#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/31/2013134.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_2013134 loop_ _publ_author_name 'Schlueter, John A.' 'Geiser, Urs' 'Manson, Jamie L.' _publ_section_title ; Tetraaquabis(carbamoyldicyanomethanido-\kN)manganese(II) dihydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m1 _journal_page_last m3 _journal_paper_doi 10.1107/S0108270102020334 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Mn (C4 H2 N3 O)2 (H2 O)4], 2H2 O' _chemical_formula_moiety 'C8 H12 Mn N6 O6 , 2(H2 O)' _chemical_formula_sum 'C8 H16 Mn N6 O8' _chemical_formula_weight 379.21 _chemical_melting_point 498 _chemical_name_systematic ; Tetraaquabis(carbamoyldicyanomethanido-\kN)manganese(II) dihydrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 108.777(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.5234(4) _cell_length_b 7.4343(4) _cell_length_c 12.1939(6) _cell_measurement_reflns_used 834 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.13 _cell_measurement_theta_min 3.28 _cell_volume 817.38(7) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method 'area detector \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 0.018 _diffrn_reflns_av_sigmaI/netI 0.018 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5354 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 2.38 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 781 _diffrn_standards_number 133 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_T_max 0.807 _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(SHELXTL; Sheldrick, 2001)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 390 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.30 _refine_diff_density_min -0.17 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 131 _refine_ls_number_reflns 1927 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.023 _refine_ls_R_factor_gt 0.021 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.1424P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.058 _refine_ls_wR_factor_ref 0.059 _reflns_number_gt 1789 _reflns_number_total 1927 _reflns_threshold_expression I>2\s(I) _cod_data_source_file fg1671.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2013134 _cod_database_fobs_code 2013134 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_assembly _atom_site_disorder_group _atom_site_type_symbol Mn1 0.5000 0.0000 0.0000 0.02597(8) Uani d S 1 . . Mn O1 -0.07867(8) 0.26994(11) 0.18492(7) 0.03217(17) Uani d . 1 . . O O2 0.65084(10) 0.10667(13) 0.15895(8) 0.0408(2) Uani d D 1 . . O H21 0.7366(17) 0.146(2) 0.1678(13) 0.049 Uiso d D 1 . . H H22 0.6214(18) 0.163(2) 0.2047(14) 0.049 Uiso d D 1 . . H O3 0.52764(10) -0.26743(11) 0.08261(7) 0.03333(17) Uani d D 1 . . O H31 0.5429(16) -0.260(2) 0.1501(12) 0.040 Uiso d D 1 . . H H32 0.588(3) -0.337(4) 0.069(2) 0.040 Uiso d PD 0.50 . . H H33 0.453(3) -0.338(4) 0.056(2) 0.040 Uiso d PD 0.50 . . H N1 0.31415(12) 0.04414(15) 0.06808(10) 0.0392(2) Uani d . 1 . . N N2 -0.02456(15) -0.20122(16) 0.19245(12) 0.0550(3) Uani d . 1 . . N N3 0.09450(11) 0.40125(13) 0.12320(9) 0.0392(2) Uani d . 1 . . N H3A 0.0583 0.5055 0.1289 0.047 Uiso calc R 1 . . H H3B 0.1703 0.3920 0.0998 0.047 Uiso calc R 1 . . H C1 0.21594(12) 0.05957(15) 0.10211(9) 0.0294(2) Uani d . 1 . . C C2 0.02883(13) -0.07441(16) 0.17037(10) 0.0346(2) Uani d . 1 . . C C3 0.09456(11) 0.08143(14) 0.14216(9) 0.0285(2) Uani d . 1 . . C C4 0.03310(11) 0.25416(14) 0.15057(8) 0.0260(2) Uani d . 1 . . C O4 0.71227(11) -0.50752(12) 0.01857(9) 0.0401(2) Uani d D 1 . . O H41 0.7683(18) -0.561(2) 0.0698(13) 0.048 Uiso d D 1 . . H H42 0.648(3) -0.580(4) -0.008(3) 0.048 Uiso d PD 0.50 . . H H43 0.673(4) -0.428(4) 0.042(3) 0.048 Uiso d PD 0.50 . . 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 0.02304(13) 0.02747(13) 0.03187(13) 0.00011(8) 0.01506(9) -0.00169(8) O1 0.0262(4) 0.0377(4) 0.0381(4) 0.0030(3) 0.0180(3) -0.0016(3) O2 0.0315(4) 0.0558(6) 0.0401(4) -0.0114(4) 0.0183(3) -0.0142(4) O3 0.0370(4) 0.0323(4) 0.0330(4) 0.0018(3) 0.0145(3) 0.0001(3) N1 0.0338(5) 0.0417(5) 0.0510(6) 0.0047(4) 0.0260(5) 0.0006(5) N2 0.0552(7) 0.0427(6) 0.0762(8) 0.0006(5) 0.0336(6) 0.0172(6) N3 0.0370(5) 0.0306(5) 0.0582(6) 0.0003(4) 0.0267(5) 0.0023(4) C1 0.0276(5) 0.0300(5) 0.0332(5) 0.0026(4) 0.0134(4) 0.0006(4) C2 0.0318(5) 0.0346(6) 0.0424(6) 0.0061(4) 0.0188(5) 0.0064(5) C3 0.0255(5) 0.0313(5) 0.0337(5) 0.0016(4) 0.0165(4) 0.0027(4) C4 0.0218(4) 0.0330(5) 0.0245(4) 0.0006(4) 0.0091(4) -0.0006(4) O4 0.0333(5) 0.0351(5) 0.0533(6) 0.0028(3) 0.0159(4) 0.0037(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' 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_ _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 O2 Mn1 O2 . 3_655 180 ? O2 Mn1 O3 . . 88.51(4) y O2 Mn1 O3 3_655 . 91.49(4) ? O2 Mn1 O3 . 3_655 91.49(4) ? O3 Mn1 O3 . 3_655 180 ? O2 Mn1 N1 . . 89.43(4) ? O2 Mn1 N1 3_655 . 90.57(4) ? O3 Mn1 N1 . . 87.39(4) y O3 Mn1 N1 3_655 . 92.61(4) ? O2 Mn1 N1 . 3_655 90.57(4) ? O3 Mn1 N1 . 3_655 92.61(4) ? N1 Mn1 N1 . 3_655 180 ? Mn1 O2 H21 . . 125.5(10) ? Mn1 O2 H22 . . 121.7(12) ? H21 O2 H22 . . 105.6(15) ? Mn1 O3 H31 . . 111.4(11) ? Mn1 O3 H32 . . 117.6(19) ? H31 O3 H32 . . 110(2) ? Mn1 O3 H33 . . 114.9(19) ? H31 O3 H33 . . 107(2) ? H32 O3 H33 . . 95(3) ? C1 N1 Mn1 . . 177.06(11) y C4 N3 H3A . . 120.0 ? C4 N3 H3B . . 120.0 ? H3A N3 H3B . . 120.0 ? N1 C1 C3 . . 178.81(13) y N2 C2 C3 . . 179.50(14) y C1 C3 C2 . . 118.04(10) y C1 C3 C4 . . 122.15(9) y C2 C3 C4 . . 119.76(9) y O1 C4 N3 . . 119.30(10) y O1 C4 C3 . . 120.90(9) y N3 C4 C3 . . 119.79(9) y H41 O4 H42 . . 102(3) ? H41 O4 H43 . . 112(3) ? H42 O4 H43 . . 105(4) ? 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 . 2.1580(9) y Mn1 O3 . 2.2059(8) y Mn1 N1 . 2.2081(9) y Mn1 Mn1 2_655 7.4144(3) ? O1 C4 . 1.2686(12) y O2 H21 . 0.841(15) ? O2 H22 . 0.815(15) ? O3 H31 . 0.790(14) ? O3 H32 . 0.83(2) ? O3 H33 . 0.86(2) ? N1 C1 . 1.1445(14) y N2 C2 . 1.1436(17) y N3 C4 . 1.3322(14) y N3 H3A . 0.86 ? N3 H3B . 0.86 ? C1 C3 . 1.4016(14) y C2 C3 . 1.4111(16) y C3 C4 . 1.4285(14) y O4 H41 . 0.788(15) ? O4 H42 . 0.80(3) ? O4 H43 . 0.80(2) ? 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 N3 H3A N2 1_565 0.86 2.52 3.3688(16) 168 y N3 H3B O4 3_655 0.86 2.26 3.0078(14) 145 y O2 H21 O1 1_655 0.841(15) 1.937(15) 2.7721(12) 171.8(15) y O2 H22 N2 2 0.815(15) 2.048(16) 2.8587(14) 173.8(16) y O3 H31 O1 2_545 0.790(14) 1.942(14) 2.7317(12) 177.6(16) y O3 H32 O4 . 0.83(2) 1.96(2) 2.7877(12) 173(3) y O3 H33 O4 3_645 0.86(2) 1.93(2) 2.7797(13) 174(3) y O4 H41 O1 1_645 0.788(15) 2.086(16) 2.8664(13) 170.9(16) y O4 H42 O3 3_645 0.80(3) 1.99(3) 2.7797(13) 173(3) y O4 H43 O3 . 0.80(2) 2.01(3) 2.7877(12) 165(3) y 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 C1 C3 C4 O1 178.58(10) C2 C3 C4 O1 1.15(15) C1 C3 C4 N3 -2.11(16) C2 C3 C4 N3 -179.55(11)