#------------------------------------------------------------------------------ #$Date: 2011-09-28 16:24:46 +0200 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003404.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_2003404 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 562 _journal_page_last 565 _publ_section_title ; Kalium-2.2-Crypt-triiodid* ; _chemical_formula_moiety '(K 1+), (C12 H26 N2 O4), (I3 1-)' _chemical_formula_sum 'C12 H26 I3 K N2 O4' _chemical_formula_structural '(K 1+), (C12 H26 N2 O4), (I3 1-)' _chemical_formula_analytical '(K 1+), (C12 H26 N2 O4), (I3 1-)' _chemical_formula_weight 682.16(1) _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.121(2) _cell_length_b 8.475(2) _cell_length_c 18.357(2) _cell_angle_alpha 90 _cell_angle_beta 105.60(2) _cell_angle_gamma 90 _cell_volume 2265.8(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.63 _cell_measurement_theta_max 22.30 _exptl_absorpt_coefficient_mu 4.336 _cell_measurement_temperature 293(2) _exptl_crystal_description 'schiefes Prisma' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_colour braun _chemical_compound_source ; erstmalige Darstellung im st\"ochiometrischen Ansatz aus den Komponenten KI, I~2~, 2.2-Crypt. ; _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w/\q _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8473 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 6031 _reflns_number_total 1987 _reflns_number_observed 1726 _reflns_observed_criterion 'F~o~>4\s(F~o~)' _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% -12.7 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0332 _refine_ls_wR_factor_obs 0.1003 _refine_ls_wR_factor_all 0.1032 _refine_ls_goodness_of_fit_obs 1.534 _refine_ls_goodness_of_fit_all 1.465 _refine_ls_number_reflns 1987 _refine_ls_number_parameters 105 _refine_ls_hydrogen_treatment 'refU' _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(F~o~^2^) + 0.0507P)^2^] where' _refine_ls_shift/esd_max 0.0005 _refine_diff_density_max .581 _refine_diff_density_min -.746 _refine_ls_extinction_method SHELXL93 _refine_ls_extinction_coef 0.00019(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0106 .0060 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0033 .0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 'I' 'I' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -.4742 1.811 'K' 'K' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .2009 .2494 ##; ##BEGIN, STDPLT, CHORT, PSI, EAC ##(SDP-Plus V1.1B, Frenz, 1978) ##; ##; ##ORFFE4 (Busing, Martin, Levy, Brown, Johnson & Thiessen, 1977), ##PARST (Nardelli, 1983), ##KRISTALL-ST (Tebbe, 1992) ##; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv I1 1 .75 .25 .5 0.0599(2) I2 1 0.88174(3) 0.32356(7) 0.64366(2) 0.0920(2) K 1 .5 0 0 0.0595(4) N1 1 0.4832(3) -0.2890(5) 0.0717(2) 0.0505(9) H1 1 0.5235(3) -0.3380(5) 0.0511(2) 0.099(6) C2 1 0.3965(5) -0.3621(9) 0.0451(4) 0.110(3) H2A 1 0.3514(5) -0.3062(9) 0.0641(4) 0.099(6) H2B 1 0.3997(5) -0.4701(9) 0.0631(4) 0.099(6) C3 1 0.3692(6) -0.3603(8) -0.0378(4) 0.106(3) H3A 1 0.4163(6) -0.4107(8) -0.0565(4) 0.099(6) H3B 1 0.3127(6) -0.4196(8) -0.0563(4) 0.099(6) O4 1 0.3559(2) -0.2050(5) -0.0653(2) 0.0669(9) C5 1 0.3213(4) -0.1990(8) -0.1458(3) 0.0703(14) H5A 1 0.2629(4) -0.2537(8) -0.1613(3) 0.099(6) H5B 1 0.3639(4) -0.2510(8) -0.1691(3) 0.099(6) C6 1 0.3092(3) -0.0306(7) -0.1708(2) 0.0650(14) H6A 1 0.2799(3) -0.0263(7) -0.2247(2) 0.099(6) H6B 1 0.2696(3) 0.0226(7) -0.1448(2) 0.099(6) O7 1 0.3974(2) 0.0494(5) -0.1545(2) 0.0738(11) C8 1 0.3906(3) 0.2142(7) -0.1740(2) 0.0624(14) H8A 1 0.3497(3) 0.2659(7) -0.1488(2) 0.099(6) H8B 1 0.3647(3) 0.2256(7) -0.2281(2) 0.099(6) C9 1 0.4821(4) 0.2914(8) -0.1513(3) 0.074(2) H9A 1 0.5242(4) 0.2363(8) -0.1741(3) 0.099(6) H9B 1 0.4769(4) 0.3996(8) -0.1691(3) 0.099(6) 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 I1 0.0671(3) 0.0053(2) 0.0341(2) 0.0522(3) 0.0014(2) 0.0696(3) I2 0.0804(3) -0.0298(3) 0.0279(2) 0.1159(5) -0.0190(2) 0.0831(3) K 0.0618(8) -0.0178(7) -0.0073(5) 0.0623(10) 0.0076(6) 0.0419(6) N1 0.054(2) -0.013(2) 0.0039(15) 0.049(2) 0.009(2) 0.043(2) C2 0.101(5) -0.050(4) -0.012(4) 0.097(5) 0.045(4) 0.109(5) C3 0.121(6) -0.039(4) -0.030(4) 0.061(4) 0.010(3) 0.100(5) O4 0.070(2) -0.021(2) -0.002(2) 0.062(2) -0.001(2) 0.059(2) C5 0.066(3) -0.017(3) -0.009(2) 0.076(4) -0.014(3) 0.054(3) C6 0.048(2) 0.000(3) -0.011(2) 0.091(4) -0.010(2) 0.043(2) O7 0.064(2) 0.004(2) 0.0025(15) 0.089(3) 0.003(2) 0.060(2) C8 0.062(3) 0.010(3) 0.003(2) 0.078(4) 0.016(2) 0.041(2) C9 0.080(4) 0.004(3) 0.011(2) 0.087(4) 0.022(3) 0.052(3) _cod_database_code 2003404