#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/59/2215957.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_2215957
loop_
_publ_author_name
'Hill, Denise D.'
'Tiekink, Edward R. T.'
_publ_section_title
;catena-Poly[[bis(O-isopropyl
 dithiocarbonato-κ²S,S')nickel(II)]-μ-1,2-di-4-pyridylethane-κ²N:N']
;
_journal_coeditor_code           HB2592
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2808
_journal_page_last               m2808
_journal_paper_doi               10.1107/S1600536807051616
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C4 H7 O S2)2 (C12 H12 N2)]'
_chemical_formula_moiety         'C20 H26 N2 Ni O2 S4'
_chemical_formula_sum            'C20 H26 N2 Ni O2 S4'
_chemical_formula_weight         513.38
_chemical_name_systematic
;
catena-Poly[[bis(O-isopropyl
dithiocarbonato-κ²S,S')nickel(II)]-μ-1,2-di-4-pyridylethane-κ²N:N']
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 104.256(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1460(6)
_cell_length_b                   15.8638(10)
_cell_length_c                   15.0545(9)
_cell_measurement_reflns_used    1905
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.9
_cell_volume                     2348.5(2)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku AFC12κ/SATURN724'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.017
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3974
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.19
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.19
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0265P)²+7.5757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.087
_refine_ls_wR_factor_ref         0.088
_reflns_number_gt                2243
_reflns_number_total             2348
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2592.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2215957
_cod_database_fobs_code          2215957
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Ni Ni 0.0000 0.25754(3) 0.2500 0.01712(13) Uani d S 1
S S1 0.11332(7) 0.24132(4) 0.12782(4) 0.02205(16) Uani d . 1
S S2 0.17407(7) 0.14873(4) 0.29958(4) 0.02095(16) Uani d . 1
O O2 0.31745(19) 0.13301(12) 0.18192(13) 0.0241(4) Uani d . 1
N N1 0.1411(2) 0.34583(13) 0.31920(14) 0.0193(4) Uani d . 1
C C1 0.2118(3) 0.17161(17) 0.19961(17) 0.0202(5) Uani d . 1
C C2 0.3651(3) 0.1563(2) 0.10060(19) 0.0287(6) Uani d . 1
H H2 0.2861 0.1678 0.0474 0.034 Uiso calc R 1
C C3 0.4532(3) 0.2335(2) 0.1236(2) 0.0348(7) Uani d . 1
H H3A 0.3977 0.2813 0.1341 0.052 Uiso calc R 1
H H3B 0.4940 0.2466 0.0726 0.052 Uiso calc R 1
H H3C 0.5253 0.2229 0.1791 0.052 Uiso calc R 1
C C4 0.4439(4) 0.0799(2) 0.0814(2) 0.0434(8) Uani d . 1
H H4A 0.3822 0.0317 0.0657 0.065 Uiso calc R 1
H H4B 0.5160 0.0665 0.1360 0.065 Uiso calc R 1
H H4C 0.4845 0.0923 0.0301 0.065 Uiso calc R 1
C C5 0.1958(3) 0.33574(17) 0.40860(17) 0.0204(5) Uani d . 1
H H5 0.1530 0.2978 0.4415 0.024 Uiso calc R 1
C C6 0.3101(3) 0.37706(18) 0.45547(18) 0.0234(6) Uani d . 1
H H6 0.3445 0.3676 0.5193 0.028 Uiso calc R 1
C C7 0.3758(3) 0.43277(17) 0.40978(19) 0.0241(6) Uani d . 1
C C8 0.3171(3) 0.44529(17) 0.31804(19) 0.0254(6) Uani d . 1
H H8 0.3566 0.4839 0.2838 0.031 Uiso calc R 1
C C9 0.2010(3) 0.40162(17) 0.27593(18) 0.0231(6) Uani d . 1
H H9 0.1617 0.4119 0.2128 0.028 Uiso calc R 1
C C10 0.5056(3) 0.4752(2) 0.4583(2) 0.0326(7) Uani d . 1
H H10A 0.5343 0.5138 0.4148 0.039 Uiso calc R 1
H H10B 0.5772 0.4319 0.4771 0.039 Uiso calc R 1
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'
Ni Ni 0.3393 1.1124 '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'
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
_geom_angle_publ_flag
N1 Ni N1 . 2 95.78(12) ?
N1 Ni S1 . . 93.15(6) ?
N1 Ni S1 2 . 95.06(6) ?
N1 Ni S1 . 2 95.06(6) ?
N1 Ni S1 2 2 93.15(6) ?
S1 Ni S1 . 2 167.74(4) ?
N1 Ni S2 . 2 168.04(6) ?
N1 Ni S2 2 2 88.07(6) ?
S1 Ni S2 . 2 97.80(2) ?
S1 Ni S2 2 2 73.38(2) ?
N1 Ni S2 . . 88.07(6) ?
N1 Ni S2 2 . 168.04(6) ?
S1 Ni S2 . . 73.38(2) y
S1 Ni S2 2 . 97.80(2) ?
S2 Ni S2 2 . 90.45(4) ?
C1 S1 Ni . . 84.25(9) ?
C1 S2 Ni . . 83.17(9) ?
C1 O2 C2 . . 120.1(2) ?
C9 N1 C5 . . 116.6(2) ?
C9 N1 Ni . . 122.77(18) ?
C5 N1 Ni . . 119.13(18) ?
O2 C1 S2 . . 117.2(2) ?
O2 C1 S1 . . 123.9(2) ?
S2 C1 S1 . . 118.98(16) ?
O2 C2 C3 . . 108.2(2) ?
O2 C2 C4 . . 104.7(2) ?
C3 C2 C4 . . 112.5(3) ?
O2 C2 H2 . . 110.4 ?
C3 C2 H2 . . 110.4 ?
C4 C2 H2 . . 110.4 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 H4A . . 109.5 ?
C2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N1 C5 C6 . . 123.6(2) ?
N1 C5 H5 . . 118.2 ?
C6 C5 H5 . . 118.2 ?
C5 C6 C7 . . 120.0(2) ?
C5 C6 H6 . . 120.0 ?
C7 C6 H6 . . 120.0 ?
C8 C7 C6 . . 116.6(2) ?
C8 C7 C10 . . 122.3(3) ?
C6 C7 C10 . . 121.1(3) ?
C7 C8 C9 . . 119.9(3) ?
C7 C8 H8 . . 120.1 ?
C9 C8 H8 . . 120.1 ?
N1 C9 C8 . . 123.4(2) ?
N1 C9 H9 . . 118.3 ?
C8 C9 H9 . . 118.3 ?
C7 C10 C10 . 5_666 113.7(3) ?
C7 C10 H10A . . 108.8 ?
C10 C10 H10A 5_666 . 108.8 ?
C7 C10 H10B . . 108.8 ?
C10 C10 H10B 5_666 . 108.8 ?
H10A C10 H10B . . 107.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N1 . 2.089(2) y
Ni N1 2 2.089(2) ?
Ni S1 . 2.4110(7) y
Ni S1 2 2.4110(7) ?
Ni S2 2 2.4509(7) ?
Ni S2 . 2.4509(7) y
S1 C1 . 1.690(3) ?
S2 C1 . 1.681(3) ?
O2 C1 . 1.318(3) ?
O2 C2 . 1.470(3) ?
N1 C9 . 1.331(3) ?
N1 C5 . 1.333(3) ?
C2 C3 . 1.505(4) ?
C2 C4 . 1.518(4) ?
C2 H2 . 1.0000 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C5 C6 . 1.367(4) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.387(4) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.377(4) ?
C7 C10 . 1.499(4) ?
C8 C9 . 1.379(4) ?
C8 H8 . 0.9500 ?
C9 H9 . 0.9500 ?
C10 C10 5_666 1.510(6) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 Ni S1 C1 . . 84.26(11)
N1 Ni S1 C1 2 . -179.65(11)
S1 Ni S1 C1 2 . -47.77(9)
S2 Ni S1 C1 2 . -90.91(9)
S2 Ni S1 C1 . . -2.78(9)
N1 Ni S2 C1 . . -91.07(11)
N1 Ni S2 C1 2 . 18.0(3)
S1 Ni S2 C1 . . 2.80(9)
S1 Ni S2 C1 2 . 174.09(9)
S2 Ni S2 C1 2 . 100.81(9)
N1 Ni N1 C9 2 . -61.03(19)
S1 Ni N1 C9 . . 34.4(2)
S1 Ni N1 C9 2 . -154.7(2)
S2 Ni N1 C9 2 . -169.4(2)
S2 Ni N1 C9 . . 107.6(2)
N1 Ni N1 C5 2 . 133.5(2)
S1 Ni N1 C5 . . -131.04(19)
S1 Ni N1 C5 2 . 39.9(2)
S2 Ni N1 C5 2 . 25.2(4)
S2 Ni N1 C5 . . -57.81(19)
C2 O2 C1 S2 . . -173.59(19)
C2 O2 C1 S1 . . 6.8(3)
Ni S2 C1 O2 . . 176.0(2)
Ni S2 C1 S1 . . -4.38(15)
Ni S1 C1 O2 . . -176.0(2)
Ni S1 C1 S2 . . 4.44(15)
C1 O2 C2 C3 . . 82.0(3)
C1 O2 C2 C4 . . -157.9(2)
C9 N1 C5 C6 . . -2.3(4)
Ni N1 C5 C6 . . 164.1(2)
N1 C5 C6 C7 . . -0.2(4)
C5 C6 C7 C8 . . 2.2(4)
C5 C6 C7 C10 . . -176.5(3)
C6 C7 C8 C9 . . -1.7(4)
C10 C7 C8 C9 . . 177.0(3)
C5 N1 C9 C8 . . 2.8(4)
Ni N1 C9 C8 . . -163.0(2)
C7 C8 C9 N1 . . -0.9(4)
C8 C7 C10 C10 . 5_666 124.9(4)
C6 C7 C10 C10 . 5_666 -56.5(5)
