N(11) .9927(11) .25 .5295(10) .082(4) Uani d . C(12) .9680(15) .25 .3952(13) .086(5) Uani d . C(13) .8112(16) .25 .3096(11) .083(5) Uani d . C(14) .6798(15) .25 .3678(10) .076(4) Uani d . C(15) .5727(15) .25 .5773(12) .081(5) Uani d . C(16) .5969(18) .25 .7172(12) .092(5) Uani d . C(17) .7597(22) .25 .7922(11) .099(6) Uani d . C(18) .8916(17) .25 .7311(10) .086(5) Uani d . C(19) .8619(13) .25 .5887(9) .066(4) Uani d . C(20) .7026(12) .25 .5087(9) .062(3) Uani d . H(1) .29099 -.07731 .06668 .076 Uiso calc N(3) H(2) .19613 -.09300 .18809 .076 Uiso calc N(3) H(3) .47219 -.03819 .25041 .076 Uiso calc C(3) H(4) .37410 .04701 .17994 .076 Uiso calc C(3) H(5) .28872 .12724 .33738 .076 Uiso calc C(5) H(6) .20761 .14765 .55503 .076 Uiso calc C(6) H(7) .22952 -.09037 .62746 .076 Uiso calc C(8) H(8) .31691 -.10957 .41187 .076 Uiso calc C(9) H(9) .06894 .08900 .72252 .076 Uiso calc C(10) H(10) .27200 .07001 .81168 .076 Uiso calc C(10) H(11) .02393 -.04503 .73473 .076 Uiso calc N(4) H(12) .20319 -.05506 .83204 .076 Uiso calc N(4) H(13) 1.07115 .25 .34906 .076 Uiso calc C(12) H(14) .79585 .25 .20064 .076 Uiso calc C(13) H(15) .55950 .25 .30493 .076 Uiso calc C(14) H(16) .45067 .25 .51760 .076 Uiso calc C(15) H(17) .49700 .25 .76734 .076 Uiso calc C(16) H(18) .78188 .25 .90163 .076 Uiso calc C(17) H(19) 1.01327 .25 .79156 .076 Uiso calc C(18) 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_2 _geom_angle_site_symmetry_3 C(1) Ni C(2) 88.3(2) . . . N(1) Cd N(3) 94.8(1) . . . N(1) Cd N(4) 94.4(1) . . 1_554 N(3) Cd N(4) 88.6(1) . . 1_554 Ni C(1) N(1) 177.1(4) . . . Ni C(2) N(2) 178.5(5) . . . Cd N(1) C(1) 156.4(4) . . . Cd N(3) C(3) 122.5(3) . . . Cd N(4) C(10) 117.7(3) . 1_554 1_554 N(3) C(3) C(4) 110.7(4) . . . C(3) C(4) C(5) 122.2(4) . . . C(3) C(4) C(9) 118.6(4) . . . C(4) C(5) C(6) 120.6(4) . . . C(5) C(6) C(7) 120.4(4) . . . C(6) C(7) C(8) 119.3(4) . . . C(7) C(8) C(9) 119.8(4) . . . C(8) C(9) C(4) 120.7(5) . . . C(9) C(4) C(12) 119.1(4) . . . C(6) C(7) C(10) 118.2(4) . . . C(10) C(7) C(8) 122.6(4) . . . N(4) C(10) C(7) 114.4(4) . . . N(11) C(12) C(13) 122.7(12) . . . N(11) C(19) C(18) 117.7(10) . . . N(11) C(19) C(20) 121.0(9) . . . C(12) N(11) C(19) 118.9(10) . . . C(12) C(13) C(14) 118.8(10) . . . C(13) C(14) C(20) 119.6(10) . . . C(14) C(20) C(15) 123.1(10) . . . C(14) C(20) C(19) 119.0(11) . . . C(15) C(16) C(17) 117.0(12) . . . C(15) C(20) C(19) 117.9(9) . . . C(16) C(17) C(18) 123.1(10) . . . C(16) C(15) C(20) 122.6(11) . . . C(17) C(18) C(19) 118.2(11) . . . C(18) C(19) C(20) 121.3(12) . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ni C(1) 1.859(4) . . Ni C(2) 1.869(5) . . Cd N(1) 2.368(4) . . Cd N(3) 2.331(3) . . Cd N(4) 2.383(3) . 1_554 C(1) N(1) 1.141(5) . . C(2) N(2) 1.146(6) . . N(3) C(3) 1.510(6) . . C(3) C(4) 1.508(6) . . C(4) C(5) 1.386(6) . . C(5) C(6) 1.400(7) . . C(6) C(7) 1.382(6) . . C(7) C(8) 1.406(7) . . C(8) C(9) 1.398(7) . . C(9) C(4) 1.389(6) . . C(7) C(10) 1.527(6) . . N(4) C(10) 1.484(6) . . N(11) C(12) 1.327(14) . . C(12) C(13) 1.421(16) . . C(13) C(14) 1.372(16) . . C(15) C(16) 1.384(15) . . C(16) C(17) 1.426(18) . . C(17) C(18) 1.394(18) . . C(18) C(19) 1.406(13) . . C(19) C(20) 1.418(13) . . N(11) C(19) 1.373(13) . . C(20) C(14) 1.394(13) . . C(20) C(15) 1.427(14) . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N(2) N(3) 3.027(7) . 3_655 N(2) N(4) 3.273(6) . 3_656 _journal_paper_doi 10.1021/ic950382n