#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202292.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202292 loop_ _publ_author_name 'Bramsen, Fabienne' 'Bond, Andrew D.' 'McKenzie, Christine J.' _publ_section_title ; Hydronium pentaaquacopper(II) triperchlorate ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i105 _journal_page_last i106 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(H3 O) [Cu (H2 O)5] (Cl O4)3' _chemical_formula_moiety 'H10 Cu O5 2+, H3 O 1+, 3Cl O4 1-' _chemical_formula_structural 'Cu (H2 O)5 (H3 O) (Cl O4)3' _chemical_formula_sum 'Cl3 Cu H13 O18' _chemical_formula_weight 470.99 _chemical_name_systematic ; Hydronium pentaaquacopper(II) triperchlorate ; _space_group_IT_number 154 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall 'P 32 2"' _symmetry_space_group_name_H-M 'P 32 2 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 10.1659(7) _cell_length_b 10.1659(7) _cell_length_c 13.1601(9) _cell_measurement_reflns_used 2728 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 26.02 _cell_measurement_theta_min 2.32 _cell_volume 1177.83(14) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 2000)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method 'thin-slice \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7204 _diffrn_reflns_theta_full 26.36 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 3.87 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.989 _exptl_absorpt_correction_T_max 0.826 _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2002)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 711 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.579 _refine_diff_density_min -0.545 _refine_ls_abs_structure_details 'Flack (1983), 671 Friedel pairs' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1610 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0451 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.6785P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.1114 _reflns_number_gt 1348 _reflns_number_total 1610 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file br6106.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'H13 Cl3 Cu O18' _cod_database_code 2202292 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 0.70337(9) 0.0000 0.1667 0.0232(2) Uani d S 1 . . Cu Cl1 0.17902(18) 0.54783(16) 0.14489(10) 0.0294(3) Uani d . 1 . . Cl Cl2 0.0840(2) 0.0000 0.1667 0.0328(5) Uani d S 1 . . Cl O1 0.8015(6) 0.1870(6) 0.0803(4) 0.0546(13) Uani d D 1 . . O H1A 0.751(6) 0.185(9) 0.025(3) 0.066 Uiso d D 1 . . H H1B 0.9000(17) 0.238(8) 0.067(4) 0.066 Uiso d D 1 . . H O2 0.7775(13) 0.1245(8) 0.2906(5) 0.139(4) Uani d D 1 . . O H2A 0.848(12) 0.220(5) 0.281(9) 0.166 Uiso d D 1 . . H H2B 0.740(14) 0.112(13) 0.353(4) 0.166 Uiso d D 1 . . H O3 0.4752(7) 0.0000 0.1667 0.104(4) Uani d SD 1 . . O H3A 0.467(2) 0.0813(17) 0.173(9) 0.125 Uiso d D 1 . . H O4 0.0663(5) 0.4543(5) 0.2197(3) 0.0448(12) Uani d . 1 . . O O5 0.1916(8) 0.6937(6) 0.1465(4) 0.0688(19) Uani d . 1 . . O O6 0.1263(8) 0.4798(7) 0.0462(4) 0.0722(17) Uani d . 1 . . O O7 0.3184(6) 0.5568(8) 0.1644(5) 0.0780(19) Uani d . 1 . . O O8 0.0735(12) 0.1327(11) 0.1774(5) 0.118(3) Uani d . 1 . . O O9 0.1730(6) 0.0179(5) 0.0797(3) 0.0469(12) Uani d . 1 . . O O100 0.3280(5) 0.3280(5) 0.0000 0.0440(16) Uani d S 1 . . O 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 Cu1 0.0238(3) 0.0229(5) 0.0227(4) 0.0114(3) -0.0036(2) -0.0071(4) Cl1 0.0287(8) 0.0273(7) 0.0307(6) 0.0129(6) 0.0003(6) -0.0033(5) Cl2 0.0326(8) 0.0484(13) 0.0227(10) 0.0242(7) 0.0016(4) 0.0032(9) O1 0.047(3) 0.055(3) 0.050(3) 0.016(3) 0.000(2) -0.001(2) O2 0.220(11) 0.055(4) 0.052(4) 0.002(5) -0.001(5) -0.021(3) O3 0.036(3) 0.083(6) 0.208(12) 0.042(3) 0.051(4) 0.101(8) O4 0.047(3) 0.044(3) 0.045(3) 0.024(2) 0.010(2) 0.008(2) O5 0.114(5) 0.040(3) 0.062(3) 0.047(3) 0.018(3) 0.005(3) O6 0.084(4) 0.079(4) 0.037(2) 0.028(3) 0.004(3) -0.018(3) O7 0.032(3) 0.092(5) 0.113(5) 0.032(4) -0.004(3) -0.005(4) O8 0.239(10) 0.180(8) 0.056(3) 0.196(8) 0.022(5) 0.016(5) O9 0.064(3) 0.039(2) 0.036(2) 0.024(2) 0.017(2) 0.0052(19) O100 0.042(3) 0.042(3) 0.043(3) 0.018(3) -0.0010(13) 0.0010(13) 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 Cu1 O2 . 1.969(6) yes Cu1 O2 5 1.969(6) yes Cu1 O1 5 2.001(5) yes Cu1 O1 . 2.001(5) yes Cu1 O3 . 2.320(7) yes Cu1 O8 1_655 3.305(10) yes Cu1 O8 5_655 3.305(10) yes Cl1 O7 . 1.398(5) no Cl1 O5 . 1.423(5) no Cl1 O6 . 1.443(5) no Cl1 O4 . 1.449(5) no Cl2 O8 5 1.412(6) no Cl2 O8 . 1.412(6) no Cl2 O9 5 1.413(4) no Cl2 O9 . 1.413(4) no O1 H1A . 0.890(10) no O1 H1B . 0.890(10) no O2 H2A . 0.880(10) no O2 H2B . 0.880(10) no O3 H3A . 0.870(10) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 Cu1 O2 . 5 172.9(8) yes O2 Cu1 O1 . 5 89.2(3) yes O2 Cu1 O1 5 5 90.7(3) yes O2 Cu1 O1 . . 90.7(3) no O2 Cu1 O1 5 . 89.2(3) no O1 Cu1 O1 5 . 177.3(3) yes O2 Cu1 O3 . . 93.5(4) yes O2 Cu1 O3 5 . 93.5(4) no O1 Cu1 O3 5 . 91.34(17) yes O1 Cu1 O3 . . 91.34(17) no O2 Cu1 O8 . 1_655 73.2(4) yes O2 Cu1 O8 5 1_655 100.0(4) yes O1 Cu1 O8 5 1_655 104.2(2) yes O1 Cu1 O8 . 1_655 73.2(2) no O3 Cu1 O8 . 1_655 159.15(13) yes O2 Cu1 O8 . 5_655 100.0(4) no O2 Cu1 O8 5 5_655 73.2(4) no O1 Cu1 O8 5 5_655 73.2(2) no O1 Cu1 O8 . 5_655 104.2(2) no O3 Cu1 O8 . 5_655 159.15(13) no O8 Cu1 O8 1_655 5_655 41.7(3) yes O7 Cl1 O5 . . 111.7(4) no O7 Cl1 O6 . . 108.5(4) no O5 Cl1 O6 . . 109.3(4) no O7 Cl1 O4 . . 111.2(3) no O5 Cl1 O4 . . 107.7(3) no O6 Cl1 O4 . . 108.4(3) no O8 Cl2 O8 5 . 112.8(9) no O8 Cl2 O9 5 5 107.9(3) no O8 Cl2 O9 . 5 109.3(4) no O8 Cl2 O9 5 . 109.3(4) no O8 Cl2 O9 . . 107.9(3) no O9 Cl2 O9 5 . 109.7(4) no Cu1 O1 H1A . . 116(5) no Cu1 O1 H1B . . 123(5) no H1A O1 H1B . . 109.0(17) no Cu1 O2 H2A . . 116(8) no Cu1 O2 H2B . . 132(8) no H2A O2 H2B . . 110.4(18) no Cu1 O3 H3A . . 124.5(11) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1B O6 1_655 0.890(10) 2.40(5) 3.184(8) 148(7) y O1 H1A O5 4 0.890(10) 2.34(3) 3.188(7) 161(6) y O2 H2A O4 1_655 0.880(10) 2.44(3) 3.299(10) 165(11) y O2 H2B O7 6_655 0.880(10) 2.58(7) 3.343(11) 145(10) y O3 H3A O5 5_665 0.870(10) 2.160(10) 3.017(7) 168(2) y _cod_database_fobs_code 2202292