#------------------------------------------------------------------------------ #$Date: 2014-07-11 17:35:18 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100602.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_1100602 loop_ _publ_author_name 'Klaus Harms' 'Jan Merle' 'C\"acili\"a Maichle-M\"ossmer' 'Werner Massa' 'Matthias Krieger' _publ_section_title ; Heterocubane Phosphoraniminato Complexes of Cadmium ; _journal_name_full 'Inorganic Chemistry' _journal_volume 37 _journal_page_first 1099 _journal_page_last 1104 _journal_year 1998 _chemical_formula_sum 'C45 H84 Cd4 I4 N4 P4' _chemical_formula_weight 1762.24 _symmetry_cell_setting rhombohedral _space_group_IT_number 160 _symmetry_space_group_name_Hall 'R 3 -2"' _symmetry_space_group_name_H-M 'R 3 m :H' _[local]_cod_cif_authors_sg_H-M 'R 3 m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -y,-x,z 5 -x+y,y,z 6 x,x-y,z 7 -1/3+x,1/3+y,1/3+z 8 -1/3-y,1/3+x-y,1/3+z 9 -1/3-x+y,1/3-x,1/3+z 10 -1/3-y,1/3-x,1/3+z 11 -1/3-x+y,1/3+y,1/3+z 12 -1/3+x,1/3+x-y,1/3+z 13 1/3+x,-1/3+y,-1/3+z 14 1/3-y,-1/3+x-y,-1/3+z 15 1/3-x+y,-1/3-x,-1/3+z 16 1/3-y,-1/3-x,-1/3+z 17 1/3-x+y,-1/3+y,-1/3+z 18 1/3+x,-1/3+x-y,-1/3+z _cell_length_a 17.842(2) _cell_length_b 17.842(2) _cell_length_c 17.290(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 4766.6(11) _cell_formula_units_Z 3 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 5.32 _cell_measurement_theta_max 12.49 _exptl_absorpt_coefficient_mu 3.394 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2353 _exptl_absorpt_correction_T_max 0.4291 _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 Cd 1.40 I 1.40 N 0.68 P 1.05 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+26.3894P] 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 0.00152(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(6) _refine_ls_number_reflns 2066 _refine_ls_number_parameters 143 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.39329(2) 0.60671(2) 0.18395(3) 0.0309(2) Uani 1 d S . . Cd2 Cd 1.3333 0.6667 0.02899(6) 0.0331(3) Uani 1 d S . . I1 I 1.47444(3) 0.52556(3) 0.23698(6) 0.0780(4) Uani 1 d S . . I2 I 1.3333 0.6667 -0.12704(7) 0.0641(5) Uani 1 d S . . P1 P 1.22483(9) 0.44966(18) 0.07923(15) 0.0381(6) Uani 1 d S . . P2 P 1.3333 0.6667 0.3515(2) 0.0321(9) Uani 1 d S . . N1 N 1.2742(2) 0.5484(5) 0.1075(6) 0.0311(16) Uani 1 d S . . N2 N 1.3333 0.6667 0.2594(8) 0.034(3) Uani 1 d S . . C11 C 1.1522(15) 0.4257(14) -0.0005(11) 0.051(4) Uani 0.50 d P . . H11A H 1.1412 0.3725 -0.0242 0.061 Uiso 0.50 d PR . . H11B H 1.1795 0.4708 -0.0384 0.061 Uiso 0.50 d PR . . C12 C 1.0636(16) 0.4184(13) 0.0224(15) 0.061(5) Uani 0.50 d P . . H12A H 1.0276 0.4059 -0.0225 0.091 Uiso 0.50 d PR . . H12B H 1.0351 0.3725 0.0594 0.091 Uiso 0.50 d PR . . H12C H 1.0738 0.4719 0.0450 0.091 Uiso 0.50 d PR . . C13 C 1.3006(15) 0.4147(13) 0.0423(18) 0.063(6) Uani 0.50 d P . . H13A H 1.2678 0.3551 0.0269 0.075 Uiso 0.50 d PR . . H13B H 1.3373 0.4183 0.0844 0.075 Uiso 0.50 d PR . . C14 C 1.3523(18) 0.4622(19) -0.0216(19) 0.090(9) Uani 0.50 d P . . H14A H 1.3894 0.4400 -0.0360 0.135 Uiso 0.50 d PR . . H14B H 1.3164 0.4578 -0.0647 0.135 Uiso 0.50 d PR . . H14C H 1.3868 0.5218 -0.0066 0.135 Uiso 0.50 d PR . . C15 C 1.2068(10) 0.3740(10) 0.1584(9) 0.045(5) Uani 0.50 d P . . H15A H 1.1728 0.3818 0.1972 0.054 Uiso 0.50 d PR . . H15B H 1.2620 0.3903 0.1811 0.054 Uiso 0.50 d PR . . C16 C 1.1624(13) 0.2791(11) 0.1386(11) 0.058(6) Uani 0.50 d P . . H16A H 1.1568 0.2465 0.1846 0.086 Uiso 0.50 d PR . . H16B H 1.1060 0.2608 0.1176 0.086 Uiso 0.50 d PR . . H16C H 1.1965 0.2695 0.1012 0.086 Uiso 0.50 d PR . . C21 C 1.2467(12) 0.6820(15) 0.3935(9) 0.055(5) Uani 0.50 d P . . H21A H 1.2541 0.6871 0.4486 0.066 Uiso 0.50 d PR . . H21B H 1.1919 0.6312 0.3832 0.066 Uiso 0.50 d PR . . C22 C 1.2426(5) 0.7574(5) 0.3663(8) 0.063(4) Uani 1 d S . . H22A H 1.1960 0.7610 0.3910 0.094 Uiso 0.50 d PR . . H22B H 1.2963 0.8096 0.3776 0.094 Uiso 0.50 d PR . . H22C H 1.2333 0.7530 0.3114 0.094 Uiso 0.50 d PR . . C100 C 1.0369(17) 0.5185(8) 0.5005(16) 0.17(2) Uani 1 d S . . C200 C 1.0721(18) 0.6014(14) 0.530(2) 0.166(13) Uani 1 d . . . H20A H 1.0444 0.6346 0.5197 0.199 Uiso 1 d R . . C300 C 1.1400(17) 0.6364(12) 0.5806(16) 0.150(12) Uani 1 d . . . H30A H 1.1616 0.6959 0.5942 0.180 Uiso 1 d R . . C400 C 1.170(3) 0.5849(13) 0.605(2) 0.168(18) Uani 1 d S . . H40A H 1.2172 0.6086 0.6407 0.202 Uiso 1 d SR . . C700 C 0.971(4) 0.4857(19) 0.454(2) 0.37(6) Uani 1 d S . . H70B H 0.9592 0.5305 0.4377 0.548 Uiso 0.50 calc PR . . H70C H 0.9213 0.4402 0.4803 0.548 Uiso 0.50 calc PR . . H70D H 0.9847 0.4619 0.4090 0.548 Uiso 0.50 calc PR . . 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 0.0339(3) 0.0339(3) 0.0295(3) 0.00030(14) -0.00030(14) 0.0206(3) Cd2 0.0377(4) 0.0377(4) 0.0239(5) 0.000 0.000 0.0189(2) I1 0.1104(8) 0.1104(8) 0.0660(6) 0.0062(2) -0.0062(2) 0.0947(8) I2 0.0826(7) 0.0826(7) 0.0270(6) 0.000 0.000 0.0413(4) P1 0.0471(12) 0.0281(13) 0.0328(12) -0.0037(10) -0.0019(5) 0.0141(6) P2 0.0367(14) 0.0367(14) 0.0228(19) 0.000 0.000 0.0184(7) N1 0.031(3) 0.027(4) 0.034(3) -0.003(4) -0.0013(18) 0.013(2) N2 0.041(5) 0.041(5) 0.021(6) 0.000 0.000 0.020(3) C11 0.058(11) 0.060(13) 0.037(7) -0.005(8) -0.003(9) 0.031(10) C12 0.043(11) 0.047(11) 0.074(12) 0.000(10) 0.005(10) 0.009(10) C13 0.045(11) 0.044(11) 0.104(19) -0.039(12) -0.004(11) 0.026(8) C14 0.083(18) 0.085(18) 0.13(2) -0.033(18) 0.011(16) 0.059(15) C15 0.051(12) 0.037(7) 0.043(7) -0.004(6) 0.004(6) 0.019(6) C16 0.071(14) 0.041(8) 0.062(9) -0.009(7) -0.006(8) 0.029(8) C21 0.046(9) 0.072(12) 0.028(7) -0.003(8) 0.001(6) 0.015(8) C22 0.079(8) 0.079(8) 0.049(7) 0.000(3) 0.000(3) 0.054(9) C100 0.054(12) 0.28(5) 0.083(15) 0.012(6) 0.023(11) 0.027(6) C200 0.103(15) 0.072(12) 0.29(4) 0.022(18) -0.01(2) 0.019(12) C300 0.17(2) 0.075(11) 0.24(3) 0.061(15) 0.12(2) 0.088(14) C400 0.18(4) 0.14(2) 0.20(4) 0.063(16) 0.13(3) 0.088(18) C700 0.23(6) 0.61(14) 0.14(4) 0.06(2) 0.13(5) 0.11(3) 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 N2 2.266(8) . ? Cd1 N1 2.266(6) . ? Cd1 N1 2.266(6) 2_755 ? Cd1 I1 2.6703(11) . ? Cd1 Cd1 3.2093(12) 3_775 ? Cd1 Cd1 3.2094(12) 2_755 ? Cd1 Cd2 3.2577(12) . ? Cd2 N1 2.277(8) 3_775 ? Cd2 N1 2.277(9) 2_755 ? Cd2 N1 2.277(8) . ? Cd2 I2 2.6977(17) . ? Cd2 Cd1 3.2577(12) 3_775 ? Cd2 Cd1 3.2577(12) 2_755 ? P1 N1 1.602(8) . ? P1 C11 1.791(18) . ? P1 C11 1.791(18) 5_755 ? P1 C15 1.835(16) 5_755 ? P1 C15 1.835(16) . ? P1 C13 1.86(2) . ? P1 C13 1.86(2) 5_755 ? P2 N2 1.593(14) . ? P2 C21 1.85(2) . ? P2 C21 1.85(2) 4_775 ? P2 C21 1.85(2) 6 ? P2 C21 1.85(2) 3_775 ? P2 C21 1.85(2) 2_755 ? P2 C21 1.85(2) 5_755 ? N1 Cd1 2.266(6) 3_775 ? N2 Cd1 2.266(8) 3_775 ? N2 Cd1 2.266(8) 2_755 ? C11 C13 0.96(3) 5_755 ? C11 C14 1.27(3) 5_755 ? C11 C12 1.57(3) . ? C12 C13 1.00(3) 5_755 ? C12 C14 1.11(4) 5_755 ? C13 C11 0.96(3) 5_755 ? C13 C12 1.00(3) 5_755 ? C13 C14 1.42(4) . ? C14 C12 1.11(4) 5_755 ? C14 C11 1.27(3) 5_755 ? C15 C15 0.71(3) 5_755 ? C15 C16 1.51(2) . ? C15 C16 1.69(2) 5_755 ? C16 C16 0.81(4) 5_755 ? C16 C15 1.69(2) 5_755 ? C21 C21 1.27(4) 4_775 ? C21 C22 1.46(3) . ? C22 C21 1.46(3) 4_775 ? C100 C700 1.29(6) . ? C100 C200 1.39(3) 6 ? C100 C200 1.39(3) . ? C200 C300 1.36(4) . ? C300 C400 1.34(3) . ? C400 C300 1.34(3) 6 ? 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 Cd1 N1 89.8(2) . . ? N2 Cd1 N1 89.8(2) . 2_755 ? N1 Cd1 N1 88.6(4) . 2_755 ? N2 Cd1 I1 124.8(3) . . ? N1 Cd1 I1 126.12(17) . . ? N1 Cd1 I1 126.12(17) 2_755 . ? N2 Cd1 Cd1 44.9(2) . 3_775 ? N1 Cd1 Cd1 44.91(16) . 3_775 ? N1 Cd1 Cd1 89.45(17) 2_755 3_775 ? I1 Cd1 Cd1 144.427(14) . 3_775 ? N2 Cd1 Cd1 44.9(2) . 2_755 ? N1 Cd1 Cd1 89.46(17) . 2_755 ? N1 Cd1 Cd1 44.91(16) 2_755 2_755 ? I1 Cd1 Cd1 144.427(14) . 2_755 ? Cd1 Cd1 Cd1 60.0 3_775 2_755 ? N2 Cd1 Cd2 90.5(3) . . ? N1 Cd1 Cd2 44.3(2) . . ? N1 Cd1 Cd2 44.3(2) 2_755 . ? I1 Cd1 Cd2 144.75(3) . . ? Cd1 Cd1 Cd2 60.490(13) 3_775 . ? Cd1 Cd1 Cd2 60.490(13) 2_755 . ? N1 Cd2 N1 88.1(3) 3_775 2_755 ? N1 Cd2 N1 88.1(3) 3_775 . ? N1 Cd2 N1 88.1(3) 2_755 . ? N1 Cd2 I2 126.6(2) 3_775 . ? N1 Cd2 I2 126.6(2) 2_755 . ? N1 Cd2 I2 126.6(2) . . ? N1 Cd2 Cd1 44.05(16) 3_775 3_775 ? N1 Cd2 Cd1 88.1(2) 2_755 3_775 ? N1 Cd2 Cd1 44.05(16) . 3_775 ? I2 Cd2 Cd1 145.335(16) . 3_775 ? N1 Cd2 Cd1 44.05(16) 3_775 2_755 ? N1 Cd2 Cd1 44.05(16) 2_755 2_755 ? N1 Cd2 Cd1 88.1(2) . 2_755 ? I2 Cd2 Cd1 145.334(16) . 2_755 ? Cd1 Cd2 Cd1 59.02(3) 3_775 2_755 ? N1 Cd2 Cd1 88.1(2) 3_775 . ? N1 Cd2 Cd1 44.05(16) 2_755 . ? N1 Cd2 Cd1 44.05(16) . . ? I2 Cd2 Cd1 145.335(16) . . ? Cd1 Cd2 Cd1 59.02(3) 3_775 . ? Cd1 Cd2 Cd1 59.02(3) 2_755 . ? N1 P1 C11 115.6(7) . . ? N1 P1 C11 115.6(7) . 5_755 ? C11 P1 C11 74.3(15) . 5_755 ? N1 P1 C15 112.3(6) . 5_755 ? C11 P1 C15 109.1(9) . 5_755 ? C11 P1 C15 124.0(9) 5_755 5_755 ? N1 P1 C15 112.3(6) . . ? C11 P1 C15 124.0(9) . . ? C11 P1 C15 109.1(9) 5_755 . ? C15 P1 C15 22.2(10) 5_755 . ? N1 P1 C13 112.4(6) . . ? C11 P1 C13 102.5(14) . . ? C11 P1 C13 30.3(10) 5_755 . ? C15 P1 C13 104.1(11) 5_755 . ? C15 P1 C13 84.2(11) . . ? N1 P1 C13 112.4(6) . 5_755 ? C11 P1 C13 30.3(10) . 5_755 ? C11 P1 C13 102.5(14) 5_755 5_755 ? C15 P1 C13 84.2(11) 5_755 5_755 ? C15 P1 C13 104.1(11) . 5_755 ? C13 P1 C13 126.6(15) . 5_755 ? N2 P2 C21 113.1(5) . . ? N2 P2 C21 113.1(5) . 4_775 ? C21 P2 C21 40.3(14) . 4_775 ? N2 P2 C21 113.1(5) . 6 ? C21 P2 C21 69.0(14) . 6 ? C21 P2 C21 105.6(6) 4_775 6 ? N2 P2 C21 113.1(5) . 3_775 ? C21 P2 C21 105.6(6) . 3_775 ? C21 P2 C21 69.0(14) 4_775 3_775 ? C21 P2 C21 131.2(10) 6 3_775 ? N2 P2 C21 113.1(5) . 2_755 ? C21 P2 C21 105.6(6) . 2_755 ? C21 P2 C21 131.2(10) 4_775 2_755 ? C21 P2 C21 40.3(14) 6 2_755 ? C21 P2 C21 105.6(6) 3_775 2_755 ? N2 P2 C21 113.1(5) . 5_755 ? C21 P2 C21 131.2(10) . 5_755 ? C21 P2 C21 105.6(6) 4_775 5_755 ? C21 P2 C21 105.6(6) 6 5_755 ? C21 P2 C21 40.3(14) 3_775 5_755 ? C21 P2 C21 69.0(14) 2_755 5_755 ? P1 N1 Cd1 123.9(3) . . ? P1 N1 Cd1 123.9(3) . 3_775 ? Cd1 N1 Cd1 90.2(3) . 3_775 ? P1 N1 Cd2 125.6(5) . . ? Cd1 N1 Cd2 91.6(2) . . ? Cd1 N1 Cd2 91.6(2) 3_775 . ? P2 N2 Cd1 125.1(3) . 3_775 ? P2 N2 Cd1 125.1(3) . 2_755 ? Cd1 N2 Cd1 90.2(4) 3_775 2_755 ? P2 N2 Cd1 125.1(3) . . ? Cd1 N2 Cd1 90.2(4) 3_775 . ? Cd1 N2 Cd1 90.2(4) 2_755 . ? C13 C11 C14 78(3) 5_755 5_755 ? C13 C11 C12 37(2) 5_755 . ? C14 C11 C12 44.3(18) 5_755 . ? C13 C11 P1 79.0(17) 5_755 . ? C14 C11 P1 129.9(19) 5_755 . ? C12 C11 P1 113.8(16) . . ? C13 C12 C14 84(3) 5_755 5_755 ? C13 C12 C11 36(2) 5_755 . ? C14 C12 C11 53.3(19) 5_755 . ? C11 C13 C12 107(4) 5_755 5_755 ? C11 C13 C14 61(3) 5_755 . ? C12 C13 C14 51(2) 5_755 . ? C11 C13 P1 70.7(17) 5_755 . ? C12 C13 P1 160(2) 5_755 . ? C14 C13 P1 116(2) . . ? C12 C14 C11 82(3) 5_755 5_755 ? C12 C14 C13 44(2) 5_755 . ? C11 C14 C13 41.3(15) 5_755 . ? C15 C15 C16 92.1(9) 5_755 . ? C15 C15 C16 63.2(9) 5_755 5_755 ? C16 C15 C16 28.9(14) . 5_755 ? C15 C15 P1 78.9(5) 5_755 . ? C16 C15 P1 117.2(11) . . ? C16 C15 P1 108.4(11) 5_755 . ? C16 C16 C15 87.9(9) 5_755 . ? C16 C16 C15 63.2(9) 5_755 5_755 ? C15 C16 C15 24.7(11) . 5_755 ? C21 C21 C22 64.2(8) 4_775 . ? C21 C21 P2 69.9(7) 4_775 . ? C22 C21 P2 116.1(11) . . ? C21 C22 C21 51.6(16) 4_775 . ? C700 C100 C200 122.6(16) . 6 ? C700 C100 C200 122.6(16) . . ? C200 C100 C200 114(3) 6 . ? C300 C200 C100 123(3) . . ? C400 C300 C200 117(3) . . ? C300 C400 C300 125(5) . 6 ? _cod_database_code 1100602 _journal_paper_doi 10.1021/ic9710364