#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/41/2234109.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_2234109
loop_
_publ_author_name
'Rusanova, Julia A.'
_publ_section_title
;
 Diaquabis(propane-1,3-diamine)nickel(II)
 bis(propane-1,3-diamine)disulfatonickelate(II)
;
_journal_coeditor_code           BR2192
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m400
_journal_page_last               m401
_journal_paper_doi               10.1107/S1600536812009750
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Ni (C3 H10 N2)2 (H2 O)2] [Ni (S O4)2 (C3 H10 N2)2]'
_chemical_formula_moiety         'C6 H24 N4 Ni O2 2+, C6 H20 N4 Ni O8 S2 2-'
_chemical_formula_sum            'C12 H44 N8 Ni2 O10 S2'
_chemical_formula_weight         642.1
_chemical_name_systematic
;
Diaquabis(propane-1,3-diamine)nickel(II)
bis(propane-1,3-diamine)disulfatonickelate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.016(2)
_cell_angle_beta                 103.795(2)
_cell_angle_gamma                105.7290(10)
_cell_formula_units_Z            1
_cell_length_a                   6.70550(10)
_cell_length_b                   8.9098(2)
_cell_length_c                   11.9504(4)
_cell_measurement_reflns_used    5917
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.50
_cell_volume                     634.52(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10425
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  0.7025
_exptl_absorpt_correction_T_min  0.4879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2009)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0341P)²+0.0694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                2728
_reflns_number_total             3078
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br2192.cif
_cod_data_source_block           I
_cod_database_code               2234109
_cod_database_fobs_code          2234109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Ni Ni1 0.5000 1.0000 0.0000 0.01064(8) Uani d S 1 1
Ni Ni2 0.5000 1.0000 0.5000 0.01320(8) Uani d S 1 1
S S1 0.89097(6) 1.01326(4) 0.23292(3) 0.01404(9) Uani d . 1 2
O O1 0.70097(16) 1.06228(13) 0.18226(9) 0.0155(2) Uani d . 1 2
O O2 1.05971(18) 1.06347(15) 0.17662(11) 0.0263(3) Uani d . 1 2
O O3 0.97660(18) 1.09600(14) 0.36389(10) 0.0240(3) Uani d . 1 2
O O4 0.8164(2) 0.83460(14) 0.20784(11) 0.0287(3) Uani d . 1 2
O O5 0.4535(2) 1.07096(17) 0.33786(11) 0.0246(3) Uani d . 1 2
N N1 0.2544(2) 0.83826(16) 0.03946(12) 0.0175(3) Uani d . 1 2
N N2 0.6059(2) 0.80081(15) -0.05714(12) 0.0155(3) Uani d . 1 2
N N3 0.6379(2) 0.82954(16) 0.43334(13) 0.0165(3) Uani d . 1 2
N N4 0.1851(2) 0.82026(17) 0.43194(13) 0.0180(3) Uani d . 1 2
C C1 0.1280(2) 0.67732(18) -0.05413(15) 0.0203(3) Uani d . 1 2
H H1A 0.0603 0.6943 -0.1294 0.024 Uiso calc R 1 2
H H1B 0.0126 0.6173 -0.0285 0.024 Uiso calc R 1 2
C C2 0.2734(3) 0.57695(18) -0.07559(15) 0.0222(3) Uani d . 1 2
H H2A 0.1811 0.4660 -0.1253 0.027 Uiso calc R 1 2
H H2B 0.3524 0.5713 0.0018 0.027 Uiso calc R 1 2
C C3 0.4379(3) 0.64240(18) -0.13651(14) 0.0200(3) Uani d . 1 2
H H3A 0.5084 0.5631 -0.1570 0.024 Uiso calc R 1 2
H H3B 0.3618 0.6566 -0.2112 0.024 Uiso calc R 1 2
C C4 0.5382(3) 0.65484(19) 0.42206(15) 0.0226(3) Uani d . 1 2
H H4A 0.5551 0.6437 0.5024 0.027 Uiso calc R 1 2
H H4B 0.6151 0.5921 0.3839 0.027 Uiso calc R 1 2
C C5 0.2966(3) 0.5844(2) 0.34818(16) 0.0264(4) Uani d . 1 2
H H5A 0.2774 0.6134 0.2738 0.032 Uiso calc R 1 2
H H5B 0.2489 0.4657 0.3263 0.032 Uiso calc R 1 2
C C6 0.1537(3) 0.64477(19) 0.41474(16) 0.0246(4) Uani d . 1 2
H H6A 0.0017 0.5803 0.3696 0.030 Uiso calc R 1 2
H H6B 0.1856 0.6275 0.4934 0.030 Uiso calc R 1 2
H H1 0.667(3) 0.788(2) 0.0068(17) 0.018(5) Uiso d . 1 2
H H2 0.707(3) 0.830(2) -0.0962(16) 0.018(4) Uiso d . 1 2
H H3 0.319(3) 0.826(2) 0.1079(18) 0.030(5) Uiso d . 1 2
H H4 0.165(3) 0.882(2) 0.0580(18) 0.031(6) Uiso d . 1 2
H H5 0.765(3) 0.868(2) 0.4867(18) 0.023(5) Uiso d . 1 2
H H6 0.663(3) 0.836(2) 0.3633(18) 0.029(5) Uiso d . 1 2
H H7 0.127(3) 0.852(2) 0.490(2) 0.037(6) Uiso d . 1 2
H H8 0.122(3) 0.828(2) 0.3723(18) 0.022(5) Uiso d . 1 2
H H9 0.533(4) 1.078(3) 0.295(2) 0.041(6) Uiso d . 1 2
H H10 0.357(4) 1.070(3) 0.299(2) 0.042(7) Uiso d . 1 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 Ni1 N1 2_675 . 180.0
N1 Ni1 N2 2_675 2_675 87.81(5)
N1 Ni1 N2 . 2_675 92.19(5)
N1 Ni1 N2 2_675 . 92.19(5)
N1 Ni1 N2 . . 87.81(5)
N2 Ni1 N2 2_675 . 180.0
N1 Ni1 O1 2_675 2_675 88.28(5)
N1 Ni1 O1 . 2_675 91.72(5)
N2 Ni1 O1 2_675 2_675 92.13(5)
N2 Ni1 O1 . 2_675 87.87(5)
N1 Ni1 O1 2_675 . 91.72(5)
N1 Ni1 O1 . . 88.28(5)
N2 Ni1 O1 2_675 . 87.87(5)
N2 Ni1 O1 . . 92.13(5)
O1 Ni1 O1 2_675 . 180.00(6)
N3 Ni2 N3 2_676 . 180.0000(10)
N3 Ni2 N4 2_676 2_676 91.66(5)
N3 Ni2 N4 . 2_676 88.34(5)
N3 Ni2 N4 2_676 . 88.34(5)
N3 Ni2 N4 . . 91.66(5)
N4 Ni2 N4 2_676 . 180.00(7)
N3 Ni2 O5 2_676 . 87.79(5)
N3 Ni2 O5 . . 92.21(5)
N4 Ni2 O5 2_676 . 87.84(5)
N4 Ni2 O5 . . 92.16(5)
N3 Ni2 O5 2_676 2_676 92.21(5)
N3 Ni2 O5 . 2_676 87.79(5)
N4 Ni2 O5 2_676 2_676 92.16(5)
N4 Ni2 O5 . 2_676 87.84(5)
O5 Ni2 O5 . 2_676 180.0000(10)
O3 S1 O4 . . 110.23(7)
O3 S1 O2 . . 110.28(7)
O4 S1 O2 . . 109.99(7)
O3 S1 O1 . . 107.70(6)
O4 S1 O1 . . 109.11(7)
O2 S1 O1 . . 109.48(6)
S1 O1 Ni1 . . 130.04(6)
Ni2 O5 H9 . . 127.9(16)
Ni2 O5 H10 . . 128.6(19)
H9 O5 H10 . . 101(2)
C1 N1 Ni1 . . 116.97(10)
C1 N1 H3 . . 110.9(12)
Ni1 N1 H3 . . 105.9(13)
C1 N1 H4 . . 108.0(13)
Ni1 N1 H4 . . 111.9(13)
H3 N1 H4 . . 102.2(18)
C3 N2 Ni1 . . 117.85(10)
C3 N2 H1 . . 108.5(12)
Ni1 N2 H1 . . 103.6(12)
C3 N2 H2 . . 107.8(11)
Ni1 N2 H2 . . 109.3(11)
H1 N2 H2 . . 109.5(16)
C4 N3 Ni2 . . 120.00(10)
C4 N3 H5 . . 108.9(13)
Ni2 N3 H5 . . 100.4(12)
C4 N3 H6 . . 108.8(12)
Ni2 N3 H6 . . 112.6(13)
H5 N3 H6 . . 104.8(17)
C6 N4 Ni2 . . 121.41(10)
C6 N4 H7 . . 106.6(13)
Ni2 N4 H7 . . 101.2(13)
C6 N4 H8 . . 107.8(14)
Ni2 N4 H8 . . 109.4(14)
H7 N4 H8 . . 110(2)
N1 C1 C2 . . 111.30(13)
N1 C1 H1A . . 109.4
C2 C1 H1A . . 109.4
N1 C1 H1B . . 109.4
C2 C1 H1B . . 109.4
H1A C1 H1B . . 108.0
C1 C2 C3 . . 115.06(13)
C1 C2 H2A . . 108.5
C3 C2 H2A . . 108.5
C1 C2 H2B . . 108.5
C3 C2 H2B . . 108.5
H2A C2 H2B . . 107.5
N2 C3 C2 . . 111.60(13)
N2 C3 H3A . . 109.3
C2 C3 H3A . . 109.3
N2 C3 H3B . . 109.3
C2 C3 H3B . . 109.3
H3A C3 H3B . . 108.0
N3 C4 C5 . . 112.50(13)
N3 C4 H4A . . 109.1
C5 C4 H4A . . 109.1
N3 C4 H4B . . 109.1
C5 C4 H4B . . 109.1
H4A C4 H4B . . 107.8
C6 C5 C4 . . 113.29(14)
C6 C5 H5A . . 108.9
C4 C5 H5A . . 108.9
C6 C5 H5B . . 108.9
C4 C5 H5B . . 108.9
H5A C5 H5B . . 107.7
N4 C6 C5 . . 113.15(13)
N4 C6 H6A . . 108.9
C5 C6 H6A . . 108.9
N4 C6 H6B . . 108.9
C5 C6 H6B . . 108.9
H6A C6 H6B . . 107.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 N1 2_675 2.0978(13)
Ni1 N1 . 2.0978(13)
Ni1 N2 2_675 2.1187(13)
Ni1 N2 . 2.1187(13)
Ni1 O1 2_675 2.1257(10)
Ni1 O1 . 2.1257(10)
Ni2 N3 2_676 2.0893(13)
Ni2 N3 . 2.0893(13)
Ni2 N4 2_676 2.1083(13)
Ni2 N4 . 2.1083(13)
Ni2 O5 . 2.1499(12)
Ni2 O5 2_676 2.1499(12)
S1 O3 . 1.4645(11)
S1 O4 . 1.4682(12)
S1 O2 . 1.4688(11)
S1 O1 . 1.4945(10)
O5 H9 . 0.82(2)
O5 H10 . 0.70(2)
N1 C1 . 1.4806(19)
N1 H3 . 0.88(2)
N1 H4 . 0.84(2)
N2 C3 . 1.4785(19)
N2 H1 . 0.823(19)
N2 H2 . 0.923(19)
N3 C4 . 1.479(2)
N3 H5 . 0.86(2)
N3 H6 . 0.90(2)
N4 C6 . 1.479(2)
N4 H7 . 0.91(2)
N4 H8 . 0.76(2)
C1 C2 . 1.518(2)
C1 H1A . 0.9700
C1 H1B . 0.9700
C2 C3 . 1.521(2)
C2 H2A . 0.9700
C2 H2B . 0.9700
C3 H3A . 0.9700
C3 H3B . 0.9700
C4 C5 . 1.521(2)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 C6 . 1.514(2)
C5 H5A . 0.9700
C5 H5B . 0.9700
C6 H6A . 0.9700
C6 H6B . 0.9700
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
O5 H9 O1 . 0.82(2) 1.96(2) 2.7739(16) 172(2)
N2 H1 O4 . 0.823(19) 2.265(19) 3.0528(18) 160.4(16)
N1 H4 O2 1_455 0.84(2) 2.28(2) 3.0621(18) 154.9(18)
O5 H10 O2 1_455 0.70(2) 2.15(3) 2.8476(18) 179(3)
N3 H5 O3 2_776 0.86(2) 2.06(2) 2.8900(17) 161.4(17)
N2 H2 O2 2_775 0.923(19) 2.145(19) 3.0600(17) 171.2(15)
N4 H7 O3 2_676 0.91(2) 2.03(2) 2.9269(18) 170(2)
