#------------------------------------------------------------------------------
#$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/38/2003807.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_2003807
loop_
_publ_author_name
'Mukherjee, M.'
'Mukherjee, A. K.'
'Pariya, C.'
'Ray Chaudhuri, N.'
_publ_section_title
;
 [<i>N</i>-(3-Aminopropyl)-1,3-propanediamine]diaquasulfatonickel(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~]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1543
_journal_page_last               1545
_journal_paper_doi               10.1107/S0108270195000813
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C6 H23 N3 Ni O7 S'
_chemical_formula_weight         340.04
_chemical_name_systematic
;
Mono-[N-(3-aminopropyl)-1,3-propanediamine] diaquasulfatonickel(II)
monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                74.53(3)
_cell_angle_beta                 74.15(3)
_cell_angle_gamma                78.64(3)
_cell_formula_units_Z            2
_cell_length_a                   7.242(3)
_cell_length_b                   8.454(3)
_cell_length_c                   12.230(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     688.0(5)
_computing_cell_refinement       SHELXTL
_computing_data_collection       'SHELXTL (Sheldrick, 1985)'
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       R3m/V
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2135
_diffrn_reflns_theta_max         23.54
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   'empirical, \y scan'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      1.63
_exptl_crystal_density_method    'method of flotation'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.276
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.944
_refine_ls_goodness_of_fit_obs   0.947
_refine_ls_hydrogen_treatment    'H atoms refined isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2044
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.201
_refine_ls_restrained_S_obs      0.953
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_obs          0.0246
_refine_ls_shift/esd_max         0.411
_refine_ls_shift/esd_mean        0.055
_refine_ls_structure_factor_coef Fsqd
_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_wR_factor_all         0.0789
_refine_ls_wR_factor_obs         0.0579
_reflns_number_observed          1801
_reflns_number_total             2047
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    li1131.cif
_[local]_cod_data_source_block   aminopropyl
_cod_database_code               2003807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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)
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
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Ni 1 0.19412(5) 0.06399(4) 0.28971(3) 0.02152(12) Uani d . Ni
S 1 -0.25827(9) 0.26314(8) 0.30796(6) 0.0249(2) Uani d . S
O1 1 -0.1116(3) 0.1365(2) 0.3590(2) 0.0293(4) Uani d . O
O2 1 -0.4441(3) 0.2568(3) 0.3956(2) 0.0386(5) Uani d . O
O3 1 -0.1964(3) 0.4264(2) 0.2800(2) 0.0420(5) Uani d . O
O4 1 -0.2761(3) 0.2206(3) 0.2028(2) 0.0376(5) Uani d . O
O5 1 0.4906(3) -0.0164(3) 0.2314(2) 0.0334(5) Uani d D O
O6 1 0.2448(3) 0.0918(3) 0.4465(2) 0.0324(5) Uani d D O
O7 1 0.4214(4) 0.3143(3) 0.6229(2) 0.0563(7) Uani d D O
N1 1 0.1461(4) -0.1787(3) 0.3796(2) 0.0329(6) Uani d D N
N2 1 0.1406(3) 0.0495(3) 0.1336(2) 0.0285(5) Uani d D N
N3 1 0.2384(4) 0.3117(3) 0.2292(2) 0.0297(6) Uani d D N
C1 1 0.1260(6) -0.3045(4) 0.3209(4) 0.0499(9) Uani d D C
C2 1 0.0370(5) -0.2310(4) 0.2183(3) 0.0453(8) Uani d . C
C3 1 0.1606(5) -0.1214(4) 0.1185(3) 0.0417(8) Uani d . C
C4 1 0.2486(5) 0.1550(4) 0.0271(3) 0.0394(8) Uani d . C
C5 1 0.2126(5) 0.3368(4) 0.0281(3) 0.0452(8) Uani d . C
C6 1 0.3143(5) 0.3837(4) 0.1045(3) 0.0391(8) Uani d . C
HN1A 1 0.2436(39) -0.2143(38) 0.4117(26) 0.038(9) Uiso d D H
HN1B 1 0.0429(44) -0.1636(48) 0.4325(29) 0.067(13) Uiso d D H
HN2A 1 0.0198(35) 0.0896(36) 0.1396(27) 0.036(9) Uiso d D H
HN3A 1 0.3099(42) 0.3240(39) 0.2726(25) 0.040(9) Uiso d D H
HN3B 1 0.1258(37) 0.3658(36) 0.2532(27) 0.040(9) Uiso d D H
HC1A 1 0.2505(44) -0.3629(51) 0.3005(38) 0.085(15) Uiso d D H
HC1B 1 0.0539(46) -0.3838(38) 0.3761(26) 0.054(10) Uiso d D H
HC2A 1 0.0178(46) -0.3211(43) 0.1926(28) 0.045(9) Uiso d . H
HC2B 1 -0.0892(48) -0.1680(40) 0.2464(27) 0.040(9) Uiso d . H
HC3A 1 0.1278(46) -0.1121(39) 0.0448(29) 0.044(9) Uiso d . H
HC3B 1 0.2946(49) -0.1621(39) 0.1097(26) 0.039(9) Uiso d . H
HC4A 1 0.3873(48) 0.1151(38) 0.0255(25) 0.038(8) Uiso d . H
HC4B 1 0.2148(46) 0.1341(40) -0.0414(30) 0.049(9) Uiso d . H
HC5A 1 0.0682(54) 0.3733(42) 0.0508(29) 0.055(10) Uiso d . H
HC5B 1 0.2611(45) 0.3929(39) -0.0513(30) 0.044(9) Uiso d . H
HC6A 1 0.4503(46) 0.3411(36) 0.0862(25) 0.034(8) Uiso d . H
HC6B 1 0.3083(44) 0.4988(43) 0.0905(27) 0.042(9) Uiso d . H
HO5A 1 0.5617(53) 0.0542(44) 0.2294(35) 0.070(14) Uiso d D H
HO5B 1 0.5254(57) -0.1107(38) 0.2754(32) 0.074(14) Uiso d D H
HO6A 1 0.2322(54) 0.0075(38) 0.5073(26) 0.066(12) Uiso d D H
HO6B 1 0.3485(40) 0.1291(41) 0.4359(29) 0.049(11) Uiso d D H
HO7A 1 0.3549(52) 0.4031(38) 0.6391(34) 0.063(13) Uiso d D H
HO7B 1 0.4371(62) 0.3267(52) 0.5512(24) 0.078(15) Uiso d D H
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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N3 Ni N2 93.49(10) yes
N3 Ni N1 169.98(10) yes
N2 Ni N1 96.22(10) yes
N3 Ni O5 91.63(10) yes
N2 Ni O5 90.81(9) yes
N1 Ni O5 90.70(10) yes
N3 Ni O6 83.87(10) yes
N2 Ni O6 177.14(9) yes
N1 Ni O6 86.37(10) yes
O5 Ni O6 90.36(9) yes
N3 Ni O1 90.69(9) yes
N2 Ni O1 91.31(9) yes
N1 Ni O1 86.62(10) yes
O5 Ni O1 176.75(8) yes
O6 Ni O1 87.63(8) yes
O3 S O4 110.98(13) yes
O3 S O2 110.59(12) yes
O4 S O2 109.96(12) yes
O3 S O1 109.21(12) yes
O4 S O1 108.41(12) yes
O2 S O1 107.59(12) yes
S O1 Ni 131.76(11) yes
Ni O5 HO5A 112.(3) no
Ni O5 HO5B 111.(3) no
HO5A O5 HO5B 109.(4) no
Ni O6 HO6A 118.(2) no
Ni O6 HO6B 113.(2) no
HO6A O6 HO6B 110.(3) no
HO7A O7 HO7B 106.(4) no
C1 N1 Ni 122.7(2) yes
C1 N1 HN1A 109.(2) no
Ni N1 HN1A 103.(2) no
C1 N1 HN1B 110.(3) no
Ni N1 HN1B 103.(3) no
HN1A N1 HN1B 109.(3) no
C3 N2 C4 110.4(2) yes
C3 N2 Ni 114.2(2) yes
C4 N2 Ni 114.9(2) yes
C3 N2 HN2A 107.(2) no
C4 N2 HN2A 106.(2) no
Ni N2 HN2A 104.(2) no
C6 N3 Ni 122.0(2) yes
C6 N3 HN3A 112.(2) no
Ni N3 HN3A 104.(2) no
C6 N3 HN3B 109.(2) no
Ni N3 HN3B 104.(2) no
HN3A N3 HN3B 105.(3) no
N1 C1 C2 112.9(3) yes
N1 C1 HC1A 107.(3) no
C2 C1 HC1A 113.(3) no
N1 C1 HC1B 109.(2) no
C2 C1 HC1B 111.(2) no
HC1A C1 HC1B 104.(3) no
C1 C2 C3 114.0(3) yes
C1 C2 HC2A 106.(2) no
C3 C2 HC2A 109.(2) no
C1 C2 HC2B 107.4(18) no
C3 C2 HC2B 110.3(18) no
HC2A C2 HC2B 110.(3) no
N2 C3 C2 113.2(3) yes
N2 C3 HC3A 106.4(19) no
C2 C3 HC3A 111.7(19) no
N2 C3 HC3B 105.5(19) no
C2 C3 HC3B 111.8(19) no
HC3A C3 HC3B 108.(3) no
N2 C4 C5 113.9(3) yes
N2 C4 HC4A 105.2(18) no
C5 C4 HC4A 108.0(18) no
N2 C4 HC4B 107.3(19) no
C5 C4 HC4B 112.0(19) no
HC4A C4 HC4B 110.(3) no
C6 C5 C4 114.8(3) yes
C6 C5 HC5A 110.3(19) no
C4 C5 HC5A 109.5(19) no
C6 C5 HC5B 108.3(19) no
C4 C5 HC5B 105.3(19) no
HC5A C5 HC5B 108.(3) no
N3 C6 C5 111.8(3) yes
N3 C6 HC6A 106.7(18) no
C5 C6 HC6A 109.7(17) no
N3 C6 HC6B 111.2(19) no
C5 C6 HC6B 111.3(19) no
HC6A C6 HC6B 106.(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N3 2.084(2) yes
Ni N2 2.088(2) yes
Ni N1 2.099(3) yes
Ni O5 2.104(2) yes
Ni O6 2.127(2) yes
Ni O1 2.171(2) yes
S O3 1.460(2) yes
S O4 1.468(2) yes
S O2 1.474(2) yes
S O1 1.491(2) yes
O5 HO5A 0.85(3) no
O5 HO5B 0.87(3) no
O6 HO6A 0.88(3) no
O6 HO6B 0.84(2) no
O7 HO7A 0.85(3) no
O7 HO7B 0.83(3) no
N1 C1 1.481(4) yes
N1 HN1A 0.87(2) no
N1 HN1B 0.86(3) no
N2 C3 1.479(4) yes
N2 C4 1.483(4) yes
N2 HN2A 0.86(2) no
N3 C6 1.475(4) yes
N3 HN3A 0.87(2) no
N3 HN3B 0.87(2) no
C1 C2 1.497(5) yes
C1 HC1A 0.94(3) no
C1 HC1B 0.94(2) no
C2 C3 1.509(5) yes
C2 HC2A 0.94(3) no
C2 HC2B 0.99(3) no
C3 HC3A 0.97(3) no
C3 HC3B 0.95(3) no
C4 C5 1.510(5) yes
C4 HC4A 0.99(3) no
C4 HC4B 1.00(3) no
C5 C6 1.504(5) yes
C5 HC5A 1.01(4) no
C5 HC5B 0.96(3) no
C6 HC6A 0.97(3) no
C6 HC6B 0.94(3) no