#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/48/2104885.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_2104885 loop_ _publ_author_name 'Smeets, Stef' 'Parois, Pascal' 'B\"urgi, Hans-Beat' 'Lutz, Martin' _publ_section_title ; Temperature-dependent analysis of thermal motion, disorder and structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate ; _journal_coeditor_code BK5101 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 53 _journal_page_last 62 _journal_volume 67 _journal_year 2011 _chemical_formula_moiety 'C6 H24 N6 Zn, O4 S' _chemical_formula_sum 'C6 H24 N6 O4 S Zn' _chemical_formula_weight 341.74 _chemical_name_systematic ; ? ; _space_group_IT_number 163 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-P 3 2c' _symmetry_space_group_name_H-M 'P -3 1 c' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 8.9929(2) _cell_length_b 8.9929(2) _cell_length_c 9.6101(2) _cell_measurement_reflns_used 10072 _cell_measurement_temperature 290(2) _cell_measurement_theta_max 34.94 _cell_measurement_theta_min 2.12 _cell_volume 673.07(3) _computing_cell_refinement 'PEAKREF (Schreurs, 2005)' _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EVAL15 (Schreurs et al., 2010), SADABS-2008/1 (Sheldrick, 2008b)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008a)' _diffrn_ambient_temperature 290(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0106 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11155 _diffrn_reflns_theta_full 30.49 _diffrn_reflns_theta_max 30.49 _diffrn_reflns_theta_min 2.62 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_T_max 0.8724 _exptl_absorpt_correction_T_min 0.6267 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008b)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 360 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.619 _refine_diff_density_min -0.289 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 696 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0233 _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^)+(0.0402P)^2^+0.1924P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.0635 _reflns_number_gt 647 _reflns_number_total 696 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bk5101.cif _[local]_cod_data_source_block 1f _cod_database_code 2104885 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' 'x, x-y, -z+1/2' '-x+y, y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' '-x, -x+y, z-1/2' 'x-y, -y, z-1/2' 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 _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn1 0.6667 0.3333 0.2500 0.02240(13) Uani d S 1 . . N N1 0.45193(17) 0.30908(19) 0.12575(14) 0.0328(3) Uani d . 1 . . H H1N 0.432(3) 0.392(4) 0.136(3) 0.053(6) Uiso d . 1 . . H H2N 0.469(3) 0.304(3) 0.038(2) 0.050(6) Uiso d . 1 . . C C1 0.2960(2) 0.1532(2) 0.17146(18) 0.0375(3) Uani d . 1 . . H H1A 0.2929 0.0527 0.1314 0.045 Uiso calc R 1 . . H H1B 0.1951 0.1564 0.1402 0.045 Uiso calc R 1 . . S S1 0.3333 0.6667 0.2500 0.02259(16) Uani d SD 1 . . O O1 0.3543(12) 0.5644(9) 0.1464(5) 0.100(3) Uani d PD 0.33333 . . O O2 0.2843(11) 0.7782(10) 0.1825(6) 0.119(4) Uani d PD 0.33333 . . 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 Zn1 0.02248(15) 0.02248(15) 0.02224(19) 0.01124(7) 0.000 0.000 N1 0.0302(6) 0.0399(7) 0.0295(6) 0.0185(5) -0.0038(5) 0.0024(5) C1 0.0255(6) 0.0417(8) 0.0407(8) 0.0134(6) -0.0072(6) -0.0070(6) S1 0.0230(2) 0.0230(2) 0.0218(3) 0.01150(11) 0.000 0.000 O1 0.206(10) 0.116(6) 0.045(3) 0.131(7) 0.015(4) -0.008(3) O2 0.239(11) 0.159(8) 0.063(4) 0.177(9) 0.020(5) 0.028(4) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 N1 Zn1 N1 6_655 2_655 80.22(7) ? N1 Zn1 N1 6_655 5 93.02(5) ? N1 Zn1 N1 2_655 5 94.56(8) ? N1 Zn1 N1 6_655 . 170.09(8) ? N1 Zn1 N1 2_655 . 93.02(5) ? N1 Zn1 N1 5 . 80.22(7) ? N1 Zn1 N1 6_655 3_665 94.56(8) ? N1 Zn1 N1 2_655 3_665 93.02(5) ? N1 Zn1 N1 5 3_665 170.09(8) ? N1 Zn1 N1 . 3_665 93.02(5) ? N1 Zn1 N1 6_655 4_665 93.02(5) ? N1 Zn1 N1 2_655 4_665 170.09(8) ? N1 Zn1 N1 5 4_665 93.02(5) ? N1 Zn1 N1 . 4_665 94.56(8) ? N1 Zn1 N1 3_665 4_665 80.22(7) ? C1 N1 Zn1 . . 107.80(10) ? C1 N1 H1N . . 106.5(18) ? Zn1 N1 H1N . . 114.3(18) ? C1 N1 H2N . . 110.8(16) ? Zn1 N1 H2N . . 111.4(17) ? H1N N1 H2N . . 106(2) ? N1 C1 C1 . 5 109.14(11) ? N1 C1 H1A . . 109.9 ? C1 C1 H1A 5 . 109.9 ? N1 C1 H1B . . 109.9 ? C1 C1 H1B 5 . 109.9 ? H1A C1 H1B . . 108.3 ? O1 S1 O1 6 . 112.3(6) ? O1 S1 O2 6 . 110.7(5) ? O1 S1 O2 . . 108.7(3) ? O1 S1 O2 6 6 108.7(3) ? O1 S1 O2 . 6 110.7(5) ? O2 S1 O2 . 6 105.6(7) ? 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 Zn1 N1 6_655 2.1866(13) ? Zn1 N1 2_655 2.1866(13) ? Zn1 N1 5 2.1866(13) ? Zn1 N1 . 2.1866(13) ? Zn1 N1 3_665 2.1866(13) ? Zn1 N1 4_665 2.1867(13) ? N1 C1 . 1.469(2) ? N1 H1N . 0.86(3) ? N1 H2N . 0.86(2) ? C1 C1 5 1.512(3) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? S1 O1 4_665 1.430(4) ? S1 O1 6 1.430(4) ? S1 O1 . 1.430(4) ? S1 O1 5_565 1.430(4) ? S1 O1 2_665 1.430(4) ? S1 O1 3_565 1.430(4) ? S1 O2 5_565 1.436(5) ? S1 O2 . 1.436(5) ? S1 O2 3_565 1.436(5) ? S1 O2 6 1.436(5) ? S1 O2 2_665 1.436(5) ? S1 O2 4_665 1.436(5) ? 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 N1 H1N O1 . 0.86(3) 1.99(3) 2.846(6) 172(3) N1 H2N O2 9_655 0.86(2) 2.17(2) 3.029(6) 178(2) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 Zn1 N1 C1 2_655 . . . 79.15(13) ? N1 Zn1 N1 C1 5 . . . -14.96(8) ? N1 Zn1 N1 C1 3_665 . . . 172.34(10) ? N1 Zn1 N1 C1 4_665 . . . -107.24(11) ? Zn1 N1 C1 C1 . . . 5 42.21(18) ? _cod_database_fobs_code 2104885