#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/91/2239174.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_2239174
loop_
_publ_author_name
'Sahbani, Thameur'
'Smirani Sta, Wajda'
'Rzaigui, Mohamed'
_publ_section_title
;
 Bis(4-aminopyridinium) hexaaquanickel(II) bis(sulfate)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m6
_journal_paper_doi               10.1107/S1600536813032558
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C5 H7 N2)2 [Ni (H2 O)6] (S O4)2'
_chemical_formula_moiety         'H12 Ni O6 2+, 2(C5 H7 N2 +), 2(O4 S 2-)'
_chemical_formula_sum            'C10 H26 N4 Ni O14 S2'
_chemical_formula_weight         549.18
_chemical_name_systematic
;
Bis(4-aminopyridinium) hexaaquanickel(II) bis(sulfate)
;
_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                100.61(3)
_cell_angle_beta                 99.26(2)
_cell_angle_gamma                99.57(2)
_cell_formula_units_Z            1
_cell_length_a                   6.212(2)
_cell_length_b                   7.015(3)
_cell_length_c                   12.422(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     514.3(3)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf--Nonius TurboCAD-4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            5919
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             286
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.752
_refine_diff_density_min         -1.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5022
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0459P)²+0.2397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                3986
_reflns_number_total             5022
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2787sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2239174
_cod_database_fobs_code          2239174
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 0.0000 0.0000 0.0000 0.01654(6) Uani d S 1 2
O O1 0.15341(17) -0.21342(15) -0.07350(9) 0.02370(18) Uani d D 1 1
O O2 0.28416(17) 0.11424(15) 0.12233(10) 0.0257(2) Uani d D 1 1
O O3 0.10291(17) 0.16756(15) -0.10704(9) 0.02297(18) Uani d . 1 1
C C1 0.9486(2) -0.2906(2) 0.45752(12) 0.0243(2) Uani d . 1 1
N N2 0.9660(3) -0.1384(2) 0.68016(12) 0.0418(4) Uani d . 1 1
H H1 0.9714 -0.0903 0.7496 0.050 Uiso calc R 1 1
C C3 0.7706(3) -0.2354(3) 0.61472(15) 0.0395(4) Uani d . 1 1
H H3 0.6434 -0.2507 0.6454 0.047 Uiso calc R 1 1
C C5 1.1512(3) -0.1901(2) 0.53005(15) 0.0316(3) Uani d . 1 1
H H5 1.2830 -0.1752 0.5032 0.038 Uiso calc R 1 1
C C4 1.1524(3) -0.1156(3) 0.63905(16) 0.0389(4) Uani d . 1 1
H H4 1.2856 -0.0473 0.6861 0.047 Uiso calc R 1 1
N N1 0.9396(3) -0.3609(3) 0.35006(12) 0.0338(3) Uani d . 1 1
C C2 0.7559(3) -0.3115(3) 0.50454(13) 0.0305(3) Uani d . 1 1
H H2 0.6191 -0.3773 0.4601 0.037 Uiso calc R 1 1
H H103 0.056(4) 0.261(3) -0.1106(18) 0.030(5) Uiso d . 1 1
H H203 0.236(3) 0.205(3) -0.1029(16) 0.023(4) Uiso d . 1 1
H H7 1.061(5) -0.333(4) 0.327(2) 0.062(8) Uiso d . 1 1
H H6 0.827(5) -0.410(4) 0.307(2) 0.048(7) Uiso d . 1 1
S S1 0.62063(5) 0.35433(4) 0.81367(3) 0.02033(7) Uani d . 1 1
O O5 0.85539(16) 0.44487(16) 0.86606(11) 0.0306(2) Uani d . 1 1
O O7 0.53371(17) 0.21768(17) 0.88249(10) 0.0295(2) Uani d . 1 1
O O4 0.48753(19) 0.50858(17) 0.81131(13) 0.0354(3) Uani d . 1 1
O O6 0.6085(2) 0.2407(2) 0.70136(11) 0.0420(3) Uani d . 1 1
H H1O1 0.257(3) -0.228(3) -0.0278(18) 0.047(7) Uiso d D 1 1
H H2O1 0.065(4) -0.327(3) -0.098(2) 0.059(8) Uiso d D 1 1
H H1O2 0.363(4) 0.225(2) 0.129(2) 0.047(7) Uiso d D 1 1
H H2O2 0.367(3) 0.034(3) 0.1328(19) 0.032(5) Uiso d D 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3147 0.7232 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 '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'
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
O3 Ni1 O3 2 . 180.00(5)
O3 Ni1 O1 2 . 92.26(5)
O3 Ni1 O1 . . 87.74(5)
O3 Ni1 O1 2 2 87.74(5)
O3 Ni1 O1 . 2 92.26(5)
O1 Ni1 O1 . 2 180.00(7)
O3 Ni1 O2 2 2 93.96(5)
O3 Ni1 O2 . 2 86.04(5)
O1 Ni1 O2 . 2 89.83(5)
O1 Ni1 O2 2 2 90.17(5)
O3 Ni1 O2 2 . 86.04(5)
O3 Ni1 O2 . . 93.96(5)
O1 Ni1 O2 . . 90.17(5)
O1 Ni1 O2 2 . 89.83(5)
O2 Ni1 O2 2 . 180.00(7)
Ni1 O1 H1O1 . . 109.7(18)
Ni1 O1 H2O1 . . 112.7(19)
H1O1 O1 H2O1 . . 107.0(19)
Ni1 O2 H1O2 . . 123.5(17)
Ni1 O2 H2O2 . . 114.9(14)
H1O2 O2 H2O2 . . 108.4(18)
Ni1 O3 H103 . . 118.3(16)
Ni1 O3 H203 . . 118.9(13)
H103 O3 H203 . . 103.5(18)
N1 C1 C2 . . 121.41(14)
N1 C1 C5 . . 121.51(14)
C2 C1 C5 . . 117.08(14)
C4 N2 C3 . . 121.02(15)
C4 N2 H1 . . 119.5
C3 N2 H1 . . 119.5
N2 C3 C2 . . 121.01(17)
N2 C3 H3 . . 119.5
C2 C3 H3 . . 119.5
C4 C5 C1 . . 119.69(16)
C4 C5 H5 . . 120.2
C1 C5 H5 . . 120.2
N2 C4 C5 . . 121.31(16)
N2 C4 H4 . . 119.3
C5 C4 H4 . . 119.3
C1 N1 H7 . . 115.4(19)
C1 N1 H6 . . 123(2)
H7 N1 H6 . . 121(3)
C3 C2 C1 . . 119.88(16)
C3 C2 H2 . . 120.1
C1 C2 H2 . . 120.1
O6 S1 O4 . . 111.02(9)
O6 S1 O5 . . 109.76(8)
O4 S1 O5 . . 110.07(7)
O6 S1 O7 . . 108.89(8)
O4 S1 O7 . . 109.07(8)
O5 S1 O7 . . 107.96(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O3 2 2.0388(11)
Ni1 O3 . 2.0388(11)
Ni1 O1 . 2.0578(12)
Ni1 O1 2 2.0578(12)
Ni1 O2 2 2.0701(12)
Ni1 O2 . 2.0701(12)
O1 H1O1 . 0.818(15)
O1 H2O1 . 0.860(15)
O2 H1O2 . 0.828(15)
O2 H2O2 . 0.839(14)
O3 H103 . 0.77(2)
O3 H203 . 0.82(2)
C1 N1 . 1.324(2)
C1 C2 . 1.412(2)
C1 C5 . 1.413(2)
N2 C4 . 1.336(3)
N2 C3 . 1.342(3)
N2 H1 . 0.8600
C3 C2 . 1.357(2)
C3 H3 . 0.9300
C5 C4 . 1.357(3)
C5 H5 . 0.9300
C4 H4 . 0.9300
N1 H7 . 0.85(3)
N1 H6 . 0.79(3)
C2 H2 . 0.9300
S1 O6 . 1.4574(14)
S1 O4 . 1.4686(12)
S1 O5 . 1.4793(12)
S1 O7 . 1.4897(12)
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
N2 H1 O2 2_656 0.86 2.43 3.102(2) 136 yes
N2 H1 O3 1_656 0.86 2.23 2.983(2) 147 yes
O1 H1O1 O7 2_656 0.82(2) 2.03(2) 2.8231(16) 163(2) yes
O1 H2O1 O5 1_444 0.86(2) 1.82(2) 2.6741(16) 172(2) yes
O2 H1O2 O4 2_666 0.832(18) 1.895(17) 2.6952(17) 161(2) yes
O2 H2O2 O7 2_656 0.84(2) 1.95(2) 2.7480(16) 159(2) yes
N1 H6 O4 2_656 0.80(3) 2.17(3) 2.957(2) 173(3) yes
N1 H7 O5 2_756 0.86(3) 2.55(3) 3.153(2) 129(2) yes
N1 H7 O6 2_756 0.86(3) 2.15(3) 2.998(2) 170(2) yes
O3 H103 O5 1_454 0.77(2) 1.96(2) 2.7072(15) 164(2) yes
O3 H203 O7 1_554 0.815(19) 1.876(19) 2.6682(15) 164(2) yes
