#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000261.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_4000261 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _publ_section_title ; (N,N,N',N'-tetramethylethylenediamine)bis-(dicyanomercury)copper(II) tetrachloromercurate(II) ; loop_ _publ_author_name 'Draper, Neil D.' 'Batchelor, Raymond J. ' 'Sih, Bryan C. ' 'Ye, Zuo-Guang ' 'Leznoff, Daniel' _chemical_formula_moiety 'Hg3 Cu Cl4 N6 C10 H16 ' _chemical_formula_sum 'Hg3 Cu Cl4 N6 C10 H16 ' _chemical_formula_weight 1027.39 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 m' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'y,-x,-z' '-x,-y,z' '-y,x,-z' '1/2-x,1/2+y,-z' '1/2-y,1/2-x,z' '1/2+x,1/2-y,-z' '1/2+y,1/2+x,z' _cell_length_a 10.9576(12) _cell_length_b 10.9576(12) _cell_length_c 9.8516(13) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 1182.87(20) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 48 _cell_measurement_theta_min 20.00 _cell_measurement_theta_max 24.50 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.885 _exptl_crystal_density_method ? _exptl_crystal_F_000 896.53 _exptl_absorpt_coefficient_mu 20.76 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0399 _exptl_absorpt_correction_T_max 0.1430 _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_standards_number 2 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 3.0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 2 0 -1 1 1 _diffrn_reflns_number 4008 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_reduction_process ? _reflns_number_total 1266 _reflns_number_observed 1081 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 1/(\s^2^(F)+0.0002F^2^) _refine_ls_extinction_coef 38.4(16) _refine_ls_extinction_method ; 'Larson 1970 Crystallographic Computing eq 22' ; _refine_ls_hydrogen_treatment constr _refine_ls_abs_structure_details 'Flack, 466 Friedel-pairs' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 1081 _refine_ls_number_parameters 65 _refine_ls_number_restraints 5 _refine_ls_R_factor_obs 0.022 _refine_ls_wR_factor_obs 0.024 _refine_ls_goodness_of_fit_obs 1.07 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean ? _refine_diff_density_max 1.0(2) _refine_diff_density_min -1.2(2) 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_type_symbol _atom_site_occupancy Hg1 0.224650(20) 0.275350(20) 0.53519(4) 0.04094(17) Uani ? S Hg 1. Hg2 0.00000 0.00000 0.50000 0.0581(4) Uani ? S Hg 1. Cu1 0.00000 0.50000 0.15147(16) 0.0342(7) Uani ? S Cu 1. Cl1 0.18900(18) 0.04264(18) 0.36975(24) 0.0535(11) Uani ? . Cl 1. N1 0.0919(6) 0.4081(6) 0.0018(11) 0.066(5) Uani ? S N 1. N3 0.0912(6) 0.4088(6) 0.2915(9) 0.038(4) Uani ? S N 1. N4 0.3367(6) 0.1633(6) 0.7995(10) 0.051(4) Uani ? S N 1. C1 0.0194(15) 0.4322(6) -0.1248(17) 0.084(7) Uiso ? . C 0.5 C20 0.0892(18) 0.2710(10) 0.0279(19) 0.067(3) Uiso ? . C 0.5 C21 0.2223(9) 0.4476(18) -0.0104(20) 0.067(3) Uiso ? . C 0.5 C3 0.1374(6) 0.3625(6) 0.3789(12) 0.036(4) Uani ? S C 1. C4 0.2967(6) 0.2033(6) 0.7053(11) 0.037(4) Uani ? S C 1. H11 0.0637(15) 0.4104(6) -0.2040(17) 0.32(8) Uiso ? . H 0.5 H12 -0.0536(15) 0.3857(6) -0.1203(17) 0.32(8) Uiso ? . H 0.5 H21 0.1361(18) 0.2517(10) 0.1061(19) 0.32(8) Uiso ? . H 0.5 H22 0.1225(18) 0.2304(10) -0.0488(19) 0.32(8) Uiso ? . H 0.5 H23 0.0073(18) 0.2452(10) 0.0412(19) 0.32(8) Uiso ? . H 0.5 H24 0.2627(9) 0.4313(18) 0.0730(20) 0.32(8) Uiso ? . H 0.5 H25 0.2259(9) 0.5326(18) -0.0292(20) 0.32(8) Uiso ? . H 0.5 H26 0.2611(9) 0.4037(18) -0.0815(20) 0.32(8) Uiso ? . H 0.5 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 _atom_site_aniso_type_symbol Hg1 0.04109(16) 0.04109(16) 0.04063(22) 0.00662(17) -0.00814(14) 0.00814(14) Hg Hg2 0.04852(23) 0.04852(23) 0.0773(6) 0.00000 0.00000 0.00000 Hg Cu1 0.0397(6) 0.0397(6) 0.0234(8) 0.0100(8) 0.00000 0.00000 Cu Cl1 0.0588(12) 0.0406(10) 0.0613(13) 0.0011(9) 0.0161(10) -0.0024(9) Cl N1 0.076(4) 0.076(4) 0.047(6) 0.013(6) 0.011(4) -0.011(4) N N3 0.037(3) 0.037(3) 0.040(5) 0.001(4) -0.003(3) 0.003(3) N N4 0.054(4) 0.054(4) 0.045(6) 0.012(4) -0.003(4) 0.003(4) N