#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/48/2104887.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_2104887 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 8.94450(10) _cell_length_b 8.94450(10) _cell_length_c 9.58260(10) _cell_measurement_reflns_used 9618 _cell_measurement_temperature 210(2) _cell_measurement_theta_max 34.97 _cell_measurement_theta_min 2.13 _cell_volume 663.936(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 210(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 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0102 _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 9739 _diffrn_reflns_theta_full 30.49 _diffrn_reflns_theta_max 30.49 _diffrn_reflns_theta_min 2.63 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_T_max 0.9404 _exptl_absorpt_correction_T_min 0.5807 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'SADABS-2008/1 (Sheldrick, 2008b)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.700 _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 0.458 _refine_diff_density_min -0.264 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 685 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.142 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0219 _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^)+(0.0302P)^2^+0.2851P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.0570 _reflns_number_gt 637 _reflns_number_total 685 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bk5101.cif _[local]_cod_data_source_block 2b _cod_original_cell_volume 663.936(16) _cod_database_code 2104887 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 0.01760(12) Uani d S 1 . . N N1 0.4559(2) 0.31159(19) 0.12711(15) 0.0352(3) Uani d . 1 . . H H1N 0.435(3) 0.390(3) 0.135(2) 0.047(6) Uiso d . 1 . . H H2N 0.468(3) 0.304(3) 0.042(2) 0.051(6) Uiso d . 1 . . C C1 0.29761(19) 0.1542(2) 0.17121(16) 0.0319(3) Uani d . 1 . . H H1A 0.2942 0.0522 0.1302 0.038 Uiso calc R 1 . . H H1B 0.1956 0.1584 0.1394 0.038 Uiso calc R 1 . . S S1 0.3333 0.6667 0.2500 0.01877(15) Uani d SD 1 . . O O1 0.3531(11) 0.5622(9) 0.1458(5) 0.087(2) Uani d PD 0.33333 . . O O2 0.2842(11) 0.7787(9) 0.1813(6) 0.107(3) 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 0.01900(14) 0.01900(14) 0.01480(17) 0.00950(7) 0.000 0.000 N1 0.0385(7) 0.0341(7) 0.0318(6) 0.0173(6) 0.0084(5) 0.0036(5) C1 0.0240(6) 0.0358(7) 0.0319(7) 0.0120(5) -0.0045(5) -0.0041(6) S1 0.0200(2) 0.0200(2) 0.0163(3) 0.01000(10) 0.000 0.000 O1 0.177(8) 0.108(5) 0.037(2) 0.117(6) -0.002(3) -0.018(3) O2 0.212(10) 0.139(7) 0.064(3) 0.157(8) 0.018(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' 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 6_655 4_665 92.82(5) ? N1 Cu1 N1 6_655 5 92.82(5) ? N1 Cu1 N1 4_665 5 92.82(5) ? N1 Cu1 N1 6_655 . 171.00(8) ? N1 Cu1 N1 4_665 . 94.02(8) ? N1 Cu1 N1 5 . 81.02(7) ? N1 Cu1 N1 6_655 3_665 94.02(8) ? N1 Cu1 N1 4_665 3_665 81.02(7) ? N1 Cu1 N1 5 3_665 171.00(8) ? N1 Cu1 N1 . 3_665 92.82(5) ? N1 Cu1 N1 6_655 2_655 81.02(7) ? N1 Cu1 N1 4_665 2_655 171.00(8) ? N1 Cu1 N1 5 2_655 94.02(8) ? N1 Cu1 N1 . 2_655 92.82(5) ? N1 Cu1 N1 3_665 2_655 92.82(5) ? C1 N1 Cu1 . . 108.04(10) ? C1 N1 H1N . . 105.8(17) ? Cu1 N1 H1N . . 115.9(17) ? C1 N1 H2N . . 108.0(17) ? Cu1 N1 H2N . . 113.4(18) ? H1N N1 H2N . . 105(2) ? N1 C1 C1 . 5 108.45(11) ? 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 . 111.5(6) ? O1 S1 O2 6 . 111.4(5) ? O1 S1 O2 . . 108.3(3) ? O2 S1 O2 . 6 105.8(7) ? O1 S1 O2 6 6 108.3(3) ? O1 S1 O2 . 6 111.4(5) ? 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 6_655 2.1479(16) ? Cu1 N1 4_665 2.1479(16) ? Cu1 N1 5 2.1479(16) ? Cu1 N1 . 2.1479(16) ? Cu1 N1 3_665 2.1479(16) ? Cu1 N1 2_655 2.1479(16) ? N1 C1 . 1.474(2) ? N1 H1N . 0.81(3) ? N1 H2N . 0.83(2) ? C1 C1 5 1.513(3) ? C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? S1 O1 4_665 1.438(4) ? S1 O1 5_565 1.438(4) ? S1 O1 6 1.438(4) ? S1 O1 . 1.438(4) ? S1 O1 2_665 1.438(4) ? S1 O1 3_565 1.438(4) ? S1 O2 . 1.439(4) ? S1 O2 6 1.439(4) ? S1 O2 4_665 1.439(4) ? S1 O2 5_565 1.439(4) ? S1 O2 3_565 1.439(4) ? S1 O2 2_665 1.439(4) ? 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) 2.01(3) 2.821(5) 172(2) N1 H2N O2 9_655 0.83(2) 2.19(2) 3.017(6) 179(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 Cu1 N1 C1 4_665 . . . -107.29(11) ? N1 Cu1 N1 C1 5 . . . -15.07(7) ? N1 Cu1 N1 C1 3_665 . . . 171.52(10) ? N1 Cu1 N1 C1 2_655 . . . 78.56(13) ? Cu1 N1 C1 C1 . . . 5 42.28(17) ? _cod_database_fobs_code 2104887