#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/48/2104889.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_2104889 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 Cu N6, O4 S' _chemical_formula_sum 'C6 H24 Cu N6 O4 S' _chemical_formula_weight 339.91 _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 8.95720(10) _cell_length_b 8.95720(10) _cell_length_c 9.59260(10) _cell_measurement_reflns_used 9343 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 34.97 _cell_measurement_theta_min 2.12 _cell_volume 666.517(13) _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 250(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 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0101 _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 9785 _diffrn_reflns_theta_full 30.46 _diffrn_reflns_theta_max 30.46 _diffrn_reflns_theta_min 2.63 _exptl_absorpt_coefficient_mu 1.813 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_correction_T_min 0.5794 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008b)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 358 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.515 _refine_diff_density_min -0.289 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 687 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.144 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0238 _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^)+(0.0310P)^2^+0.3143P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.0609 _reflns_number_gt 638 _reflns_number_total 687 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bk5101.cif _[local]_cod_data_source_block 2d _cod_original_cell_volume 666.517(16) _cod_database_code 2104889 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 Cu Cu1 0.6667 0.3333 0.2500 0.02025(13) Uani d S 1 . . N N1 0.4560(2) 0.3115(2) 0.12733(17) 0.0385(3) Uani d . 1 . . H H1N 0.436(3) 0.390(4) 0.135(3) 0.048(7) Uiso d . 1 . . H H2N 0.469(3) 0.304(3) 0.043(3) 0.056(7) Uiso d . 1 . . C C1 0.2980(2) 0.1544(2) 0.17132(18) 0.0361(3) Uani d . 1 . . H H1A 0.2946 0.0526 0.1303 0.043 Uiso calc R 1 . . H H1B 0.1962 0.1587 0.1396 0.043 Uiso calc R 1 . . S S1 0.3333 0.6667 0.2500 0.02154(16) Uani d SD 1 . . O O1 0.3551(12) 0.5636(9) 0.1464(5) 0.096(3) Uani d PD 0.33333 . . O O2 0.2847(11) 0.7790(10) 0.1813(7) 0.116(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 Cu1 0.02168(15) 0.02168(15) 0.01737(19) 0.01084(7) 0.000 0.000 N1 0.0427(8) 0.0376(7) 0.0347(7) 0.0198(6) 0.0076(6) 0.0034(6) C1 0.0266(7) 0.0402(8) 0.0370(8) 0.0134(6) -0.0056(6) -0.0050(6) S1 0.0227(2) 0.0227(2) 0.0193(3) 0.01133(11) 0.000 0.000 O1 0.191(9) 0.119(6) 0.045(3) 0.127(7) 0.001(4) -0.019(3) O2 0.222(11) 0.145(8) 0.075(4) 0.163(9) 0.019(5) 0.032(5) 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' 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' 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' 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 Cu1 N1 5 2_655 94.01(9) ? N1 Cu1 N1 5 . 80.96(8) ? N1 Cu1 N1 2_655 . 92.85(6) ? N1 Cu1 N1 5 4_665 92.85(6) ? N1 Cu1 N1 2_655 4_665 170.97(9) ? N1 Cu1 N1 . 4_665 94.01(9) ? N1 Cu1 N1 5 6_655 92.85(6) ? N1 Cu1 N1 2_655 6_655 80.96(8) ? N1 Cu1 N1 . 6_655 170.97(9) ? N1 Cu1 N1 4_665 6_655 92.85(6) ? N1 Cu1 N1 5 3_665 170.97(9) ? N1 Cu1 N1 2_655 3_665 92.85(6) ? N1 Cu1 N1 . 3_665 92.85(6) ? N1 Cu1 N1 4_665 3_665 80.96(8) ? N1 Cu1 N1 6_655 3_665 94.01(9) ? C1 N1 Cu1 . . 108.10(11) ? C1 N1 H1N . . 106.3(18) ? Cu1 N1 H1N . . 116.1(18) ? C1 N1 H2N . . 108.4(18) ? Cu1 N1 H2N . . 113.0(19) ? H1N N1 H2N . . 105(3) ? N1 C1 C1 . 5 108.44(12) ? N1 C1 H1A . . 110.0 ? C1 C1 H1A 5 . 110.0 ? N1 C1 H1B . . 110.0 ? C1 C1 H1B 5 . 110.0 ? H1A C1 H1B . . 108.4 ? O1 S1 O1 6 . 112.3(6) ? O1 S1 O2 6 . 110.8(5) ? O1 S1 O2 . . 108.6(3) ? O1 S1 O2 6 6 108.6(3) ? O1 S1 O2 . 6 110.8(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 Cu1 N1 5 2.1479(17) ? Cu1 N1 2_655 2.1479(17) ? Cu1 N1 . 2.1479(17) ? Cu1 N1 4_665 2.1479(17) ? Cu1 N1 6_655 2.1479(17) ? Cu1 N1 3_665 2.1479(17) ? N1 C1 . 1.473(2) ? N1 H1N . 0.81(3) ? N1 H2N . 0.83(3) ? C1 C1 5 1.513(3) ? C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? S1 O1 6 1.434(4) ? S1 O1 3_565 1.434(4) ? S1 O1 . 1.434(4) ? S1 O1 5_565 1.434(4) ? S1 O1 4_665 1.434(4) ? S1 O1 2_665 1.434(4) ? S1 O2 5_565 1.440(5) ? S1 O2 2_665 1.440(5) ? S1 O2 . 1.440(5) ? S1 O2 3_565 1.440(5) ? S1 O2 6 1.440(5) ? S1 O2 4_665 1.440(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 . 0.81(3) 2.02(3) 2.827(6) 173(3) N1 H2N O2 9_655 0.83(3) 2.19(3) 3.022(7) 180(3) 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 Cu1 N1 C1 5 . . . -15.06(8) ? N1 Cu1 N1 C1 2_655 . . . 78.55(15) ? N1 Cu1 N1 C1 4_665 . . . -107.32(12) ? N1 Cu1 N1 C1 3_665 . . . 171.55(11) ? Cu1 N1 C1 C1 . . . 5 42.26(19) ? _cod_database_fobs_code 2104889