#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:53:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180361 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/30/7203048.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_7203048
loop_
_publ_author_name
'Aragoni, M. Carla'
'Arca, Massimiliano'
'Crespo, Miriam'
'Devillanova, Francesco A.'
'Hursthouse, Michael B.'
'Huth, Susanne L.'
'Isaia, Francesco'
'Lippolis, Vito'
'Verani, Gaetano'
_publ_section_title
;
 Predictable and unpredictable reactions between
 4,4′-dipyridyldisulfide and phosphonodithioato/dithiophosphato
 NiII complexes: novel coordination polymers and the unique example of
 4,4′-dipyridyltrisulfide
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              873
_journal_paper_doi               10.1039/b708972d
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C18 H28 N2 Ni O4 P2 S5'
_chemical_formula_weight         617.37
_chemical_name_systematic
;
?
;
_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                99.453(7)
_cell_angle_beta                 99.986(5)
_cell_angle_gamma                94.511(9)
_cell_formula_units_Z            2
_cell_length_a                   8.1601(4)
_cell_length_b                   9.4126(11)
_cell_length_c                   17.9991(9)
_cell_measurement_reflns_used    6130
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1334.85(19)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick ,1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'Φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49804
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.8839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.766
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0393
_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)+(0.0680P)²+1.8065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                5918
_reflns_number_total             6113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708972d.txt
_cod_data_source_block           04slh0874
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1334.85(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203048
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4916(3) 0.6770(3) 0.64256(16) 0.0217(5) Uani 1 1 d . . .
H1A H 0.4941 0.5790 0.6130 0.026 Uiso 1 1 calc R . .
H1B H 0.4077 0.6711 0.6759 0.026 Uiso 1 1 calc R . .
C2 C 0.6621(4) 0.7332(3) 0.69048(18) 0.0278(6) Uani 1 1 d . . .
H2A H 0.6950 0.6676 0.7261 0.042 Uiso 1 1 calc R . .
H2B H 0.6580 0.8300 0.7196 0.042 Uiso 1 1 calc R . .
H2C H 0.7441 0.7384 0.6569 0.042 Uiso 1 1 calc R . .
C3 C 0.1596(3) 0.9285(3) 0.44527(15) 0.0180(5) Uani 1 1 d . . .
H3A H 0.1258 1.0261 0.4607 0.022 Uiso 1 1 calc R . .
H3B H 0.0605 0.8566 0.4384 0.022 Uiso 1 1 calc R . .
C4 C 0.2221(4) 0.9207(3) 0.37116(16) 0.0248(6) Uani 1 1 d . . .
H4A H 0.1333 0.9406 0.3313 0.037 Uiso 1 1 calc R . .
H4B H 0.2544 0.8236 0.3558 0.037 Uiso 1 1 calc R . .
H4C H 0.3195 0.9928 0.3780 0.037 Uiso 1 1 calc R . .
C5 C -0.1323(4) 1.3297(4) -0.14551(19) 0.0313(7) Uani 1 1 d . . .
H5A H -0.1380 1.2278 -0.1717 0.038 Uiso 1 1 calc R . .
H5B H -0.0143 1.3640 -0.1213 0.038 Uiso 1 1 calc R . .
C6 C -0.1958(4) 1.4226(3) -0.20205(17) 0.0294(6) Uani 1 1 d . . .
H6A H -0.1273 1.4178 -0.2419 0.044 Uiso 1 1 calc R . .
H6B H -0.1890 1.5231 -0.1755 0.044 Uiso 1 1 calc R . .
H6C H -0.3125 1.3876 -0.2257 0.044 Uiso 1 1 calc R . .
C7 C -0.3767(6) 1.2624(6) 0.0876(3) 0.0551(10) Uani 1 1 d . . .
H7A H -0.2652 1.2651 0.1203 0.066 Uiso 1 1 calc R . .
H7B H -0.4358 1.1640 0.0812 0.066 Uiso 1 1 calc R . .
C8 C -0.4735(7) 1.3700(6) 0.1253(2) 0.0572(11) Uani 1 1 d . . .
H8A H -0.4861 1.3476 0.1754 0.086 Uiso 1 1 calc R . .
H8B H -0.5843 1.3663 0.0932 0.086 Uiso 1 1 calc R . .
H8C H -0.4141 1.4673 0.1322 0.086 Uiso 1 1 calc R . .
C10 C -0.1260(3) 0.6017(3) 0.35155(14) 0.0162(5) Uani 1 1 d . . .
H10 H -0.0513 0.5381 0.3331 0.019 Uiso 1 1 calc R . .
C11 C -0.2028(3) 0.6866(3) 0.30292(14) 0.0183(5) Uani 1 1 d . . .
H11 H -0.1802 0.6820 0.2526 0.022 Uiso 1 1 calc R . .
C12 C -0.3142(3) 0.7790(3) 0.32920(14) 0.0166(5) Uani 1 1 d . . .
C13 C -0.3482(3) 0.7769(3) 0.40244(14) 0.0151(4) Uani 1 1 d . . .
H13 H -0.4277 0.8346 0.4213 0.018 Uiso 1 1 calc R . .
C14 C -0.2640(3) 0.6894(3) 0.44689(14) 0.0138(4) Uani 1 1 d . . .
H14 H -0.2871 0.6893 0.4968 0.017 Uiso 1 1 calc R . .
C15 C -0.0751(3) 1.0344(3) 0.16124(15) 0.0203(5) Uani 1 1 d . . .
H15 H 0.0209 1.1037 0.1722 0.024 Uiso 1 1 calc R . .
C16 C -0.1594(4) 1.0154(3) 0.22019(15) 0.0224(5) Uani 1 1 d . . .
H16 H -0.1236 1.0721 0.2701 0.027 Uiso 1 1 calc R . .
C17 C -0.2970(3) 0.9117(3) 0.20451(15) 0.0199(5) Uani 1 1 d . . .
C18 C -0.3447(3) 0.8314(3) 0.13150(15) 0.0201(5) Uani 1 1 d . . .
H18 H -0.4369 0.7580 0.1196 0.024 Uiso 1 1 calc R . .
C19 C -0.2554(3) 0.8597(3) 0.07594(15) 0.0189(5) Uani 1 1 d . . .
H19 H -0.2899 0.8055 0.0254 0.023 Uiso 1 1 calc R . .
N1 N -0.1514(3) 0.6044(2) 0.42345(12) 0.0131(4) Uani 1 1 d . . .
N2 N -0.1230(3) 0.9597(2) 0.08975(12) 0.0166(4) Uani 1 1 d . . .
O1 O 0.4487(2) 0.77725(19) 0.59090(10) 0.0177(4) Uani 1 1 d . . .
O2 O 0.2912(2) 0.89902(19) 0.50476(11) 0.0175(4) Uani 1 1 d . . .
O3 O -0.2362(3) 1.3396(2) -0.08832(11) 0.0226(4) Uani 1 1 d . . .
O4 O -0.3575(3) 1.2924(3) 0.01637(13) 0.0376(6) Uani 1 1 d . . .
P1 P 0.27178(7) 0.75076(6) 0.53491(4) 0.01319(14) Uani 1 1 d . . .
P2 P -0.21660(8) 1.23433(7) -0.02731(4) 0.01853(15) Uani 1 1 d . . .
S1 S 0.25159(7) 0.57997(6) 0.45178(3) 0.01435(14) Uani 1 1 d . . .
S2 S 0.08119(7) 0.73379(6) 0.58956(3) 0.01465(14) Uani 1 1 d . . .
S3 S 0.00607(8) 1.26581(7) 0.04073(4) 0.01990(15) Uani 1 1 d . . .
S4 S -0.27102(8) 1.02856(7) -0.07772(4) 0.01962(15) Uani 1 1 d . . .
S5 S -0.42103(9) 0.89441(8) 0.27532(4) 0.02429(16) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.5000 0.5000 0.01090(11) Uani 1 2 d S . .
Ni2 Ni 0.0000 1.0000 0.0000 0.01417(12) Uani 1 2 d S . .
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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 107.4(2) . . ?
O1 C1 H1A 110.2 . . ?
C2 C1 H1A 110.2 . . ?
O1 C1 H1B 110.2 . . ?
C2 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O2 C3 C4 109.7(2) . . ?
O2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 C6 107.6(2) . . ?
O3 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
O3 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O4 C7 C8 110.3(4) . . ?
O4 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
O4 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C10 C11 123.5(2) . . ?
N1 C10 H10 118.3 . . ?
C11 C10 H10 118.3 . . ?
C10 C11 C12 118.7(2) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C11 C12 C13 118.2(2) . . ?
C11 C12 S5 124.54(19) . . ?
C13 C12 S5 117.21(19) . . ?
C14 C13 C12 118.7(2) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
N1 C14 C13 123.6(2) . . ?
N1 C14 H14 118.2 . . ?
C13 C14 H14 118.2 . . ?
N2 C15 C16 123.0(3) . . ?
N2 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
C17 C16 C15 118.4(2) . . ?
C17 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
C18 C17 C16 119.1(2) . . ?
C18 C17 S5 120.5(2) . . ?
C16 C17 S5 120.2(2) . . ?
C17 C18 C19 118.6(3) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
N2 C19 C18 123.3(2) . . ?
N2 C19 H19 118.4 . . ?
C18 C19 H19 118.4 . . ?
C10 N1 C14 117.1(2) . . ?
C10 N1 Ni1 121.06(16) . . ?
C14 N1 Ni1 121.39(16) . . ?
C19 N2 C15 117.7(2) . . ?
C19 N2 Ni2 120.36(17) . . ?
C15 N2 Ni2 121.96(18) . . ?
C1 O1 P1 119.44(16) . . ?
C3 O2 P1 118.78(15) . . ?
C5 O3 P2 119.19(17) . . ?
C7 O4 P2 123.4(3) . . ?
O2 P1 O1 95.30(10) . . ?
O2 P1 S1 112.33(8) . . ?
O1 P1 S1 113.01(8) . . ?
O2 P1 S2 113.25(8) . . ?
O1 P1 S2 113.00(8) . . ?
S1 P1 S2 109.44(4) . . ?
O4 P2 O3 96.07(12) . . ?
O4 P2 S3 111.87(9) . . ?
O3 P2 S3 113.30(9) . . ?
O4 P2 S4 112.62(11) . . ?
O3 P2 S4 111.46(8) . . ?
S3 P2 S4 110.80(4) . . ?
P1 S1 Ni1 84.35(3) . . ?
P1 S2 Ni1 84.28(3) . . ?
P2 S3 Ni2 83.10(3) . . ?
P2 S4 Ni2 83.61(3) . . ?
C12 S5 C17 102.70(12) . . ?
N1 Ni1 N1 180.00(9) . 2_566 ?
N1 Ni1 S2 89.70(6) . . ?
N1 Ni1 S2 90.30(6) 2_566 . ?
N1 Ni1 S2 90.30(6) . 2_566 ?
N1 Ni1 S2 89.70(6) 2_566 2_566 ?
S2 Ni1 S2 180.0 . 2_566 ?
N1 Ni1 S1 90.78(6) . . ?
N1 Ni1 S1 89.22(6) 2_566 . ?
S2 Ni1 S1 81.89(2) . . ?
S2 Ni1 S1 98.11(2) 2_566 . ?
N1 Ni1 S1 89.22(6) . 2_566 ?
N1 Ni1 S1 90.78(6) 2_566 2_566 ?
S2 Ni1 S1 98.11(2) . 2_566 ?
S2 Ni1 S1 81.89(2) 2_566 2_566 ?
S1 Ni1 S1 180.000(1) . 2_566 ?
N2 Ni2 N2 180.00(12) . 2_575 ?
N2 Ni2 S4 90.34(6) . 2_575 ?
N2 Ni2 S4 89.66(6) 2_575 2_575 ?
N2 Ni2 S4 89.66(6) . . ?
N2 Ni2 S4 90.34(6) 2_575 . ?
S4 Ni2 S4 180.0 2_575 . ?
N2 Ni2 S3 88.69(6) . 2_575 ?
N2 Ni2 S3 91.31(6) 2_575 2_575 ?
S4 Ni2 S3 82.41(2) 2_575 2_575 ?
S4 Ni2 S3 97.59(2) . 2_575 ?
N2 Ni2 S3 91.31(6) . . ?
N2 Ni2 S3 88.69(6) 2_575 . ?
S4 Ni2 S3 97.59(2) 2_575 . ?
S4 Ni2 S3 82.41(2) . . ?
S3 Ni2 S3 180.00(3) 2_575 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.451(3) . ?
C1 C2 1.509(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 O2 1.457(3) . ?
C3 C4 1.501(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 O3 1.439(3) . ?
C5 C6 1.500(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 O4 1.389(5) . ?
C7 C8 1.482(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 N1 1.342(3) . ?
C10 C11 1.385(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.396(3) . ?
C12 S5 1.756(2) . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 N1 1.342(3) . ?
C14 H14 0.9500 . ?
C15 N2 1.337(3) . ?
C15 C16 1.388(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(4) . ?
C17 S5 1.779(3) . ?
C18 C19 1.383(4) . ?
C18 H18 0.9500 . ?
C19 N2 1.336(3) . ?
C19 H19 0.9500 . ?
N1 Ni1 2.106(2) . ?
N2 Ni2 2.113(2) . ?
O1 P1 1.5866(18) . ?
O2 P1 1.5847(18) . ?
O3 P2 1.592(2) . ?
O4 P2 1.584(2) . ?
P1 S1 1.9832(9) . ?
P1 S2 1.9887(9) . ?
P2 S3 1.9782(10) . ?
P2 S4 1.9798(10) . ?
S1 Ni1 2.4747(6) . ?
S2 Ni1 2.4729(6) . ?
S3 Ni2 2.4830(7) . ?
S4 Ni2 2.4626(6) . ?
Ni1 N1 2.106(2) 2_566 ?
Ni1 S2 2.4729(6) 2_566 ?
Ni1 S1 2.4747(6) 2_566 ?
Ni2 N2 2.113(2) 2_575 ?
Ni2 S4 2.4626(6) 2_575 ?
Ni2 S3 2.4830(7) 2_575 ?
