#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003675.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_2003675 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1388 _journal_page_last 1390 _publ_section_title ; Urotropin-3-Diiod, Ur.3I~2~ ; _chemical_formula_moiety 'C6 H12 N4,3I2' _chemical_formula_sum 'C6 H12 I6 N4' _chemical_formula_structural '(CH2)6N4,3I2' _chemical_formula_weight 901.615(6) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, y+1/2' 'z+1/2, y+1/2, x+1/2' _symmetry_space_group_name_H-M 'R 3 c' _cell_length_a 9.841(2) _cell_length_b 9.841 _cell_length_c 9.841 _cell_angle_alpha 81.33(2) _cell_angle_beta 81.33 _cell_angle_gamma 81.33 _cell_volume 923.4(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 3.243 _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 12.74 _cell_measurement_theta_max 17.13 _exptl_absorpt_coefficient_mu 9.978 _cell_measurement_temperature 295 _exptl_crystal_description Rhomboeder _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.125 _exptl_crystal_colour rotschwarz _chemical_compound_source ; Umsetzung von Urotropiniumiodid UrHI mit iodges\"attigter Acetonitrill\"osung ; _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method 3\w/4\q _exptl_absorpt_correction_type 'empirisch' _exptl_absorpt_correction_T_min 0.6951 _exptl_absorpt_correction_T_max 0.9990 _diffrn_reflns_number 4182 _reflns_number_total 1222 _reflns_number_observed 1122 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3.9 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0262 _refine_ls_wR_factor_obs 0.069 _refine_ls_wR_factor_all 0.0705 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_number_reflns 1220 _refine_ls_number_parameters 51 _refine_ls_hydrogen_treatment 'Berechnete H-Lagen' _refine_ls_weighting_scheme 'calc w=1/[\s^2^(F~o~^2^)+(0.0426P)^2^+0.7916P]' _refine_ls_shift/esd_max 0.000 _refine_diff_density_max .5 _refine_diff_density_min -.5 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0166(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'I' 'I' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -.4742 1.811 '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 _refine_ls_abs_structure_details 'Flack (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 'Flack-Parameter, x = 0.01(10)' ##; ##MolEN (Fair, 1990) ##; ##; ## SCHAKAL92 (Keller, 1993), ORTEP (Davenport, Hall & Dreissig, 1990) ##; ##; ## ORFFE4 (Busing et al., 1976), PARST (Nardelli, 1983) ##; 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 0.31235(6) 0.72114(8) 0.12654(6) 0.0510(2) I2 1 0.30187(7) 0.97944(6) -0.02583(7) 0.0652(2) N1 1 0.2500(8) 0.2500 0.2500 0.063(3) N3 1 0.3217(7) 0.4728(6) 0.2610(7) 0.048(1) C2 1 0.2464(9) 0.3927(9) 0.1862(8) 0.054(2) H2A 1 0.1507 0.4353 0.1872 0.07(1) H2B 1 0.2885 0.3954 0.0904 0.07(1) C4 1 0.4678(8) 0.4074(9) 0.2572(8) 0.051(2) H4A 1 0.5119 0.4115 0.1618 0.07(1) H4B 1 0.5179 0.4573 0.3068 0.07(1) 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 0.0450(3) -0.0106(2) -0.0056(2) 0.0542(3) -0.0009(2) 0.0529(3) I2 0.0728(4) -0.0101(2) 0.0014(3) 0.0458(3) -0.0092(2) 0.0747(4) N1 0.064(3) -0.012(3) -0.012(3) 0.064(3) -0.012(3) 0.064(3) N3 0.047(3) -0.005(2) -0.006(2) 0.042(3) 0.003(3) 0.051(3) C2 0.049(4) -0.006(3) -0.011(3) 0.061(5) -0.005(4) 0.051(4) C4 0.043(4) -0.009(3) -0.002(3) 0.058(4) -0.006(3) 0.051(4)