#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003807.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003807 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1995 _journal_volume 51 _journal_page_first 1543 _journal_page_last 1545 _publ_section_title ; [N-(3-Aminopropyl)-1,3-propanediamine]diaquosulfatonickel(II) Monohydrate, [Ni(SO~4~)(dpt)(H~2~O)~2~].H~2~O [dpt = NH~2~(CH~2~)~3~NH(CH~2~)~3~NH~2~] ; _chemical_formula_sum 'C6 H23 N3 Ni O7 S' _chemical_formula_weight 340.04 _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.242(3) _cell_length_b 8.454(3) _cell_length_c 12.230(6) _cell_angle_alpha 74.53(3) _cell_angle_beta 74.15(3) _cell_angle_gamma 78.64(3) _cell_volume 688.0(5) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_meas 1.63 _exptl_crystal_density_method 'method of flotation' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_absorpt_coefficient_mu 1.591 _cell_measurement_temperature 293(2) _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_colour 'light blue' _diffrn_measurement_device 'R3m/V' _diffrn_measurement_method \w _exptl_absorpt_correction_type 'empirical, \y scan' _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.784 _diffrn_reflns_number 2135 _reflns_number_total 2047 _reflns_number_observed 1801 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_theta_max 23.54 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% <3 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0246 _refine_ls_wR_factor_obs 0.0579 _refine_ls_wR_factor_all 0.0789 _refine_ls_goodness_of_fit_obs 0.947 _refine_ls_goodness_of_fit_all 0.944 _refine_ls_number_reflns 2044 _refine_ls_number_parameters 255 _refine_ls_hydrogen_treatment 'H atoms refined isotropically' _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(Fo^2^) + (0.0316P)^2^ + 0.6850P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.411 _refine_diff_density_max 0.238 _refine_diff_density_min -0.276 _refine_ls_extinction_method none _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.0060 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.1234 'Ni' 'Ni' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3393 1.1124 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ni 1 0.19412(5) 0.06399(4) 0.28971(3) 0.02152(12) S 1 -0.25827(9) 0.26314(8) 0.30796(6) 0.0249(2) O1 1 -0.1116(3) 0.1365(2) 0.3590(2) 0.0293(4) O2 1 -0.4441(3) 0.2568(3) 0.3956(2) 0.0386(5) O3 1 -0.1964(3) 0.4264(2) 0.2800(2) 0.0420(5) O4 1 -0.2761(3) 0.2206(3) 0.2028(2) 0.0376(5) O5 1 0.4906(3) -0.0164(3) 0.2314(2) 0.0334(5) O6 1 0.2448(3) 0.0918(3) 0.4465(2) 0.0324(5) O7 1 0.4214(4) 0.3143(3) 0.6229(2) 0.0563(7) N1 1 0.1461(4) -0.1787(3) 0.3796(2) 0.0329(6) N2 1 0.1406(3) 0.0495(3) 0.1336(2) 0.0285(5) N3 1 0.2384(4) 0.3117(3) 0.2292(2) 0.0297(6) C1 1 0.1260(6) -0.3045(4) 0.3209(4) 0.0499(9) C2 1 0.0370(5) -0.2310(4) 0.2183(3) 0.0453(8) C3 1 0.1606(5) -0.1214(4) 0.1185(3) 0.0417(8) C4 1 0.2486(5) 0.1550(4) 0.0271(3) 0.0394(8) C5 1 0.2126(5) 0.3368(4) 0.0281(3) 0.0452(8) C6 1 0.3143(5) 0.3837(4) 0.1045(3) 0.0391(8) HN1A 1 0.2436(39) -0.2143(38) 0.4117(26) 0.038(9) HN1B 1 0.0429(44) -0.1636(48) 0.4325(29) 0.067(13) HN2A 1 0.0198(35) 0.0896(36) 0.1396(27) 0.036(9) HN3A 1 0.3099(42) 0.3240(39) 0.2726(25) 0.040(9) HN3B 1 0.1258(37) 0.3658(36) 0.2532(27) 0.040(9) HC1A 1 0.2505(44) -0.3629(51) 0.3005(38) 0.085(15) HC1B 1 0.0539(46) -0.3838(38) 0.3761(26) 0.054(10) HC2A 1 0.0178(46) -0.3211(43) 0.1926(28) 0.045(9) HC2B 1 -0.0892(48) -0.1680(40) 0.2464(27) 0.040(9) HC3A 1 0.1278(46) -0.1121(39) 0.0448(29) 0.044(9) HC3B 1 0.2946(49) -0.1621(39) 0.1097(26) 0.039(9) HC4A 1 0.3873(48) 0.1151(38) 0.0255(25) 0.038(8) HC4B 1 0.2148(46) 0.1341(40) -0.0414(30) 0.049(9) HC5A 1 0.0682(54) 0.3733(42) 0.0508(29) 0.055(10) HC5B 1 0.2611(45) 0.3929(39) -0.0513(30) 0.044(9) HC6A 1 0.4503(46) 0.3411(36) 0.0862(25) 0.034(8) HC6B 1 0.3083(44) 0.4988(43) 0.0905(27) 0.042(9) HO5A 1 0.5617(53) 0.0542(44) 0.2294(35) 0.070(14) HO5B 1 0.5254(57) -0.1107(38) 0.2754(32) 0.074(14) HO6A 1 0.2322(54) 0.0075(38) 0.5073(26) 0.066(12) HO6B 1 0.3485(40) 0.1291(41) 0.4359(29) 0.049(11) HO7A 1 0.3549(52) 0.4031(38) 0.6391(34) 0.063(13) HO7B 1 0.4371(62) 0.3267(52) 0.5512(24) 0.078(15) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ni 0.0200(2) -0.00403(13) -0.00124(14) 0.0202(2) -0.00480(14) 0.0226(2) S 0.0179(3) -0.0042(3) -0.0003(3) 0.0250(4) -0.0070(3) 0.0297(4) O1 0.0217(10) -0.0036(8) -0.0013(8) 0.0323(11) -0.0021(8) 0.0281(10) O2 0.0206(10) -0.0089(9) 0.0071(9) 0.0466(13) -0.0189(10) 0.0464(13) O3 0.0324(12) -0.0077(9) 0.0021(10) 0.0261(11) -0.0112(10) 0.0619(15) O4 0.0304(11) -0.0085(10) -0.0091(9) 0.0516(13) -0.0098(10) 0.0332(11) O5 0.0229(11) -0.0012(10) -0.0031(9) 0.0352(13) -0.0096(10) 0.0391(12) O6 0.0298(12) -0.0143(10) -0.0040(9) 0.0402(13) -0.0034(10) 0.0273(11) O7 0.068(2) 0.0166(13) -0.0101(14) 0.0389(14) -0.0128(12) 0.051(2) N1 0.032(2) -0.0042(12) -0.0017(13) 0.0267(13) -0.0080(11) 0.037(2) N2 0.0228(13) -0.0024(11) -0.0017(11) 0.0344(14) -0.0107(11) 0.0275(13) N3 0.0246(14) -0.0055(11) -0.0014(12) 0.0255(13) -0.0051(11) 0.0354(15) C1 0.061(3) -0.013(2) -0.015(2) 0.029(2) -0.011(2) 0.065(2) C2 0.045(2) -0.012(2) -0.011(2) 0.039(2) -0.023(2) 0.062(2) C3 0.039(2) -0.006(2) -0.005(2) 0.046(2) -0.027(2) 0.047(2) C4 0.036(2) -0.008(2) 0.0008(14) 0.053(2) -0.0080(14) 0.024(2) C5 0.043(2) -0.003(2) -0.002(2) 0.050(2) 0.008(2) 0.028(2) C6 0.037(2) -0.0111(15) 0.0034(15) 0.029(2) 0.0028(14) 0.040(2) _cod_database_code 2003807