#------------------------------------------------------------------------------ #$Date: 2011-03-06 05:03:40 +0200 (Sun, 06 Mar 2011) $ #$Revision: 13306 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/8102567.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_8102567 loop_ _publ_author_name 'Harald Euler' 'Hartmut Kutzke' 'Bruno Barbier' 'Armin Kirfel' _publ_section_title ; Refinement of crystal structure of copper acetate diammine, Cu(CH3COO)2 · 2NH3 ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 725 _journal_volume 224 _journal_year 2009 _chemical_formula_sum 'C4 H12 Cu N2 O4' _chemical_formula_weight 215.70 _chemical_name_systematic ; copper acetate diammine Cu(CH~3~COO)~2~.2NH~3~ ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'manual editing of SHELXL-97 -output file' _cell_angle_alpha 90.00 _cell_angle_beta 107.067(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.452(2) _cell_length_b 10.220(5) _cell_length_c 7.518(5) _cell_measurement_reflns_used 21 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 15.80 _cell_measurement_theta_min 10.89 _cell_volume 400.5(4) _computing_cell_refinement 'MSC TEXSAN v5.0' _computing_data_collection 'MSC TEXSAN v5.0' _computing_data_reduction 'REDUCE (Eichhorn, 1987)' _computing_molecular_graphics 'DIAMOND v3.1 [8]' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997) [7]' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997) [7]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990) [6]' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'RIGAKU AFC-6R' _diffrn_measurement_method 'Omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1378 _diffrn_reflns_theta_full 25.05 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_min 3.47 _diffrn_standards_decay_% 64.0 _diffrn_standards_interval_count 50 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.698 _exptl_absorpt_correction_T_max 0.6423 _exptl_absorpt_correction_T_min 0.4116 _exptl_absorpt_correction_type none _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 222 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.524 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.093 _refine_ls_extinction_coef 0.007(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 77 _refine_ls_number_reflns 714 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.935 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0315 _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^)+(0.0589P)^2^+0.0806P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0819 _reflns_number_gt 593 _reflns_number_total 714 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file 1267-2783.cff _[local]_cod_data_source_block cuatz _cod_database_code 8102567 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.5000 0.0000 0.5000 0.0246(3) Uani 1 2 d S . . O1 O 0.5756(4) -0.2589(2) 0.4947(3) 0.0419(6) Uani 1 1 d . . . O2 O 0.8328(3) -0.09392(17) 0.6105(2) 0.0302(5) Uani 1 1 d . . . N N 0.5946(6) 0.0168(3) 0.2666(4) 0.0307(6) Uani 1 1 d . . . C1 C 0.7929(5) -0.2152(2) 0.5724(3) 0.0266(6) Uani 1 1 d . . . C2 C 0.0205(6) -0.3046(4) 0.6245(5) 0.0415(8) Uani 1 1 d . . . H1 H 0.526(6) 0.073(4) 0.202(4) 0.033(10) Uiso 1 1 d . . . H4 H 0.983(7) -0.383(4) 0.603(5) 0.062(12) Uiso 1 1 d . . . H3 H 0.581(7) -0.054(4) 0.203(5) 0.037(10) Uiso 1 1 d . . . H2 H 0.746(9) 0.034(4) 0.293(5) 0.046(11) Uiso 1 1 d . . . H5 H 0.161(8) -0.268(4) 0.577(5) 0.078(11) Uiso 1 1 d . . . H6 H 0.100(11) -0.291(6) 0.752(8) 0.122(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0171(3) 0.0242(4) 0.0320(4) 0.00115(16) 0.0064(2) 0.00239(15) O1 0.0227(10) 0.0381(12) 0.0604(13) -0.0121(9) 0.0054(8) -0.0030(11) O2 0.0212(9) 0.0264(10) 0.0418(10) 0.0026(8) 0.0072(8) 0.0026(8) N 0.0266(16) 0.0317(17) 0.0341(14) 0.0048(12) 0.0093(12) 0.0073(13) C1 0.0235(14) 0.0285(16) 0.0299(14) 0.0029(12) 0.0113(11) 0.0016(12) C2 0.0293(17) 0.0320(17) 0.063(2) 0.0030(16) 0.0131(16) 0.0053(14) 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Cu N 180.0 3_656 . ? N Cu O2 91.77(11) 3_656 . ? N Cu O2 88.23(11) . . ? N Cu O2 88.23(11) 3_656 3_656 ? N Cu O2 91.77(11) . 3_656 ? O2 Cu O2 180.0 . 3_656 ? N Cu O1 90.51(10) 3_656 . ? N Cu O1 89.49(10) . . ? O2 Cu O1 53.77(7) . . ? O2 Cu O1 126.23(7) 3_656 . ? C1 O1 Cu 76.54(15) . . ? C1 O2 Cu 107.36(16) . . ? Cu N O1 122.63(13) . 2_655 ? Cu N O2 105.12(13) . 3_756 ? O1 N O2 95.32(11) 2_655 3_756 ? Cu N O1 120.58(14) . 4 ? O1 N O1 104.92(11) 2_655 4 ? O2 N O1 103.49(10) 3_756 4 ? Cu N H1 115(2) . . ? O1 N H1 11(2) 2_655 . ? O2 N H1 105(2) 3_756 . ? O1 N H1 106(2) 4 . ? Cu N H3 115(2) . . ? O1 N H3 109(2) 2_655 . ? O2 N H3 107(2) 3_756 . ? O1 N H3 6(2) 4 . ? H1 N H3 109(4) . . ? Cu N H2 108(3) . . ? O1 N H2 95(3) 2_655 . ? O2 N H2 4(3) 3_756 . ? O1 N H2 100(3) 4 . ? H1 N H2 105(4) . . ? H3 N H2 104(3) . . ? O1 C1 O2 122.1(2) . . ? O1 C1 C2 120.5(3) . 1_655 ? O2 C1 C2 117.4(2) . 1_655 ? C1 C2 H5 110(2) 1_455 . ? C1 C2 H6 106(4) 1_455 . ? H5 C2 H6 98(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N 1.977(3) 3_656 ? Cu N 1.977(3) . ? Cu O2 2.0047(17) . ? Cu O2 2.0047(17) 3_656 ? Cu O1 2.680(3) . ? O1 C1 1.240(3) . ? O2 C1 1.276(3) . ? N O1 2.984(4) 2_655 ? N O2 3.087(4) 3_756 ? N O1 3.318(4) 4 ? N H1 0.77(4) . ? N H3 0.86(4) . ? N H2 0.81(4) . ? C1 C2 1.497(4) 1_655 ? C2 C1 1.497(4) 1_455 ? C2 H5 1.00(4) . ? C2 H6 0.94(5) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N H1 O1 0.77(4) 2.23(4) 2.984(4) 166(3) 2_655 N H2 O2 0.81(4) 2.28(5) 3.087(4) 175(4) 3_756 N H3 O1 0.86(4) 2.46(4) 3.318(4) 172(3) 4