#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2214415.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_2214415 loop_ _publ_author_name 'Srinivasan, Krishnan' 'Govindarajan, Subbaiah' 'Harrison, William T. A.' _publ_section_title ; Mn(N~2~H~5~)~2~(SO~4~)~2~ from synchrotron data ; _journal_coeditor_code WM2112 _journal_issue 7 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i152 _journal_page_last i152 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'Mn (N2 H5)2 (S O4)2' _chemical_formula_moiety 'H10 Mn N4 O8 S2' _chemical_formula_structural 'Mn (N2 H5)2 (S O4)2' _chemical_formula_sum 'H10 Mn N4 O8 S2' _chemical_formula_weight 313.18 _chemical_name_systematic ; catena-poly[[dihydraziniummanganese(II)]-di-\m-sulfato-\k^4^O:O'] ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 92.651(2) _cell_angle_beta 104.332(2) _cell_angle_gamma 99.249(2) _cell_formula_units_Z 1 _cell_length_a 5.3910(10) _cell_length_b 5.8678(11) _cell_length_c 7.3954(14) _cell_measurement_temperature 120(2) _cell_volume 222.81(7) _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.634 _diffrn_measured_fraction_theta_max 0.634 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'beam line 9.8 at Daresbury synchrotron' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.69050 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1414 _diffrn_reflns_theta_full 29.73 _diffrn_reflns_theta_max 29.73 _diffrn_reflns_theta_min 3.85 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 159 _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.001 _refine_diff_density_max 0.730 _refine_diff_density_min -1.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 71 _refine_ls_number_reflns 881 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.230 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0819 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2471 _refine_ls_wR_factor_ref 0.2483 _reflns_number_gt 852 _reflns_number_total 881 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm2112.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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_ _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 Mn Mn1 0.0000 0.0000 0.0000 0.0057(5) Uani d S 1 S S1 0.63753(11) 0.24939(10) 0.22017(8) 0.0049(5) Uani d . 1 O O1 0.3752(4) 0.2300(3) 0.0925(3) 0.0112(6) Uani d . 1 O O2 0.8345(4) 0.2732(3) 0.1091(3) 0.0082(6) Uani d . 1 O O3 0.6580(4) 0.0439(3) 0.3271(3) 0.0098(6) Uani d . 1 O O4 0.6915(4) 0.4609(3) 0.3504(3) 0.0081(6) Uani d . 1 N N1 0.0682(4) -0.1820(4) 0.2659(3) 0.0073(6) Uani d . 1 H H1A 0.1181 -0.0716 0.3665 0.009 Uiso calc R 1 H H1B -0.0870 -0.2701 0.2709 0.009 Uiso calc R 1 N N2 0.2616(5) -0.3304(4) 0.2857(3) 0.0089(6) Uani d . 1 H H2A 0.2730 -0.3998 0.3943 0.011 Uiso calc R 1 H H2B 0.4187 -0.2440 0.2883 0.011 Uiso calc R 1 H H2C 0.2146 -0.4408 0.1871 0.011 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 0.0062(6) 0.0061(6) 0.0046(6) 0.0002(4) 0.0013(4) 0.0010(3) S1 0.0056(6) 0.0052(6) 0.0039(7) -0.0009(4) 0.0023(4) 0.0001(4) O1 0.0065(10) 0.0126(10) 0.0115(12) -0.0026(7) -0.0006(8) 0.0011(8) O2 0.0095(9) 0.0097(10) 0.0075(10) -0.0005(7) 0.0075(7) 0.0011(7) O3 0.0131(10) 0.0075(10) 0.0090(11) 0.0002(7) 0.0035(8) 0.0037(7) O4 0.0115(9) 0.0070(10) 0.0055(10) 0.0000(7) 0.0029(7) -0.0005(7) N1 0.0071(10) 0.0084(11) 0.0081(11) 0.0022(8) 0.0042(8) 0.0018(8) N2 0.0111(11) 0.0087(11) 0.0070(12) 0.0018(8) 0.0026(8) 0.0014(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 Mn1 O2 2_655 2.1712(19) y Mn1 O2 1_455 2.1712(19) ? Mn1 O1 2 2.1752(18) ? Mn1 O1 . 2.1752(18) y Mn1 N1 . 2.259(2) y Mn1 N1 2 2.259(2) ? S1 O3 . 1.4765(19) ? S1 O1 . 1.4772(19) ? S1 O4 . 1.4787(19) ? S1 O2 . 1.489(2) ? O2 Mn1 1_655 2.1712(19) ? N1 N2 . 1.447(3) ? N1 H1A . 0.9200 ? N1 H1B . 0.9200 ? N2 H2A . 0.9100 ? N2 H2B . 0.9100 ? N2 H2C . 0.9100 ? 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 O2 Mn1 O2 2_655 1_455 180.0 O2 Mn1 O1 2_655 2 87.22(7) O2 Mn1 O1 1_455 2 92.78(7) O2 Mn1 O1 2_655 . 92.78(7) O2 Mn1 O1 1_455 . 87.22(7) O1 Mn1 O1 2 . 180.0 O2 Mn1 N1 2_655 . 84.77(8) O2 Mn1 N1 1_455 . 95.23(8) O1 Mn1 N1 2 . 87.42(8) O1 Mn1 N1 . . 92.58(8) O2 Mn1 N1 2_655 2 95.23(8) O2 Mn1 N1 1_455 2 84.77(8) O1 Mn1 N1 2 2 92.58(8) O1 Mn1 N1 . 2 87.42(8) N1 Mn1 N1 . 2 180.0 O3 S1 O1 . . 111.04(11) O3 S1 O4 . . 109.90(11) O1 S1 O4 . . 108.98(13) O3 S1 O2 . . 109.51(11) O1 S1 O2 . . 109.35(12) O4 S1 O2 . . 107.99(11) S1 O1 Mn1 . . 142.28(13) S1 O2 Mn1 . 1_655 127.72(11) N2 N1 Mn1 . . 115.31(15) N2 N1 H1A . . 108.4 Mn1 N1 H1A . . 108.4 N2 N1 H1B . . 108.4 Mn1 N1 H1B . . 108.4 H1A N1 H1B . . 107.5 N1 N2 H2A . . 109.5 N1 N2 H2B . . 109.5 H2A N2 H2B . . 109.5 N1 N2 H2C . . 109.5 H2A N2 H2C . . 109.5 H2B N2 H2C . . 109.5 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 O3 S1 O1 Mn1 . . -1.2(3) O4 S1 O1 Mn1 . . -122.4(2) O2 S1 O1 Mn1 . . 119.8(2) O2 Mn1 O1 S1 2_655 . -61.4(2) O2 Mn1 O1 S1 1_455 . 118.6(2) N1 Mn1 O1 S1 . . 23.5(2) N1 Mn1 O1 S1 2 . -156.5(2) O3 S1 O2 Mn1 . 1_655 27.96(18) O1 S1 O2 Mn1 . 1_655 -93.92(16) O4 S1 O2 Mn1 . 1_655 147.62(14) O2 Mn1 N1 N2 2_655 . 21.43(16) O2 Mn1 N1 N2 1_455 . -158.57(16) O1 Mn1 N1 N2 2 . 108.87(17) O1 Mn1 N1 N2 . . -71.13(17) 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 H1A O3 2_656 0.92 2.27 3.014(3) 137 N1 H1B O4 1_445 0.92 2.02 2.879(3) 154 N2 H2A O4 2_656 0.91 1.91 2.794(3) 165 N2 H2B O3 . 0.91 1.92 2.755(3) 152 N2 H2C O2 2_655 0.91 2.41 2.882(3) 112 N2 H2C O2 1_445 0.91 2.36 2.988(3) 126 N2 H2C O1 1_545 0.91 2.38 3.110(3) 137 _cod_database_code 2214415