#------------------------------------------------------------------------------ #$Date: 2008-02-29 13:03:34 +0200 (Fri, 29 Feb 2008) $ #$Revision: 179 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2015334.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_2015334 loop_ _publ_author_name 'Nishikiori, Shin-ichi' 'Sekiya, Ryo' 'Hosoya, Kazumasa' _publ_section_title ; Cu~3~(CN)~4~(NH~3~)~2~Hg(CN)~2~: a novel interpenetrating framework formed with Cu^I^, Cu^II^, Hg^II^ and cyanide bridges ; _journal_coeditor_code SQ3012 _journal_issue 5 _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first i32 _journal_page_last i34 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Cu3 Hg (C N)6 (N H3)2]' _chemical_formula_moiety 'C6 H6 Cu3 Hg N8' _chemical_formula_structural 'Cu3 (CN)4 (NH3)2 Hg (CN)2' _chemical_formula_sum 'C6 H6 Cu3 Hg N8' _chemical_formula_weight 581.40 _chemical_name_systematic ; poly[diamminehexa-\m-cyano-dicopper(I)copper(II)mercury(II)] ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 116.00(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.915(5) _cell_length_b 8.095(4) _cell_length_c 10.572(6) _cell_measurement_reflns_used 3838 _cell_measurement_temperature 153 _cell_measurement_theta_max 29.96 _cell_measurement_theta_min 4.29 _cell_volume 685.7(7) _computing_cell_refinement PROCESS-AUTO _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction PROCESS-AUTO _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 153 _diffrn_detector_area_resol_mean 10.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID imaging-plate' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3830 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 3.55 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 15.733 _exptl_absorpt_correction_T_max 0.177 _exptl_absorpt_correction_T_min 0.088 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(NUMABS; Higashi, 1999)' _exptl_crystal_colour 'dark blue' _exptl_crystal_density_diffrn 2.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 530 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _refine_diff_density_max 3.214 _refine_diff_density_min -2.018 _refine_ls_extinction_coef 0.0103(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 1071 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.123 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0301 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.6087P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.0853 _reflns_number_gt 1071 _reflns_number_total 1071 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sq3012.cif loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 -x,-y,-z 4 x,-y,z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,z loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Hg Hg1 1.0000 0.0000 0.5000 0.01986(17) Uani d S 1 Cu Cu1 0.32327(10) 0.0000 0.39352(8) 0.0240(2) Uani d S 1 Cu Cu2 0.5000 0.0000 0.0000 0.0236(2) Uani d S 1 C X1 0.2688(6) 0.1954(6) 0.4734(5) 0.0264(8) Uani d P 0.50 N X11 0.2688(6) 0.1954(6) 0.4734(5) 0.0264(8) Uani d P 0.50 C C2 0.3934(9) 0.0000 0.2459(7) 0.0249(12) Uani d S 1 N N2 0.4355(8) 0.0000 0.1565(6) 0.0292(12) Uani d S 1 N N3 0.5000 0.2513(9) 0.0000 0.0384(15) Uani d S 1 H H1 0.6040 0.2929 -0.0051 0.058 Uiso calc PR 0.50 H H2 0.4978 0.2929 0.0892 0.058 Uiso calc PR 0.50 H H3 0.3982 0.2929 -0.0841 0.058 Uiso calc PR 0.50 C C4 0.8857(8) 0.0000 0.2844(7) 0.0252(12) Uani d S 1 N N4 0.8263(10) 0.0000 0.1651(7) 0.0414(17) Uani d S 1 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 Hg1 0.0184(2) 0.0222(2) 0.0185(2) 0.000 0.00768(13) 0.000 Cu1 0.0247(4) 0.0270(4) 0.0216(4) 0.000 0.0114(3) 0.000 Cu2 0.0309(6) 0.0228(5) 0.0204(5) 0.000 0.0143(4) 0.000 X1 0.0293(19) 0.0198(17) 0.036(2) -0.0040(15) 0.0196(17) -0.0020(16) X11 0.0293(19) 0.0198(17) 0.036(2) -0.0040(15) 0.0196(17) -0.0020(16) C2 0.028(3) 0.024(3) 0.026(3) 0.000 0.014(2) 0.000 N2 0.034(3) 0.031(3) 0.023(3) 0.000 0.013(2) 0.000 N3 0.049(4) 0.030(3) 0.051(4) 0.000 0.035(3) 0.000 C4 0.019(3) 0.030(3) 0.022(3) 0.000 0.006(2) 0.000 N4 0.044(4) 0.052(4) 0.021(3) 0.000 0.008(3) 0.000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 C4 . 2.049(7) yes Cu1 X1 . 1.952(5) yes Cu1 C2 . 1.919(8) yes Cu2 N2 . 1.975(7) yes Cu2 N3 . 2.034(7) yes Cu2 N4 . 2.657(9) yes X1 X1 7_556 1.172(9) yes N2 C2 . 1.160(10) yes N4 C4 . 1.134(9) yes N3 H1 . 1.01 no N3 H2 . 1.01 no N3 H3 . 1.01 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cu1 X1 X1 . 7_556 174.8(6) yes Cu1 C2 N2 . . 179.9(7) yes X1 Cu1 X1 4_555 . 108.3(2) yes X1 Cu1 C2 . . 125.69(15) yes Cu2 N2 C2 . . 178.3(7) yes Cu2 N4 C4 . . 125.0(7) yes N2 Cu2 N3 . . 90.00(2) yes N2 Cu2 N4 . . 95.0(3) yes N2 Cu2 N4 . 3_655 85.0(3) yes N3 Cu2 N4 . . 90.00(2) yes Hg1 C4 N4 . . 178.3(8) yes Cu2 N3 H1 . . 109.0 no Cu2 N3 H2 . . 109.0 no Cu2 N3 H3 . . 109.0 no H1 N3 H2 . . 109.0 no H1 N3 H3 . . 109.0 no H2 N3 H3 . . 109.0 no