#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/48/2204837.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_2204837 loop_ _publ_author_name 'Krause Bauer, Jeanette A.' 'Edison, Sara E.' 'Baldwin, Michael J.' _publ_section_title ; Bis(ethylenediamine)nickel(II) dinitrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m82 _journal_page_last m84 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Ni (C2 H8 N2)2] (N O3)2' _chemical_formula_moiety 'C4 H16 N4 Ni 2+, 2N O3 -' _chemical_formula_sum 'C4 H16 N6 Ni O6' _chemical_formula_weight 302.94 _chemical_name_systematic ; Bis(ethylenediamine)nickel(II) dinitrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 111.9980(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.2382(2) _cell_length_b 10.0125(3) _cell_length_c 7.8277(2) _cell_measurement_reflns_used 2387 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 64.99 _cell_measurement_theta_min 4.42 _cell_volume 598.66(3) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 2003)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker SMART 6000 CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3389 _diffrn_reflns_theta_full 66.96 _diffrn_reflns_theta_max 66.96 _diffrn_reflns_theta_min 5.79 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.670 _exptl_absorpt_correction_T_max 0.9738 _exptl_absorpt_correction_T_min 0.5115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_crystal_colour 'pale purple' _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 316 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.376 _refine_diff_density_min -0.265 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 1027 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0314 _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^)+(0.0595P)^2^+0.1767P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.0915 _reflns_number_gt 926 _reflns_number_total 1027 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ac6145.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P21/c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2204837 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_type_symbol Ni 0.5000 0.0000 0.0000 0.0172(2) Uani d S 1 Ni N1 0.6621(2) 0.15537(18) 0.0206(3) 0.0328(4) Uani d . 1 N H1A 0.6860 0.1620 -0.0849 0.039 Uiso calc R 1 H H1B 0.6101 0.2336 0.0350 0.039 Uiso calc R 1 H N2 0.7099(2) -0.08746(18) 0.1871(2) 0.0298(4) Uani d . 1 N H2A 0.7012 -0.0859 0.3009 0.036 Uiso calc R 1 H H2B 0.7168 -0.1751 0.1551 0.036 Uiso calc R 1 H C3 0.8260(3) 0.1333(2) 0.1815(4) 0.0439(6) Uani d . 1 C H3A 0.8117 0.1638 0.2954 0.053 Uiso calc R 1 H H3B 0.9228 0.1846 0.1670 0.053 Uiso calc R 1 H C4 0.8675(4) -0.0141(2) 0.1942(4) 0.0383(6) Uani d . 1 C H4A 0.9010 -0.0416 0.0905 0.046 Uiso calc R 1 H H4B 0.9663 -0.0338 0.3110 0.046 Uiso calc R 1 H N3 0.3284(2) 0.05798(19) 0.3331(2) 0.0289(4) Uani d . 1 N O1 0.2690(2) 0.12956(16) 0.4279(2) 0.0390(4) Uani d . 1 O O2 0.4085(2) 0.11111(16) 0.2437(2) 0.0400(4) Uani d . 1 O O3 0.3045(2) -0.06558(16) 0.3278(2) 0.0408(4) Uani d . 1 O 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 Ni 0.0233(3) 0.0102(3) 0.0182(3) 0.00025(15) 0.0080(2) 0.00177(14) N1 0.0416(11) 0.0208(9) 0.0370(10) 0.0001(8) 0.0160(8) -0.0003(7) N2 0.0377(10) 0.0249(9) 0.0274(9) 0.0021(7) 0.0129(7) 0.0008(7) C3 0.0402(14) 0.0293(13) 0.0540(15) -0.0053(10) 0.0083(11) -0.0047(11) C4 0.0362(13) 0.0319(13) 0.0441(14) 0.0015(9) 0.0119(11) -0.0009(9) N3 0.0377(11) 0.0230(10) 0.0245(9) 0.0006(8) 0.0101(8) 0.0008(7) O1 0.0578(11) 0.0300(9) 0.0368(9) 0.0050(7) 0.0264(8) -0.0006(7) O2 0.0584(11) 0.0305(9) 0.0420(9) -0.0067(7) 0.0312(8) -0.0036(7) O3 0.0599(11) 0.0210(9) 0.0448(10) -0.0020(8) 0.0235(8) 0.0015(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 N2 Ni N2 . 3_655 180.0 ? N2 Ni N1 . . 85.08(7) y N2 Ni N1 3_655 . 94.92(7) ? N2 Ni N1 . 3_655 94.92(7) y N2 Ni N1 3_655 3_655 85.08(7) ? N1 Ni N1 . 3_655 180.0 ? C3 N1 Ni . . 108.60(14) y C3 N1 H1A . . 110.0 ? Ni N1 H1A . . 110.0 ? C3 N1 H1B . . 110.0 ? Ni N1 H1B . . 110.0 ? H1A N1 H1B . . 108.3 ? C4 N2 Ni . . 108.47(14) y C4 N2 H2A . . 110.0 ? Ni N2 H2A . . 110.0 ? C4 N2 H2B . . 110.0 ? Ni N2 H2B . . 110.0 ? H2A N2 H2B . . 108.4 ? N1 C3 C4 . . 108.30(19) y N1 C3 H3A . . 110.0 ? C4 C3 H3A . . 110.0 ? N1 C3 H3B . . 110.0 ? C4 C3 H3B . . 110.0 ? H3A C3 H3B . . 108.4 ? N2 C4 C3 . . 108.1(2) y N2 C4 H4A . . 110.1 ? C3 C4 H4A . . 110.1 ? N2 C4 H4B . . 110.1 ? C3 C4 H4B . . 110.1 ? H4A C4 H4B . . 108.4 ? O2 N3 O3 . . 120.85(17) ? O2 N3 O1 . . 119.59(18) ? O3 N3 O1 . . 119.55(16) ? 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 Ni N2 . 2.0015(18) y Ni N2 3_655 2.0015(18) ? Ni N1 . 2.0171(18) y Ni N1 3_655 2.0171(18) ? N1 C3 . 1.478(3) y N1 H1A . 0.9200 ? N1 H1B . 0.9200 ? N2 C4 . 1.474(3) y N2 H2A . 0.9200 ? N2 H2B . 0.9200 ? C3 C4 . 1.510(3) y C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? N3 O2 . 1.247(2) ? N3 O3 . 1.251(3) ? N3 O1 . 1.255(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 N1 H1A O3 3_655 0.92 2.16 2.980(3) 148 y N1 H1B O3 2_655 0.92 2.26 3.008(2) 138 y N2 H2A O1 3_656 0.92 2.09 2.983(2) 163 y N2 H2B O1 2_645 0.92 2.08 2.998(2) 178 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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag N2 Ni N1 C3 . -11.64(15) y N2 Ni N1 C3 3_655 168.36(15) ? N1 Ni N1 C3 3_655 82(7) ? N2 Ni N2 C4 3_655 -35(7) ? N1 Ni N2 C4 . -16.22(15) y N1 Ni N2 C4 3_655 163.78(15) ? Ni N1 C3 C4 . 36.6(2) y Ni N2 C4 C3 . 40.4(2) y N1 C3 C4 N2 . -51.2(3) y _cod_database_fobs_code 2204837 _journal_paper_doi 10.1107/S1600536804032052