#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2204841.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_2204841 _space_group_IT_number 12 _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _[local]_cod_cif_authors_sg_H-M 'C 2/m' loop_ _publ_author_name Ma,Zhijie 'Tao, Jun' 'Huang, Rong-Bin' 'Zhang, Lan-Sun' _publ_section_title ; Hexaaquamanganese(II) bis[5-(4-cyanophenyl)-2H-tetrazolate] ; _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1 _journal_page_last m2 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Mn (H2 O)6] (C8 H4 N5)2' _chemical_formula_moiety 'H12 Mn O6 2+, 2C8 H8 N5 -' _chemical_formula_sum 'C16 H20 Mn N10 O6' _chemical_formula_weight 503.36 _chemical_name_systematic ; Hexaaquamanganese(II) bis[5-(4-cyanophenyl)-2H-tetrazolate] ; _symmetry_cell_setting monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.5240(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.5565(9) _cell_length_b 10.2568(7) _cell_length_c 8.1885(5) _cell_measurement_reflns_used 3037 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.095 _cell_measurement_theta_min 2.503 _cell_volume 1122.89(13) _computing_cell_refinement 'SAINT (Bruker 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker SMART APEX 2000' _diffrn_measurement_method '\f and \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 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4708 _diffrn_reflns_theta_full 26.99 _diffrn_reflns_theta_max 26.99 _diffrn_reflns_theta_min 2.50 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_T_max 0.8822 _exptl_absorpt_correction_T_min 0.7831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 518 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.353 _refine_diff_density_min -0.225 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 1284 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.154 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0432 _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^)+(0.0577P)^2^+0.8233P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1102 _reflns_number_gt 1262 _reflns_number_total 1284 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file br6174.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 _atom_site_type_symbol Mn1 0.0000 0.0000 0.0000 0.0360(2) Uani d S 1 . Mn O1 -0.11681(14) -0.14023(18) -0.0510(3) 0.0693(6) Uani d . 1 . O O2 -0.0215(3) 0.0000 0.2585(4) 0.0978(14) Uani d S 1 . O C1 0.3190(2) 0.0000 0.3754(4) 0.0647(11) Uani d S 1 . C C2 0.3619(2) 0.1158(3) 0.3430(4) 0.0725(8) Uani d . 1 . C H2A 0.3314 0.1941 0.3626 0.087 Uiso calc R 1 . H C3 0.45063(18) 0.1158(3) 0.2811(3) 0.0593(6) Uani d . 1 . C H3A 0.4800 0.1946 0.2595 0.071 Uiso calc R 1 . H C4 0.4960(2) 0.0000 0.2511(3) 0.0408(6) Uani d S 1 . C C5 0.59140(19) 0.0000 0.1892(3) 0.0374(6) Uani d S 1 . C C6 0.2286(3) 0.0000 0.4451(5) 0.0854(16) Uani d S 1 . C N1 0.153(3) 0.031(13) 0.483(3) 0.071(15) Uani d P 0.25 1 N N1' 0.165(3) 0.026(9) 0.522(3) 0.063(13) Uani d P 0.25 2 N N2 0.64006(13) -0.10642(17) 0.1578(2) 0.0482(4) Uani d . 1 . N N3 0.72188(13) -0.06365(18) 0.1035(2) 0.0497(5) Uani d . 1 . N H1W1 -0.119(2) -0.204(3) -0.090(3) 0.054(8) Uiso d . 1 . H H1W2 -0.158(2) -0.135(3) -0.011(4) 0.072(10) Uiso d . 1 . H H2W1 -0.066(5) 0.0000 0.292(7) 0.099(19) Uiso d S 1 . H H2W2 0.021(5) 0.0000 0.311(9) 0.12(3) Uiso d S 1 . H 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 0.0272(3) 0.0328(3) 0.0515(4) 0.000 0.0165(2) 0.000 O1 0.0451(10) 0.0445(9) 0.1301(18) -0.0135(7) 0.0488(11) -0.0299(10) O2 0.0417(16) 0.199(5) 0.0578(17) 0.000 0.0243(14) 0.000 C1 0.0304(15) 0.122(3) 0.0442(16) 0.000 0.0148(12) 0.000 C2 0.0482(13) 0.098(2) 0.0783(17) 0.0219(14) 0.0306(12) -0.0001(15) C3 0.0470(12) 0.0621(15) 0.0756(16) 0.0086(11) 0.0298(11) 0.0020(12) C4 0.0309(13) 0.0550(16) 0.0389(13) 0.000 0.0127(10) 0.000 C5 0.0322(12) 0.0418(14) 0.0409(13) 0.000 0.0142(10) 0.000 C6 0.0370(18) 0.172(5) 0.0503(19) 0.000 0.0167(15) 0.000 N1 0.035(8) 0.14(4) 0.038(11) 0.002(13) 0.012(8) 0.006(19) N1' 0.042(9) 0.11(4) 0.038(11) 0.005(12) 0.010(8) -0.003(19) N2 0.0415(9) 0.0402(9) 0.0696(11) -0.0040(7) 0.0288(8) -0.0073(8) N3 0.0413(9) 0.0460(9) 0.0685(11) -0.0013(8) 0.0285(8) -0.0050(8) 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 O1 5 2.1288(17) ? Mn1 O1 . 2.1288(17) y Mn1 O1 6 2.1288(17) ? Mn1 O1 2 2.1288(17) ? Mn1 O2 . 2.184(3) y Mn1 O2 5 2.184(3) ? O1 H1W1 . 0.72(3) ? O1 H1W2 . 0.70(3) ? O2 H2W1 . 0.71(6) ? O2 H2W2 . 0.66(7) ? C1 C2 . 1.367(4) y C1 C2 6 1.367(4) ? C1 C6 . 1.435(4) y C2 C3 . 1.381(3) y C2 H2A . 0.9300 ? C3 C4 . 1.379(3) y C3 H3A . 0.9300 ? C4 C3 6 1.379(3) ? C4 C5 . 1.464(3) y C5 N2 6 1.322(2) ? C5 N2 . 1.322(2) y C6 N1 6 1.17(5) ? C6 N1 . 1.17(5) y C6 N1' 6 1.18(5) ? C6 N1' . 1.18(5) y N1 N1 6 0.6(3) ? N1' N1' 6 0.54(18) ? N2 N3 . 1.336(2) y N3 N3 6 1.306(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 O1 Mn1 O1 5 . 180.00(9) y O1 Mn1 O1 5 6 94.99(11) ? O1 Mn1 O1 . 6 85.01(11) ? O1 Mn1 O1 5 2 85.01(11) ? O1 Mn1 O1 . 2 94.99(11) ? O1 Mn1 O1 6 2 180.00(9) ? O1 Mn1 O2 5 . 91.38(10) ? O1 Mn1 O2 . . 88.62(10) y O1 Mn1 O2 6 . 88.62(10) ? O1 Mn1 O2 2 . 91.38(10) ? O1 Mn1 O2 5 5 88.62(10) ? O1 Mn1 O2 . 5 91.38(10) ? O1 Mn1 O2 6 5 91.38(10) ? O1 Mn1 O2 2 5 88.62(10) ? O2 Mn1 O2 . 5 180.00(18) ? Mn1 O1 H1W1 . . 132(2) ? Mn1 O1 H1W2 . . 119(3) ? H1W1 O1 H1W2 . . 107(3) ? Mn1 O2 H2W1 . . 130(5) ? Mn1 O2 H2W2 . . 114(6) ? H2W1 O2 H2W2 . . 117(7) ? C2 C1 C2 . 6 120.6(3) ? C2 C1 C6 . . 119.69(15) y C2 C1 C6 6 . 119.69(15) ? C1 C2 C3 . . 119.7(3) y C1 C2 H2A . . 120.1 ? C3 C2 H2A . . 120.1 ? C4 C3 C2 . . 120.5(3) y C4 C3 H3A . . 119.8 ? C2 C3 H3A . . 119.8 ? C3 C4 C3 6 . 119.0(3) ? C3 C4 C5 6 . 120.49(14) ? C3 C4 C5 . . 120.49(14) y N2 C5 N2 6 . 111.3(2) ? N2 C5 C4 6 . 124.37(11) ? N2 C5 C4 . . 124.37(11) y N1 C6 N1 6 . 32(10) ? N1 C6 N1' 6 6 17(3) ? N1 C6 N1' . 6 34(2) ? N1 C6 N1' 6 . 34(2) ? N1 C6 N1' . . 17(3) ? N1' C6 N1' 6 . 26(9) ? N1 C6 C1 6 . 163(6) ? N1 C6 C1 . . 163(6) y N1' C6 C1 6 . 164(4) ? N1' C6 C1 . . 164(4) ? N1 N1 C6 6 . 74(6) ? N1' N1' C6 6 . 77(4) ? C5 N2 N3 . . 105.20(17) y N3 N3 N2 6 . 109.18(11) y 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 O2 H2W2 N1 . 0.66(7) 2.11(8) 2.76(4) 171(4) O1 H1W1 N2 7_545 0.72(3) 2.03(3) 2.743(3) 168(3) O1 H1W2 N3 1_455 0.70(3) 2.14(3) 2.813(2) 164(4) _cod_database_code 2204841