#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2223379.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_2223379 loop_ _publ_author_name 'Lu, Jing' _publ_section_title ; Tris(ethylenediamine)manganese(II) sulfate ; _journal_coeditor_code HB5060 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1187 _journal_volume 65 _journal_year 2009 _chemical_formula_iupac '[Mn (C2 H8 N2 )3] S O4' _chemical_formula_moiety 'C6 H24 Mn N6 +, O4 S -' _chemical_formula_sum 'C6 H24 Mn N6 O4 S' _chemical_formula_weight 331.31 _chemical_name_systematic ; Tris(ethylenediamine)manganese(II) sulfate ; _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 geom _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 2 _cell_length_a 8.9460(13) _cell_length_b 8.9460(13) _cell_length_c 9.6230(19) _cell_measurement_reflns_used 2640 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.99 _cell_measurement_theta_min 2.63 _cell_volume 666.96(19) _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_collection 'SMART (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2640 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.63 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_T_max 0.736 _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 350 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.720 _refine_diff_density_min -0.630 _refine_ls_extinction_coef 0.051(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXS97 (Sheldrick, 2008)' _refine_ls_goodness_of_fit_ref 1.549 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 44 _refine_ls_number_reflns 402 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.894 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0575 _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^)+(0.0637P)^2^+1.2291P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1567 _refine_ls_wR_factor_ref 0.1593 _reflns_number_gt 386 _reflns_number_total 402 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hb5060.cif _[local]_cod_data_source_block I _cod_database_code 2223379 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+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_group Mn Mn1 0.3333 0.6667 0.7500 0.0200(8) Uani d SU 1 . S S1 0.3333 0.6667 0.2500 0.0332(10) Uani d S 1 . O O1 0.489(3) 0.813(4) 0.186(2) 0.051(4) Uani d P 0.220(12) 1 O O2 0.489(3) 0.721(6) 0.163(3) 0.051(4) Uani d P 0.210(13) 2 O O3 0.373(6) 0.799(3) 0.146(3) 0.051(4) Uani d P 0.203(14) 3 O O4 0.3333 0.6667 0.114(9) 0.051(4) Uani d SP 0.10(2) 4 N N1 0.3136(7) 0.4590(8) 0.8712(6) 0.0427(14) Uani d U 1 . H H1A 0.4072 0.4479 0.8581 0.051 Uiso calc R 1 . H H1B 0.3070 0.4791 0.9621 0.051 Uiso calc R 1 . C C1 0.1570(9) 0.3007(9) 0.8275(8) 0.0491(18) Uani d . 1 . H H1C 0.0561 0.2960 0.8692 0.059 Uiso calc R 1 . H H1D 0.1626 0.2002 0.8578 0.059 Uiso calc R 1 . 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 Mn1 0.0208(9) 0.0208(9) 0.0184(12) 0.0104(5) 0.000 0.000 S1 0.0327(13) 0.0327(13) 0.034(2) 0.0163(7) 0.000 0.000 O1 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8) O2 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8) O3 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8) O4 0.045(8) 0.042(12) 0.047(7) 0.008(10) 0.007(6) 0.000(8) N1 0.041(3) 0.051(3) 0.040(3) 0.026(3) 0.008(2) 0.000(2) C1 0.051(4) 0.053(4) 0.054(4) 0.035(3) 0.002(3) -0.006(3) 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' Mn Mn 0.3368 0.7283 '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 Mn1 N1 6_566 3_565 81.6(3) ? N1 Mn1 N1 6_566 2_665 93.5(3) ? N1 Mn1 N1 3_565 2_665 92.7(2) ? N1 Mn1 N1 6_566 5_556 92.7(2) ? N1 Mn1 N1 3_565 5_556 93.5(3) ? N1 Mn1 N1 2_665 5_556 171.8(3) ? N1 Mn1 N1 6_566 4_666 92.7(2) ? N1 Mn1 N1 3_565 4_666 171.8(3) ? N1 Mn1 N1 2_665 4_666 81.6(3) ? N1 Mn1 N1 5_556 4_666 92.7(2) ? N1 Mn1 N1 6_566 . 171.8(3) ? N1 Mn1 N1 3_565 . 92.7(2) ? N1 Mn1 N1 2_665 . 92.7(2) ? N1 Mn1 N1 5_556 . 81.6(3) y N1 Mn1 N1 4_666 . 93.5(3) ? O4 S1 O4 . 4_665 180.000(19) ? O4 S1 O3 . 5 133.7(10) ? O4 S1 O3 4_665 5 46.3(10) ? O4 S1 O3 . 2_665 46.3(10) ? O4 S1 O3 4_665 2_665 133.7(10) ? O3 S1 O3 5 2_665 156(4) ? O4 S1 O3 . . 46.3(10) ? O4 S1 O3 4_665 . 133.7(10) ? O3 S1 O3 5 . 90(2) ? O3 S1 O3 2_665 . 77.5(15) ? O4 S1 O3 . 4_665 133.7(10) ? O4 S1 O3 4_665 4_665 46.3(10) ? O3 S1 O3 5 4_665 77.5(15) ? O3 S1 O3 2_665 4_665 90(2) ? O3 S1 O3 . 4_665 121(3) ? O4 S1 O3 . 3_565 46.3(10) ? O4 S1 O3 4_665 3_565 133.7(10) ? O3 S1 O3 5 3_565 121(3) ? O3 S1 O3 2_665 3_565 77.5(15) ? O3 S1 O3 . 3_565 77.5(15) ? O3 S1 O3 4_665 3_565 156(4) ? O4 S1 O3 . 6_565 133.7(10) ? O4 S1 O3 4_665 6_565 46.3(10) ? O3 S1 O3 5 6_565 77.5(15) ? O3 S1 O3 2_665 6_565 121(3) ? O3 S1 O3 . 6_565 156(4) ? O3 S1 O3 4_665 6_565 77.5(15) ? O3 S1 O3 3_565 6_565 90(2) ? O4 S1 O2 . 2_665 55.7(10) ? O4 S1 O2 4_665 2_665 124.3(10) ? O3 S1 O2 5 2_665 97(2) ? O3 S1 O2 2_665 2_665 62.4(15) ? O3 S1 O2 . 2_665 30.1(12) ? O3 S1 O2 4_665 2_665 94(3) ? O3 S1 O2 3_565 2_665 99.3(13) ? O3 S1 O2 6_565 2_665 170.3(17) ? O4 S1 O2 . 5 124.3(10) ? O4 S1 O2 4_665 5 55.7(10) ? O3 S1 O2 5 5 62.4(15) ? O3 S1 O2 2_665 5 97(2) ? O3 S1 O2 . 5 94(3) ? O3 S1 O2 4_665 5 30.1(12) ? O3 S1 O2 3_565 5 170.3(17) ? O3 S1 O2 6_565 5 99.3(13) ? O2 S1 O2 2_665 5 71(2) ? O4 S1 O2 . 6_565 124.3(11) ? O4 S1 O2 4_665 6_565 55.7(10) ? O3 S1 O2 5 6_565 30.1(12) ? O3 S1 O2 2_665 6_565 170.3(18) ? O3 S1 O2 . 6_565 97(2) ? O3 S1 O2 4_665 6_565 99.3(13) ? O3 S1 O2 3_565 6_565 94(3) ? O3 S1 O2 6_565 6_565 62.4(15) ? O2 S1 O2 2_665 6_565 116(3) ? O2 S1 O2 5 6_565 91.3(15) ? O4 S1 O2 . 3_565 55.7(10) ? O4 S1 O2 4_665 3_565 124.3(10) ? O3 S1 O2 5 3_565 170.3(17) ? O3 S1 O2 2_665 3_565 30.1(12) ? O3 S1 O2 . 3_565 99.3(13) ? O3 S1 O2 4_665 3_565 97(2) ? O3 S1 O2 3_565 3_565 62.4(15) ? O3 S1 O2 6_565 3_565 94(3) ? O2 S1 O2 2_665 3_565 91.3(15) ? O2 S1 O2 5 3_565 116(3) ? O2 S1 O2 6_565 3_565 147(4) ? S1 O1 O1 . 6_565 54.1(11) ? S1 O2 O2 . 6_565 54.5(12) ? S1 O3 O3 . 2_665 51.2(7) ? S1 O3 O3 . 3_565 51.2(7) ? O3 O3 O3 2_665 3_565 60.0000(10) ? C1 N1 Mn1 . . 107.9(4) ? C1 N1 H1A . . 110.1 ? Mn1 N1 H1A . . 110.1 ? C1 N1 H1B . . 110.1 ? Mn1 N1 H1B . . 110.1 ? H1A N1 H1B . . 108.4 ? N1 C1 C1 . 5_556 108.9(5) ? N1 C1 H1C . . 109.9 ? C1 C1 H1C 5_556 . 109.9 ? N1 C1 H1D . . 109.9 ? C1 C1 H1D 5_556 . 109.9 ? H1C C1 H1D . . 108.3 ? 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 Mn1 N1 6_566 2.125(6) ? Mn1 N1 3_565 2.125(6) ? Mn1 N1 2_665 2.125(6) ? Mn1 N1 5_556 2.125(6) ? Mn1 N1 4_666 2.125(6) ? Mn1 N1 . 2.125(6) y S1 O4 . 1.30(9) ? S1 O4 4_665 1.30(9) ? S1 O3 5 1.45(3) ? S1 O3 2_665 1.45(3) ? S1 O3 . 1.45(3) ? S1 O3 4_665 1.45(3) ? S1 O3 3_565 1.45(3) ? S1 O3 6_565 1.45(3) ? S1 O2 2_665 1.48(3) ? S1 O2 5 1.48(3) ? S1 O2 6_565 1.48(3) ? S1 O2 3_565 1.48(3) ? O1 O1 6_565 1.74(5) ? O2 O2 6_565 1.72(6) ? O3 O3 2_665 1.82(4) ? O3 O3 3_565 1.82(4) ? N1 C1 . 1.471(9) ? N1 H1A . 0.9000 ? N1 H1B . 0.9000 ? C1 C1 5_556 1.496(15) ? C1 H1C . 0.9700 ? C1 H1D . 0.9700 ? 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 N1 H1A O1 9_656 0.90 2.28 3.16(3) 166 yes N1 H1A O1 12_656 0.90 2.43 3.15(3) 138 yes N1 H1B O1 3_566 0.90 2.17 3.06(2) 170 yes N1 H1B O2 3_566 0.90 2.11 3.00(2) 167 yes N1 H1A O2 7_666 0.90 2.14 2.95(5) 148 yes N1 H1A O3 9_656 0.90 1.92 2.80(3) 166 yes N1 H1B O3 3_566 0.90 2.15 2.96(3) 150 yes N1 H1B O3 2_666 0.90 2.36 3.18(3) 152 yes N1 H1B O4 1_556 0.90 2.15 2.94(7) 146 yes 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_4 _geom_torsion O4 S1 O1 O1 . 6_565 -129(2) O4 S1 O1 O1 4_665 6_565 51(2) O3 S1 O1 O1 5 6_565 65.8(19) O3 S1 O1 O1 2_665 6_565 -140(3) O3 S1 O1 O1 . 6_565 179(3) O3 S1 O1 O1 4_665 6_565 100(3) O3 S1 O1 O1 3_565 6_565 -77(2) O3 S1 O1 O1 6_565 6_565 0(2) O2 S1 O1 O1 2_665 6_565 171(2) O2 S1 O1 O1 5 6_565 112.2(18) O2 S1 O1 O1 6_565 6_565 34.5(19) O2 S1 O1 O1 3_565 6_565 -108(3) O4 S1 O2 O2 . 6_565 163(4) O4 S1 O2 O2 4_665 6_565 -17(4) O3 S1 O2 O2 5 6_565 20(2) O3 S1 O2 O2 2_665 6_565 179(4) O3 S1 O2 O2 . 6_565 109(4) O3 S1 O2 O2 4_665 6_565 -0E1(2) O3 S1 O2 O2 3_565 6_565 -136(5) O3 S1 O2 O2 6_565 6_565 -58(2) O2 S1 O2 O2 2_665 6_565 117(4) O2 S1 O2 O2 5 6_565 61(2) O2 S1 O2 O2 3_565 6_565 -151(4) O4 S1 O3 O3 . 2_665 39.9(5) O4 S1 O3 O3 4_665 2_665 -140.1(5) O3 S1 O3 O3 5 2_665 -159(3) O3 S1 O3 O3 4_665 2_665 -83(2) O3 S1 O3 O3 3_565 2_665 79.8(10) O3 S1 O3 O3 6_565 2_665 141.8(18) O2 S1 O3 O3 2_665 2_665 -55(3) O2 S1 O3 O3 5 2_665 -96(3) O2 S1 O3 O3 6_565 2_665 172(3) O2 S1 O3 O3 3_565 2_665 20.9(16) O4 S1 O3 O3 . 3_565 -39.9(5) O4 S1 O3 O3 4_665 3_565 140.1(5) O3 S1 O3 O3 5 3_565 122(4) O3 S1 O3 O3 2_665 3_565 -79.8(10) O3 S1 O3 O3 4_665 3_565 -163(2) O3 S1 O3 O3 6_565 3_565 62(2) O2 S1 O3 O3 2_665 3_565 -135(3) O2 S1 O3 O3 5 3_565 -176(3) O2 S1 O3 O3 6_565 3_565 92(3) O2 S1 O3 O3 3_565 3_565 -58.9(16) N1 Mn1 N1 C1 6_566 . 32.2(4) N1 Mn1 N1 C1 3_565 . 78.5(5) N1 Mn1 N1 C1 2_665 . 171.4(4) N1 Mn1 N1 C1 5_556 . -14.7(3) N1 Mn1 N1 C1 4_666 . -106.9(4) Mn1 N1 C1 C1 . 5_556 41.5(7)