#------------------------------------------------------------------------------
#$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2009087.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_2009087
loop_
_publ_author_name
'Freire, E.'
'Baggio, S.'
'Baggio, R.'
'Suescun, L.'
_publ_section_title
;
Triaqua(2,2'-bipyridyl-N,N')(thiosulfato-S)nickel(II)
dihydrate and
triaqua(1,10-phenanthroline-N,N')(thiosulfato-S)nickel(II)
monohydrate
;
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 1780
_journal_page_last 1784
_journal_volume 55
_journal_year 1999
_chemical_formula_iupac '[Ni (S2 O3) (C12 H8 N2) (H2 O1)3], H2 O1'
_chemical_formula_sum 'C12 H16 N2 Ni O7 S2'
_chemical_formula_weight 423.10
_chemical_name_systematic
;
Triaqua-(2,10-phenanthroline-N,N')-(thiosulfato-S)-nickel(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-97
_cell_angle_alpha 90.47(3)
_cell_angle_beta 91.27(3)
_cell_angle_gamma 104.23(3)
_cell_formula_units_Z 2
_cell_length_a 8.434(2)
_cell_length_b 8.782(2)
_cell_length_c 11.344(2)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 7.5
_cell_volume 814.2(3)
_computing_cell_refinement 'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1988)
;
_computing_data_reduction 'MSC/AFC Diffractometer Control Software'
_computing_molecular_graphics 'XP in SHELXTL/PC (Sheldrick,1994)'
_computing_publication_material
'PARST (Nardelli, 1983) and CSD (Allen & Kennard, 1993)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'Rigaku AFC-7S'
_diffrn_measurement_method \w/2\q
_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 0.022
_diffrn_reflns_av_sigmaI/netI 0.019
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 3982
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 2.39
_diffrn_standards_decay_% <3
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.49
_exptl_absorpt_correction_T_max 0.87
_exptl_absorpt_correction_T_min 0.65
_exptl_absorpt_correction_type '\y scan'
_exptl_absorpt_process_details '(Molecular Structure Corporation, 1988)'
_exptl_crystal_colour 'light blue'
_exptl_crystal_density_diffrn 1.73
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 436
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.40
_refine_diff_density_min -0.59
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.09
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 250
_refine_ls_number_reflns 3738
_refine_ls_R_factor_all 0.026
_refine_ls_R_factor_gt 0.025
_refine_ls_shift/su_max <0.01
_refine_ls_shift/su_mean <0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.035P)^2^+0.460P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref 0.071
_reflns_number_gt 3566
_reflns_number_total 3738
_reflns_threshold_expression I>2\s(I)
_[local]_cod_data_source_file bk1471.cif
_[local]_cod_data_source_block II
_[local]_cod_cif_authors_sg_H-M 'P -1 '
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.
'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).
'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (16
times).
'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (48
times).
'_geom_torsion_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (65 times).
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_database_code 2009087
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_type_symbol
Ni1 0.29519(2) 0.24412(2) 0.299088(17) 0.02081(7) Uani d . 1 Ni
S1 0.54825(5) 0.42774(5) 0.23985(4) 0.02758(10) Uani d . 1 S
S2 0.74157(5) 0.45253(5) 0.35055(4) 0.02623(10) Uani d . 1 S
O1 0.69127(16) 0.36762(18) 0.46170(12) 0.0364(3) Uani d . 1 O
O2 0.86783(17) 0.3931(2) 0.29355(14) 0.0459(4) Uani d . 1 O
O3 0.80137(19) 0.62163(17) 0.37856(13) 0.0422(3) Uani d . 1 O
N1 0.35981(17) 0.04395(16) 0.24144(12) 0.0240(3) Uani d . 1 N
N2 0.22031(17) 0.24226(17) 0.12434(12) 0.0241(3) Uani d . 1 N
C1 0.4326(2) -0.0512(2) 0.30002(16) 0.0328(4) Uani d . 1 C
H1B 0.4670 -0.0259 0.3778 0.039 Uiso calc R 1 H
C2 0.4600(3) -0.1885(2) 0.24942(19) 0.0400(4) Uani d . 1 C
H2B 0.5116 -0.2524 0.2931 0.048 Uiso calc R 1 H
C3 0.4104(3) -0.2272(2) 0.13609(19) 0.0377(4) Uani d . 1 C
H3B 0.4270 -0.3185 0.1020 0.045 Uiso calc R 1 H
C4 0.3339(2) -0.1291(2) 0.07020(17) 0.0304(4) Uani d . 1 C
C5 0.2797(3) -0.1587(2) -0.05027(18) 0.0383(4) Uani d . 1 C
H5A 0.2918 -0.2494 -0.0881 0.046 Uiso calc R 1 H
C6 0.2117(3) -0.0579(3) -0.10962(17) 0.0400(5) Uani d . 1 C
H6A 0.1773 -0.0802 -0.1877 0.048 Uiso calc R 1 H
C7 0.1913(2) 0.0836(2) -0.05465(15) 0.0310(4) Uani d . 1 C
C8 0.1293(3) 0.1981(3) -0.11371(17) 0.0396(5) Uani d . 1 C
H8A 0.0973 0.1839 -0.1928 0.047 Uiso calc R 1 H
C9 0.1167(3) 0.3300(3) -0.05395(18) 0.0414(5) Uani d . 1 C
H9A 0.0787 0.4075 -0.0926 0.050 Uiso calc R 1 H
C10 0.1614(2) 0.3477(2) 0.06594(17) 0.0326(4) Uani d . 1 C
H10A 0.1494 0.4367 0.1062 0.039 Uiso calc R 1 H
C11 0.2382(2) 0.1138(2) 0.06444(14) 0.0241(3) Uani d . 1 C
C12 0.31172(19) 0.00643(19) 0.12771(14) 0.0238(3) Uani d . 1 C
O1W 0.37137(18) 0.22882(17) 0.47174(12) 0.0303(3) Uani d . 1 O
H1WA 0.327(4) 0.270(4) 0.515(3) 0.058(9) Uiso d . 1 H
H1WB 0.472(4) 0.282(3) 0.473(2) 0.049(7) Uiso d . 1 H
O2W 0.19318(17) 0.43142(16) 0.33647(12) 0.0314(3) Uani d . 1 O
H2WB 0.096(4) 0.417(3) 0.333(2) 0.045(7) Uiso d . 1 H
H2WA 0.234(4) 0.500(3) 0.391(3) 0.054(8) Uiso d . 1 H
O3W 0.07151(17) 0.09086(17) 0.34605(12) 0.0311(3) Uani d . 1 O
H3WB 0.020(4) 0.126(3) 0.390(2) 0.048(8) Uiso d . 1 H
H3WA 0.086(3) 0.011(3) 0.375(2) 0.047(7) Uiso d . 1 H
O4W 1.0872(2) 0.81431(18) 0.46086(15) 0.0405(3) Uani d . 1 O
H4WB 1.009(4) 0.744(4) 0.432(3) 0.062(9) Uiso d . 1 H
H4WA 1.162(4) 0.776(4) 0.482(3) 0.065(9) Uiso 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 0.02055(11) 0.02355(12) 0.01987(11) 0.00851(8) 0.00020(8) -0.00288(8)
S1 0.02071(19) 0.0310(2) 0.0314(2) 0.00708(16) -0.00087(15) 0.00399(16)
S2 0.01843(18) 0.0340(2) 0.0270(2) 0.00819(15) 0.00047(15) -0.00763(16)
O1 0.0277(6) 0.0487(8) 0.0328(7) 0.0096(6) -0.0040(5) 0.0043(6)
O2 0.0263(7) 0.0743(11) 0.0447(8) 0.0274(7) -0.0008(6) -0.0177(7)
O3 0.0405(8) 0.0374(8) 0.0421(8) -0.0024(6) 0.0020(6) -0.0140(6)
N1 0.0268(7) 0.0244(7) 0.0227(6) 0.0097(5) 0.0023(5) -0.0009(5)
N2 0.0217(6) 0.0268(7) 0.0244(7) 0.0073(5) 0.0002(5) 0.0001(5)
C1 0.0410(10) 0.0336(9) 0.0283(9) 0.0182(8) 0.0002(7) 0.0010(7)
C2 0.0491(12) 0.0332(10) 0.0448(11) 0.0234(9) 0.0056(9) 0.0041(8)
C3 0.0424(11) 0.0253(8) 0.0480(11) 0.0129(8) 0.0099(9) -0.0045(8)
C4 0.0292(9) 0.0281(8) 0.0327(9) 0.0046(7) 0.0068(7) -0.0073(7)
C5 0.0398(10) 0.0378(10) 0.0341(10) 0.0034(8) 0.0064(8) -0.0158(8)
C6 0.0374(10) 0.0532(12) 0.0247(9) 0.0025(9) 0.0014(7) -0.0142(8)
C7 0.0253(8) 0.0431(10) 0.0217(8) 0.0028(7) 0.0010(6) -0.0020(7)
C8 0.0349(10) 0.0603(13) 0.0222(8) 0.0095(9) -0.0026(7) 0.0056(8)
C9 0.0380(10) 0.0556(13) 0.0345(10) 0.0188(9) -0.0014(8) 0.0167(9)
C10 0.0316(9) 0.0362(9) 0.0332(9) 0.0140(7) 0.0001(7) 0.0056(7)
C11 0.0199(7) 0.0294(8) 0.0217(7) 0.0038(6) 0.0021(6) -0.0008(6)
C12 0.0215(7) 0.0252(7) 0.0241(8) 0.0047(6) 0.0036(6) -0.0029(6)
O1W 0.0275(7) 0.0394(7) 0.0241(6) 0.0087(6) 0.0000(5) -0.0024(5)
O2W 0.0251(6) 0.0350(7) 0.0376(7) 0.0147(5) -0.0019(5) -0.0113(6)
O3W 0.0287(7) 0.0317(7) 0.0332(7) 0.0075(5) 0.0038(5) 0.0012(6)
O4W 0.0321(7) 0.0313(7) 0.0586(10) 0.0090(6) 0.0002(7) 0.0026(6)
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'
S S 0.1246 0.1234 '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'
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
O1W Ni1 N2 175.69(5) n
O1W Ni1 N1 95.18(6) n
N2 Ni1 N1 80.63(6) n
O1W Ni1 O2W 93.02(6) n
N2 Ni1 O2W 91.03(6) n
N1 Ni1 O2W 169.51(6) n
O1W Ni1 O3W 86.59(6) n
N2 Ni1 O3W 92.06(6) n
N1 Ni1 O3W 85.79(6) n
O2W Ni1 O3W 88.19(6) n
O1W Ni1 S1 95.18(5) n
N2 Ni1 S1 86.29(5) n
N1 Ni1 S1 95.52(5) n
O2W Ni1 S1 90.23(5) n
O3W Ni1 S1 177.69(4) n
S2 S1 Ni1 116.33(3) n
O2 S2 O3 110.66(10) n
O2 S2 O1 110.87(10) n
O3 S2 O1 108.55(9) n
O2 S2 S1 109.27(7) n
O3 S2 S1 107.34(8) n
O1 S2 S1 110.08(6) n
C1 N1 C12 118.10(15) n
C1 N1 Ni1 129.66(12) n
C12 N1 Ni1 112.18(11) n
C10 N2 C11 118.13(15) n
C10 N2 Ni1 129.28(13) n
C11 N2 Ni1 112.59(11) n
N1 C1 C2 122.65(18) n
C3 C2 C1 119.36(18) n
C2 C3 C4 119.99(17) n
C12 C4 C3 116.90(17) n
C12 C4 C5 119.05(18) n
C3 C4 C5 124.05(17) n
C6 C5 C4 121.22(18) n
C5 C6 C7 121.19(17) n
C11 C7 C8 116.98(18) n
C11 C7 C6 119.05(18) n
C8 C7 C6 123.96(18) n
C9 C8 C7 119.52(17) n
C8 C9 C10 119.55(18) n
N2 C10 C9 122.50(19) n
N2 C11 C7 123.24(17) n
N2 C11 C12 117.03(15) n
C7 C11 C12 119.72(16) n
N1 C12 C4 122.99(16) n
N1 C12 C11 117.29(14) n
C4 C12 C11 119.71(16) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 2.0695(14) y
Ni1 N2 2.0658(15) y
Ni1 O1W 2.0634(14) y
Ni1 O2W 2.0800(14) y
Ni1 O3W 2.1125(15) y
Ni1 S1 2.4488(10) y
S1 S2 2.0031(9) y
S2 O1 1.4865(15) y
S2 O2 1.4570(14) y
S2 O3 1.4757(15) y
N1 C1 1.327(2) n
N1 C12 1.357(2) n
N2 C10 1.328(2) n
N2 C11 1.354(2) n
C1 C2 1.403(3) n
C2 C3 1.357(3) n
C3 C4 1.407(3) n
C4 C12 1.407(2) n
C4 C5 1.433(3) n
C5 C6 1.345(3) n
C6 C7 1.435(3) n
C7 C11 1.404(2) n
C7 C8 1.409(3) n
C8 C9 1.365(3) n
C9 C10 1.400(3) n
C11 C12 1.438(2) n
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
O1W H1WA O3 2_666 0.76(3) 2.02(3) 2.783(2) 175(3)
O1W H1WB O1 1_555 0.86(2) 1.82(2) 2.679(2) 170(3)
O2W H2WA O1 2_666 0.86(2) 2.02(2) 2.880(2) 170(2)
O2W H2WB O2 1_455 0.80(3) 1.92(3) 2.714(2) 168(3)
O3W H3WA O4W 1_445 0.81(3) 1.99(3) 2.795(2) 170(2)
O3W H3WB O4W 2_666 0.78(3) 2.05(3) 2.816(2) 164(2)
O4W H4WA O1 2_766 0.82(3) 2.06(3) 2.869(2) 167(3)
O4W H4WB O3 1_555 0.84(2) 1.90(3) 2.723(2) 165(3)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
O1W Ni1 S1 S2 14.52(5) n
N2 Ni1 S1 S2 -161.41(5) n
N1 Ni1 S1 S2 -81.22(5) n
O2W Ni1 S1 S2 107.57(5) n
O3W Ni1 S1 S2 154.3(10) n
Ni1 S1 S2 O2 114.41(9) n
Ni1 S1 S2 O3 -125.55(7) n
Ni1 S1 S2 O1 -7.57(7) n
O1W Ni1 N1 C1 -2.86(17) n
N2 Ni1 N1 C1 178.17(17) n
O2W Ni1 N1 C1 -144.2(3) n
O3W Ni1 N1 C1 -89.05(17) n
S1 Ni1 N1 C1 92.86(16) n
O1W Ni1 N1 C12 174.18(11) n
N2 Ni1 N1 C12 -4.79(11) n
O2W Ni1 N1 C12 32.9(4) n
O3W Ni1 N1 C12 88.00(12) n
S1 Ni1 N1 C12 -90.09(11) n
O1W Ni1 N2 C10 171.4(7) n
N1 Ni1 N2 C10 -174.89(16) n
O2W Ni1 N2 C10 11.50(16) n
O3W Ni1 N2 C10 99.72(16) n
S1 Ni1 N2 C10 -78.66(15) n
O1W Ni1 N2 C11 -9.5(8) n
N1 Ni1 N2 C11 4.23(11) n
O2W Ni1 N2 C11 -169.38(11) n
O3W Ni1 N2 C11 -81.16(12) n
S1 Ni1 N2 C11 100.46(11) n
C12 N1 C1 C2 -0.6(3) n
Ni1 N1 C1 C2 176.28(15) n
N1 C1 C2 C3 -0.1(3) n
C1 C2 C3 C4 0.6(3) n
C2 C3 C4 C12 -0.5(3) n
C2 C3 C4 C5 179.00(19) n
C12 C4 C5 C6 1.5(3) n
C3 C4 C5 C6 -178.0(2) n
C4 C5 C6 C7 0.2(3) n
C5 C6 C7 C11 -2.3(3) n
C5 C6 C7 C8 176.39(19) n
C11 C7 C8 C9 -0.4(3) n
C6 C7 C8 C9 -179.09(19) n
C7 C8 C9 C10 -1.7(3) n
C11 N2 C10 C9 0.4(3) n
Ni1 N2 C10 C9 179.51(14) n
C8 C9 C10 N2 1.8(3) n
C10 N2 C11 C7 -2.7(2) n
Ni1 N2 C11 C7 178.05(13) n
C10 N2 C11 C12 176.18(15) n
Ni1 N2 C11 C12 -3.05(18) n
C8 C7 C11 N2 2.7(3) n
C6 C7 C11 N2 -178.54(16) n
C8 C7 C11 C12 -176.16(16) n
C6 C7 C11 C12 2.6(3) n
C1 N1 C12 C4 0.8(2) n
Ni1 N1 C12 C4 -176.62(13) n
C1 N1 C12 C11 -177.90(15) n
Ni1 N1 C12 C11 4.68(18) n
C3 C4 C12 N1 -0.3(3) n
C5 C4 C12 N1 -179.76(16) n
C3 C4 C12 C11 178.40(16) n
C5 C4 C12 C11 -1.1(2) n
N2 C11 C12 N1 -1.1(2) n
C7 C11 C12 N1 177.81(15) n
N2 C11 C12 C4 -179.87(15) n
C7 C11 C12 C4 -0.9(2) n