#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003016.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_2003016 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 663 _journal_page_last 670 _chemical_formula_sum 'C6 H14 I2 N2 O2 Zn' _[local]_cod_chemical_formula_sum_orig '[Zn I2 (C3 H7 N O )2 ]' _chemical_formula_weight 465.36 _symmetry_cell_setting Monoclinic _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 C2/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 14.005(8) _cell_length_b 13.697(6) _cell_length_c 15.755(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.88(3) _cell_angle_gamma 90.00 _cell_volume 2824(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.36 _cell_measurement_theta_max 12.49 _cell_measurement_temperature 233(2) _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 6.092 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_T_max 0.901 _diffrn_ambient_temperature 233(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4 four-circle' _diffrn_measurement_method \w _diffrn_reflns_number 3384 _diffrn_reflns_av_R_equivalents 0.0094 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'No decay; steady +/-2.5' _reflns_number_total 3236 _reflns_number_observed 2310 _reflns_observed_criterion I>2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_obs 0.0490 _refine_ls_wR_factor_all 0.1183 _refine_ls_wR_factor_obs 0.1059 _refine_ls_goodness_of_fit_all 1.081 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.152 _refine_ls_number_reflns 3236 _refine_ls_number_parameters 132 _refine_ls_number_restraints 7 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.0436P)^2^+25.8561P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.994 _refine_diff_density_min -1.359 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol I1 0.17690(4) 0.03893(4) 0.15652(4) 0.0583(2) Uani d . 1 . I I2 0.43661(5) -0.11479(5) 0.36062(4) 0.0735(2) Uani d . 1 . I Zn 0.25471(7) -0.11222(6) 0.24758(6) 0.0443(2) Uani d . 1 . Zn O1 0.2377(4) -0.2259(4) 0.1629(3) 0.0462(12) Uani d . 1 . O O2 0.1616(5) -0.1526(4) 0.3112(4) 0.062(2) Uani d . 1 . O N1 0.3023(5) -0.3460(4) 0.1020(4) 0.0449(14) Uani d . 1 . N N2 0.0850(6) -0.2627(6) 0.3719(6) 0.070(2) Uani d . 1 . N C1 0.3098(6) -0.2720(5) 0.1565(5) 0.046(2) Uani d . 1 . C H1 0.3758(6) -0.2527(5) 0.1938(5) 0.055 Uiso calc R 1 . H C2 0.3927(7) -0.3996(8) 0.1023(8) 0.082(3) Uani d . 1 . C H2A 0.387(3) -0.413(4) 0.0402(8) 0.098 Uiso calc R 1 . H H2B 0.398(3) -0.461(2) 0.135(4) 0.098 Uiso calc R 1 . H H2C 0.4533(9) -0.361(2) 0.132(4) 0.098 Uiso calc R 1 . H C3 0.2028(7) -0.3831(7) 0.0446(6) 0.067(2) Uani d . 1 . C H3A 0.184(2) -0.437(3) 0.0748(18) 0.080 Uiso calc R 1 . H H3B 0.2063(13) -0.405(4) -0.0127(16) 0.080 Uiso calc R 1 . H H3C 0.1523(11) -0.3315(13) 0.033(3) 0.080 Uiso calc R 1 . H C4 0.1397(7) -0.2361(7) 0.3231(7) 0.064(2) Uani d . 1 . C H4 0.1639(7) -0.2859(7) 0.2950(7) 0.077 Uiso calc R 1 . H C6 0.0454(9) -0.1903(8) 0.4161(7) 0.082(3) Uani d . 1 . C H6A 0.092(3) -0.182(4) 0.4781(15) 0.099 Uiso calc R 1 . H H6B -0.021(2) -0.211(2) 0.416(4) 0.099 Uiso calc R 1 . H H6C 0.038(5) -0.1288(15) 0.384(3) 0.099 Uiso calc R 1 . H C5 0.053(3) -0.3676(12) 0.373(3) 0.109(10) Uani d P 0.81(6) 2 C H51 0.014(3) -0.3738(12) 0.413(3) 0.163 Uiso calc PR 0.81(6) 2 H H52 0.113(3) -0.4085(12) 0.396(3) 0.163 Uiso calc PR 0.81(6) 2 H H53 0.012(3) -0.3879(12) 0.312(3) 0.163 Uiso calc PR 0.81(6) 2 H 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 I1 0.0605(3) 0.0453(3) 0.0672(4) 0.0066(3) 0.0206(3) 0.0046(3) I2 0.0570(4) 0.0836(5) 0.0629(4) 0.0074(3) 0.0007(3) -0.0174(3) Zn 0.0462(5) 0.0420(5) 0.0494(5) 0.0007(4) 0.0226(4) -0.0022(4) O1 0.038(3) 0.043(3) 0.058(3) 0.003(2) 0.017(2) -0.011(2) O2 0.073(4) 0.051(3) 0.081(4) -0.003(3) 0.049(3) -0.001(3) N1 0.047(3) 0.046(3) 0.046(3) -0.001(3) 0.022(3) -0.003(3) N2 0.080(5) 0.060(5) 0.094(6) 0.012(4) 0.058(5) 0.024(4) C1 0.046(4) 0.043(4) 0.050(4) 0.000(3) 0.019(3) -0.006(3) C2 0.066(6) 0.076(7) 0.109(8) 0.010(5) 0.037(6) -0.033(6) C3 0.065(5) 0.064(6) 0.073(6) -0.019(5) 0.027(5) -0.025(5) C4 0.069(6) 0.053(5) 0.084(6) 0.016(4) 0.043(5) 0.012(5) C6 0.105(8) 0.080(7) 0.088(7) -0.022(6) 0.065(7) -0.017(6) C5 0.16(2) 0.066(10) 0.15(2) -0.003(11) 0.11(2) 0.020(11)