#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202465.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_2202465 loop_ _publ_author_name K.Rajagopal R.V.Krishnakumar 'M.Subha Nandhini' K.Ravikumar S.Natarajan _publ_section_title ; Bis(DL-alanine)tetraaquacobalt(II) dinitrate ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m562 _journal_page_last m564 _journal_paper_doi 10.1107/S1600536803014533 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Co (C3 H7 N O2)2 (H2 O)4] (N O3)2' _chemical_formula_moiety 'C6 H22 Co N2 O8, 2N O3' _chemical_formula_sum 'C6 H22 Co N4 O14' _chemical_formula_weight 433.21 _chemical_name_systematic ; Bis(DL-alanine)tetraaquacobalt(II) dinitrate ; _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 _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 96.220(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.5021(6) _cell_length_b 6.6396(8) _cell_length_c 23.821(3) _cell_measurement_reflns_used 3463 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 27.97 _cell_measurement_theta_min 3.2 _cell_volume 865.10(18) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _diffrn_measurement_device 'Bruker SMART APEX' _diffrn_measurement_device_type 'CCD Area Detector' _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 0.0141 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 5063 _diffrn_reflns_theta_full 27.97 _diffrn_reflns_theta_max 27.97 _diffrn_reflns_theta_min 1.72 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_T_max 0.8735 _exptl_absorpt_correction_T_min 0.7910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1998)' _exptl_crystal_colour 'pale pink' _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_meas 1.670(10) _exptl_crystal_density_method 'flotation in a mixture of bromoform and carbon tetrachloride' _exptl_crystal_description plate _exptl_crystal_F_000 450 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.698 _refine_diff_density_min -0.341 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1968 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.245 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0482 _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^)+(0.0632P)^2^+1.2873P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1396 _refine_ls_wR_factor_ref 0.1414 _reflns_number_gt 1854 _reflns_number_total 1968 _reflns_threshold_expression I>2s\(I) _cod_data_source_file ci6232.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2202465 _cod_database_fobs_code 2202465 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 Co 0.0000 0.5000 0.0000 0.0236(2) Uani d S 1 . . Co O1W -0.2038(4) 0.3305(3) 0.05495(9) 0.0297(5) Uani d . 1 . . O O2W 0.2893(4) 0.3007(4) 0.01459(10) 0.0361(5) Uani d . 1 . . O O1 -0.1034(5) 0.9394(4) 0.06679(11) 0.0420(6) Uani d . 1 . . O O2 0.1414(4) 0.6714(3) 0.06990(9) 0.0330(5) Uani d . 1 . . O O3 0.4812(6) 0.8863(6) 0.28596(14) 0.0613(9) Uani d . 1 . . O O4 0.7665(6) 1.0195(5) 0.34189(12) 0.0547(8) Uani d . 1 . . O O5 0.8453(6) 0.9037(6) 0.26089(12) 0.0575(8) Uani d . 1 . . O N1 0.2997(6) 0.7256(5) 0.17821(12) 0.0371(6) Uani d . 1 . . N H1A 0.1885 0.6300 0.1813 0.056 Uiso calc R 1 . . H H1B 0.3623 0.7646 0.2125 0.056 Uiso calc R 1 . . H H1C 0.4184 0.6774 0.1594 0.056 Uiso calc R 1 . . H N2 0.7017(6) 0.9349(5) 0.29550(12) 0.0379(7) Uani d . 1 . . N C1 0.0640(6) 0.8306(5) 0.08930(13) 0.0294(6) Uani d . 1 . . C C2 0.1832(7) 0.8993(5) 0.14737(14) 0.0350(7) Uani d . 1 . . C H2 0.0556 0.9527 0.1689 0.042 Uiso calc R 1 . . H C3 0.3685(9) 1.0602(7) 0.14224(19) 0.0559(11) Uani d . 1 . . C H3A 0.4389 1.0999 0.1792 0.084 Uiso calc R 1 . . H H3B 0.2914 1.1743 0.1231 0.084 Uiso calc R 1 . . H H3C 0.4947 1.0099 0.1211 0.084 Uiso calc R 1 . . H H1W1 -0.2206 0.3872 0.0867 0.050 Uiso d . 1 . . H H2W1 -0.1636 0.2135 0.0627 0.050 Uiso d . 1 . . H H1W2 0.4405 0.3262 0.0226 0.050 Uiso d . 1 . . H H2W2 0.2657 0.1935 -0.0045 0.050 Uiso d . 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 Co 0.0235(3) 0.0240(3) 0.0227(3) 0.0024(2) -0.0009(2) -0.0034(2) O1W 0.0322(11) 0.0282(11) 0.0289(11) 0.0000(9) 0.0034(9) -0.0007(9) O2W 0.0318(12) 0.0336(12) 0.0407(13) 0.0078(10) -0.0067(10) -0.0052(10) O1 0.0492(15) 0.0293(12) 0.0436(14) 0.0090(11) -0.0132(11) -0.0075(11) O2 0.0342(12) 0.0317(12) 0.0311(11) 0.0051(9) -0.0051(9) -0.0085(9) O3 0.0442(16) 0.083(2) 0.0551(18) -0.0065(16) -0.0019(13) -0.0254(17) O4 0.0652(19) 0.067(2) 0.0306(13) -0.0274(16) 0.0020(13) -0.0052(12) O5 0.0605(18) 0.070(2) 0.0445(16) 0.0075(16) 0.0181(14) -0.0032(15) N1 0.0410(15) 0.0388(16) 0.0295(14) -0.0008(13) -0.0049(11) -0.0030(12) N2 0.0449(17) 0.0406(15) 0.0276(14) -0.0010(14) 0.0007(12) 0.0021(12) C1 0.0338(16) 0.0274(15) 0.0261(14) -0.0032(12) -0.0007(12) -0.0027(12) C2 0.0429(18) 0.0309(17) 0.0297(16) 0.0021(14) -0.0028(13) -0.0066(13) C3 0.066(3) 0.051(2) 0.048(2) -0.021(2) -0.007(2) -0.001(2) 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' Co Co 0.3494 0.9721 '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 O2W Co O2W 3_565 . 180 y O2W Co O2 3_565 3_565 90.07(9) y O2W Co O2 . 3_565 89.93(9) y O2W Co O2 3_565 . 89.93(9) y O2W Co O2 . . 90.07(9) y O2 Co O2 3_565 . 180 y O2W Co O1W 3_565 3_565 90.31(9) ? O2W Co O1W . 3_565 89.69(9) y O2 Co O1W 3_565 3_565 88.48(9) ? O2 Co O1W . 3_565 91.52(9) y O2W Co O1W 3_565 . 89.69(9) ? O2W Co O1W . . 90.31(9) y O2 Co O1W 3_565 . 91.52(9) ? O2 Co O1W . . 88.48(9) y O1W Co O1W 3_565 . 180 y Co O1W H1W1 . . 115.01 ? Co O1W H2W1 . . 119.27 ? H1W1 O1W H2W1 . . 105.55 ? Co O2W H1W2 . . 128.78 ? Co O2W H2W2 . . 112.13 ? H1W2 O2W H2W2 . . 112.16 ? C1 O2 Co . . 130.0(2) ? C2 N1 H1A . . 109.5 ? C2 N1 H1B . . 109.5 ? H1A N1 H1B . . 109.5 ? C2 N1 H1C . . 109.5 ? H1A N1 H1C . . 109.5 ? H1B N1 H1C . . 109.5 ? O5 N2 O3 . . 121.3(3) ? O5 N2 O4 . . 121.8(3) ? O3 N2 O4 . . 116.9(3) ? O1 C1 O2 . . 126.8(3) ? O1 C1 C2 . . 116.1(3) ? O2 C1 C2 . . 117.1(3) ? N1 C2 C3 . . 109.7(3) ? N1 C2 C1 . . 109.7(3) ? C3 C2 C1 . . 111.6(3) ? N1 C2 H2 . . 108.6 ? C3 C2 H2 . . 108.6 ? C1 C2 H2 . . 108.6 ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? 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 Co O2W 3_565 2.070(2) ? Co O2W . 2.070(2) y Co O2 3_565 2.096(2) ? Co O2 . 2.096(2) y Co O1W 3_565 2.134(2) ? Co O1W . 2.134(2) y O1W H1W1 . 0.86 ? O1W H2W1 . 0.82 ? O2W H1W2 . 0.85 ? O2W H2W2 . 0.85 ? O1 C1 . 1.245(4) y O2 C1 . 1.247(4) y O3 N2 . 1.252(4) y O4 N2 . 1.256(4) y O5 N2 . 1.220(4) y N1 C2 . 1.476(4) y N1 H1A . 0.89 ? N1 H1B . 0.89 ? N1 H1C . 0.89 ? C1 C2 . 1.535(4) y C2 C3 . 1.491(6) y C2 H2 . 0.98 ? C3 H3A . 0.96 ? C3 H3B . 0.96 ? C3 H3C . 0.96 ? 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_545 0.89 2.06 2.912(5) 159 N1 H1B O3 . 0.89 1.97 2.858(4) 172 N1 H1C O4 2_645 0.89 2.03 2.836(4) 150 O1W H1W1 O4 2_545 0.86 1.96 2.813(4) 179 O1W H2W1 O1 1_545 0.82 1.85 2.664(3) 169 O2W H2W2 O1 3_565 0.85 1.87 2.630(3) 149 O2W H1W2 O1W 1_655 0.85 2.02 2.857(3) 166 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 _geom_torsion_publ_flag O2W Co O2 C1 3_565 -1.3(3) ? O2W Co O2 C1 . 178.7(3) ? O1W Co O2 C1 3_565 89.0(3) ? O1W Co O2 C1 . -91.0(3) ? Co O2 C1 O1 . -9.6(5) ? Co O2 C1 C2 . 169.3(2) ? O1 C1 C2 N1 . 157.4(3) y O2 C1 C2 N1 . -21.7(4) y O1 C1 C2 C3 . -80.9(4) y O2 C1 C2 C3 . 100.1(4) y