#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200484.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_2200484 loop_ _publ_author_name 'Guzm\'an-Miralles, Carmen' 'Castillo, Oscar' 'Luque, Antonio' 'Beitia, Javier I.' 'Rom\'an, Pascual' _publ_section_title ; \m-Oxalato-bis[aqua(diethylenetriamine)nickel(II)] dinitrate ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m407 _journal_page_last m409 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ni2 (C2 O4) (C4 H13 N3)2 (H2 O)2] (N O3)2' _chemical_formula_moiety 'C10 H30 N6 Ni2 O6 2+, 2N O3 1-' _chemical_formula_sum 'C10 H30 N8 Ni2 O12' _chemical_formula_weight 571.80 _chemical_name_systematic ; \m-oxalato-bis[aqua(diethylenetriamine)nickel(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' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 117.96(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.560(2) _cell_length_b 7.243(2) _cell_length_c 13.387(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 13.2 _cell_measurement_theta_min 7.5 _cell_volume 1075.7(4) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_measured_fraction_theta_full 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device 'Enraf Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0190 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5512 _diffrn_reflns_theta_full 34.96 _diffrn_reflns_theta_max 34.96 _diffrn_reflns_theta_min 1.84 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_T_max .633 _exptl_absorpt_correction_T_min .494 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'via \y scan (North et al., 1968)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas 1.750(10) _exptl_crystal_density_method 'flotation in a mixture of carbon tetrachloride and bromoform' _exptl_crystal_description prism _exptl_crystal_F_000 596 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .25 _refine_diff_density_max .575 _refine_diff_density_min -.726 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 184 _refine_ls_number_reflns 4732 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all .0594 _refine_ls_R_factor_gt .0325 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.5287P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0889 _reflns_number_gt 3495 _reflns_number_total 4732 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file dn6002.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200484 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z 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 Ni1 .55907(2) .76308(2) .178205(14) .02110(5) Uani d . 1 . Ni O1 .58089(10) 1.04120(13) .14506(8) .0249(2) Uani d . 1 . O O2 .47092(10) .76468(12) -.00044(9) .0254(2) Uani d . 1 . O C1 .53176(11) 1.0802(2) .04158(10) .0200(2) Uani d . 1 . C O3W .71952(11) .6948(2) .17523(12) .0360(3) Uani d . 1 . O N1 .64163(13) .8183(2) .35098(11) .0315(3) Uani d D 1 . N C2 .5489(2) .8330(3) .38839(14) .0403(4) Uani d . 1 . C H2A .5777(2) .9115(3) .45470(14) .048 Uiso calc R 1 . H H2B .5320(2) .7118(3) .40838(14) .048 Uiso calc R 1 . H C3 .4348(2) .9145(3) .2931(2) .0417(4) Uani d . 1 . C H3A .3697(2) .9083(3) .3128(2) .05 Uiso calc R 1 . H H3B .4481(2) 1.0431(3) .2822(2) .05 Uiso calc R 1 . H N4 .40125(12) .8110(2) .18794(12) .0295(2) Uani d D 1 . N C5 .3425(2) .6328(3) .1840(2) .0434(4) Uani d D 1 . C H5A .2557(2) .6476(3) .1420(2) .052 Uiso calc PR .9 1 H H5B .3626(2) .5948(3) .2603(2) .052 Uiso calc PR .9 1 H H5C .3074(2) .6398(3) .2348(2) .052 Uiso d PR .1 2 H H5D .2769(2) .6158(3) .1081(2) .052 Uiso d PR .1 2 H C6 .3819(2) .4853(3) .1287(2) .0394(4) Uani d PD .9 1 C H6A .3556(2) .3651(3) .1406(2) .047 Uiso calc PR .9 1 H H6B .3459(2) .5074(3) .0480(2) .047 Uiso calc PR .9 1 H N7 .51403(14) .4891(2) .17864(12) .0319(3) Uani d D 1 . N C6A .4150(16) .4776(19) .2122(16) .042(4) Uani d PD .1 2 C H3C .3651(16) .3710(19) .1757(16) .051 Uiso calc PR .1 2 H H3D .4511(16) .4587(19) .2933(16) .051 Uiso calc PR .1 2 H N10 .82822(14) .8786(2) .01015(13) .0363(3) Uani d . 1 . N O11 .75272(14) .9460(2) .03687(13) .0467(3) Uani d . 1 . O O12 .8234(2) .9207(4) -.07927(15) .0796(6) Uani d . 1 . O O13 .9063(2) .7776(4) .0781(2) .0932(8) Uani d . 1 . O H31W .781(2) .679(4) .237(2) .049(7) Uiso d . 1 . H H32W .743(3) .767(4) .142(3) .063(9) Uiso d . 1 . H H71 .553(2) .440(3) .2473(16) .048(6) Uiso d D 1 . H H41 .354(2) .876(3) .1313(19) .059(7) Uiso d D 1 . H H72 .532(2) .431(4) .133(2) .054(7) Uiso d D 1 . H H11 .682(2) .920(3) .365(2) .051(7) Uiso d D 1 . H H12 .695(2) .736(3) .394(2) .052(8) Uiso d 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 Ni1 .02101(8) .02123(8) .02057(8) -.00034(6) .00934(6) .00223(6) O1 .0285(5) .0237(4) .0193(4) -.0037(4) .0085(4) .0000(3) O2 .0331(5) .0200(4) .0225(4) -.0025(3) .0126(4) .0005(3) C1 .0187(5) .0202(4) .0211(5) -.0007(4) .0093(4) -.0008(4) O3W .0257(5) .0456(6) .0374(6) .0091(5) .0152(5) .0132(5) N1 .0325(7) .0330(6) .0232(5) -.0044(5) .0082(5) .0022(5) C2 .0475(10) .0481(9) .0274(7) .0034(8) .0193(7) -.0024(6) C3 .0443(10) .0440(9) .0402(9) .0108(7) .0225(8) -.0044(7) N4 .0262(6) .0337(6) .0295(6) .0027(5) .0139(5) .0022(5) C5 .0351(9) .0506(10) .0511(11) -.0116(8) .0257(8) -.0026(8) C6 .0433(10) .0354(8) .0369(9) -.0161(8) .0167(8) -.0040(7) N7 .0410(7) .0237(5) .0317(6) .0004(5) .0177(6) .0017(4) C6A .051(11) .032(7) .045(10) -.017(7) .024(8) -.006(7) N10 .0366(7) .0385(7) .0374(7) .0036(6) .0204(6) .0003(6) O11 .0522(8) .0429(7) .0623(9) .0069(6) .0412(7) .0024(6) O12 .0843(14) .123(2) .0527(10) .0302(13) .0494(10) .0219(11) O13 .087(2) .109(2) .091(2) .0644(14) .0473(13) .0509(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 3 0 -2 2 5 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 Ni1 O2 . . 78.89(4) yes O1 Ni1 O3W . . 90.02(6) yes O1 Ni1 N1 . . 90.23(5) yes O1 Ni1 N4 . . 94.34(6) yes O1 Ni1 N7 . . 169.13(5) yes O2 Ni1 O3W . . 88.74(6) yes O2 Ni1 N1 . . 168.57(5) yes O2 Ni1 N4 . . 93.50(6) yes O2 Ni1 N7 . . 90.55(5) yes O3W Ni1 N1 . . 94.82(7) yes O3W Ni1 N4 . . 175.41(6) yes O3W Ni1 N7 . . 92.32(7) yes N1 Ni1 N4 . . 83.75(7) yes N1 Ni1 N7 . . 100.13(6) yes N4 Ni1 N7 . . 83.66(7) yes Ni1 O1 C1 . . 113.68(8) no Ni1 O2 C1 . 3_675 113.38(8) no Ni1 O3W H31W . . 117.8(18) no Ni1 O3W H32W . . 117(3) no H31W O3W H32W . . 103(3) no Ni1 N1 C2 . . 109.30(11) no C3 N4 C5 . . 113.18(16) no Ni1 N4 C5 . . 109.15(13) no Ni1 N4 C3 . . 106.98(13) no Ni1 N7 C6 . . 105.65(12) no Ni1 N7 C6A . . 108.6(5) no C2 N1 H12 . . 107.9(17) no H11 N1 H12 . . 104(2) no Ni1 N1 H11 . . 109.9(16) no Ni1 N1 H12 . . 115.3(15) no C2 N1 H11 . . 109.8(17) no C5 N4 H41 . . 108.5(16) no Ni1 N4 H41 . . 108.9(19) no C3 N4 H41 . . 110.1(15) no C6 N7 H72 . . 106.5(18) no Ni1 N7 H71 . . 111.7(14) no Ni1 N7 H72 . . 108.3(19) no C6 N7 H71 . . 114.8(17) no C6A N7 H71 . . 78.5(19) no C6A N7 H72 . . 135(2) no H71 N7 H72 . . 110(2) no O12 N10 O13 . . 122.6(2) no O11 N10 O12 . . 119.34(19) no O11 N10 O13 . . 118.04(19) no O1 C1 O2 . 3_675 126.01(12) no O1 C1 C1 . 3_675 116.50(11) no O2 C1 C1 3_675 3_675 117.48(11) no N1 C2 C3 . . 109.14(15) no N4 C3 C2 . . 109.79(17) no N4 C5 C6A . . 116.5(8) no N4 C5 C6 . . 111.32(19) no N7 C6 C5 . . 108.87(17) no N7 C6A C5 . . 113.8(11) no C3 C2 H2B . . 109.9 no H2A C2 H2B . . 108.3 no C3 C2 H2A . . 109.8 no N1 C2 H2A . . 109.9 no N1 C2 H2B . . 109.9 no N4 C3 H3A . . 109.7 no N4 C3 H3B . . 109.7 no C2 C3 H3A . . 109.7 no C2 C3 H3B . . 109.7 no H3A C3 H3B . . 108.2 no N4 C5 H5B . . 109.4 no C6 C5 H5A . . 109.4 no N4 C5 H5C . . 108.3 no N4 C5 H5D . . 108.3 no N4 C5 H5A . . 109.4 no C6A C5 H5D . . 108.1 no H5C C5 H5D . . 107.4 no C6 C5 H5B . . 109.4 no H5A C5 H5B . . 108.0 no C6A C5 H5C . . 108.0 no N7 C6 H6A . . 109.9 no N7 C6 H6B . . 109.9 no C5 C6 H6A . . 109.9 no C5 C6 H6B . . 109.9 no H6A C6 H6B . . 108.3 no N7 C6A H3D . . 109 no H3C C6A H3D . . 108 no C5 C6A H3C . . 109 no C5 C6A H3D . . 108.8 no N7 C6A H3C . . 109 no 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 Ni1 O1 . 2.1081(11) yes Ni1 O2 . 2.1125(12) yes Ni1 O3W . 2.0935(17) yes Ni1 N1 . 2.0822(14) yes Ni1 N4 . 2.0758(18) yes Ni1 N7 . 2.0641(15) yes O1 C1 . 1.2561(16) no O2 C1 3_675 1.2451(15) no O3W H32W . .83(4) no O3W H31W . .83(2) no O11 N10 . 1.258(3) no O12 N10 . 1.209(3) no O13 N10 . 1.220(3) no N1 C2 . 1.471(3) no N4 C3 . 1.472(2) no N4 C5 . 1.476(3) no N7 C6A . 1.51(2) no N7 C6 . 1.470(3) no N1 H12 . .88(2) no N1 H11 . .87(2) no N4 H41 . .85(2) no N7 H71 . .888(19) no N7 H72 . .86(3) no C1 C1 3_675 1.5463(17) no C2 C3 . 1.522(3) no C5 C6 . 1.509(3) no C5 C6A . 1.383(17) no C2 H2B . .97 no C2 H2A . .97 no C3 H3A . .97 no C3 H3B . .97 no C5 H5A . .97 no C5 H5D . .97 no C5 H5B . .97 no C5 H5C . .97 no C6 H6A . .97 no C6 H6B . .97 no C6A H3C . .97 no C6A H3D . .97 no 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 H11 O3W 2_655 .87(2) 2.53(2) 3.343(2) 157(2) yes N1 H12 O11 2_645 .88(2) 2.26(2) 3.069(2) 152(2) yes O3W H31W O1 2_645 .83(2) 1.98(3) 2.767(2) 157(3) yes O3W H32W O11 . .83(4) 1.96(3) 2.764(2) 165(4) yes O3W H32W O13 . .83(4) 2.57(4) 3.227(3) 138(3) yes N4 H41 O11 3_675 .85(2) 2.39(2) 3.231(2) 170(3) yes N4 H41 O12 3_675 .85(2) 2.49(3) 3.164(3) 137(2) yes N7 H71 O13 2_645 .888(19) 2.45(2) 3.301(3) 161(2) yes N7 H72 O2 3_665 .86(3) 2.25(3) 3.087(2) 164(3) yes