#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:37:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179119 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/81/4308187.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_4308187
loop_
_publ_author_name
'Cory A. Black'
'Lyall R. Hanton'
'Mark D. Spicer'
_publ_contact_author             'Hanton, Lyall R.'
_publ_contact_author_email       lhanton@alkali.otago.ac.nz
_publ_section_title
;
Probing Anion-π Interactions in 1-D Co(II), Ni(II), and Cd(II)
Coordination Polymers Containing Flexible Pyrazine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3669
_journal_page_last               3679
_journal_paper_doi               10.1021/ic070194k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C10 H10 N6 Ni O6 S'
_chemical_formula_sum            'C10 H10 N6 Ni O6 S'
_chemical_formula_weight         400.98
_chemical_name_common            'Compound 2 cbd'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.835(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8097(4)
_cell_length_b                   14.2323(10)
_cell_length_c                   11.2912(7)
_cell_measurement_reflns_used    4528
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.91
_cell_volume                     1413.98(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.040373
_diffrn_orient_matrix_UB_12      0.0593578
_diffrn_orient_matrix_UB_13      -0.0369972
_diffrn_orient_matrix_UB_21      0.0462741
_diffrn_orient_matrix_UB_22      0.0368998
_diffrn_orient_matrix_UB_23      0.0679675
_diffrn_orient_matrix_UB_31      0.0956302
_diffrn_orient_matrix_UB_32      0.0072043
_diffrn_orient_matrix_UB_33      -0.0432959
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8914
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0397
_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)+(0.0389P)²+1.4110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2019
_reflns_number_total             2491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070194ksi20070201_040954_3.cif
_cod_data_source_block           cbd
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.2085(4) 0.0925(3) 0.0808(3) 0.0321(8) Uani 1 1 d . . .
H1 H 0.2729 0.1379 0.0474 0.039 Uiso 1 1 calc R . .
C2 C 0.2108(4) 0.0013(3) 0.0398(3) 0.0337(9) Uani 1 1 d . . .
H2 H 0.2805 -0.0151 -0.0183 0.040 Uiso 1 1 calc R . .
C3 C 0.0283(4) -0.0386(3) 0.1642(3) 0.0318(8) Uani 1 1 d . . .
H3 H -0.0387 -0.0838 0.1947 0.038 Uiso 1 1 calc R . .
C4 C 0.0274(4) 0.0518(2) 0.2110(3) 0.0279(8) Uani 1 1 d . . .
C5 C -0.0698(4) 0.0757(3) 0.3124(3) 0.0302(8) Uani 1 1 d . . .
H5A H -0.0144 0.0580 0.3876 0.036 Uiso 1 1 calc R . .
H5B H -0.1637 0.0375 0.3055 0.036 Uiso 1 1 calc R . .
C6 C -0.2637(4) 0.2102(3) 0.1984(3) 0.0273(8) Uani 1 1 d . . .
H6A H -0.3147 0.1487 0.1864 0.033 Uiso 1 1 calc R . .
H6B H -0.3417 0.2557 0.2221 0.033 Uiso 1 1 calc R . .
C7 C -0.2061(4) 0.2413(2) 0.0823(3) 0.0254(8) Uani 1 1 d . . .
C8 C -0.0271(4) 0.3093(3) -0.0305(3) 0.0318(8) Uani 1 1 d . . .
H8 H 0.0710 0.3357 -0.0381 0.038 Uiso 1 1 calc R . .
C9 C -0.1266(4) 0.3058(3) -0.1284(3) 0.0321(8) Uani 1 1 d . . .
H9 H -0.0964 0.3318 -0.2011 0.039 Uiso 1 1 calc R . .
C10 C -0.3042(4) 0.2365(2) -0.0178(3) 0.0272(8) Uani 1 1 d . . .
H10 H -0.4027 0.2107 -0.0103 0.033 Uiso 1 1 calc R . .
N1 N 0.1176(3) 0.1186(2) 0.1669(2) 0.0262(6) Uani 1 1 d . . .
N2 N 0.1177(3) -0.0650(2) 0.0792(3) 0.0341(7) Uani 1 1 d . . .
N3 N -0.2650(3) 0.2669(2) -0.1242(2) 0.0249(6) Uani 1 1 d . . .
N4 N -0.0654(3) 0.2759(2) 0.0763(2) 0.0268(7) Uani 1 1 d . . .
N5 N -0.0416(3) 0.4415(2) 0.2879(3) 0.0328(7) Uani 1 1 d . . .
N6 N 0.3427(4) 0.3641(2) 0.1005(3) 0.0371(8) Uani 1 1 d . . .
Ni1 Ni 0.09169(5) 0.25826(3) 0.22213(4) 0.02515(16) Uani 1 1 d . . .
O51 O 0.0798(2) 0.39381(17) 0.2804(2) 0.0315(6) Uani 1 1 d . . .
O52 O -0.1673(3) 0.4027(2) 0.2773(3) 0.0472(7) Uani 1 1 d . . .
O53 O -0.0307(3) 0.5266(2) 0.3090(3) 0.0513(8) Uani 1 1 d . . .
O61 O 0.2876(3) 0.28788(17) 0.1354(2) 0.0303(6) Uani 1 1 d . . .
O62 O 0.2583(3) 0.4312(2) 0.0699(2) 0.0445(7) Uani 1 1 d . . .
O63 O 0.4824(3) 0.3692(2) 0.0924(2) 0.0401(7) Uani 1 1 d . . .
S1 S -0.12230(10) 0.19871(6) 0.32020(7) 0.0271(2) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 '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
N1 C1 C2 121.5(4) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
N2 C2 C1 122.2(3) . . ?
N2 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
N2 C3 C4 123.5(3) . . ?
N2 C3 H3 118.2 . . ?
C4 C3 H3 118.2 . . ?
N1 C4 C3 119.7(3) . . ?
N1 C4 C5 119.4(3) . . ?
C3 C4 C5 120.9(3) . . ?
C4 C5 S1 114.3(2) . . ?
C4 C5 H5A 108.7 . . ?
S1 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
S1 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C7 C6 S1 116.1(2) . . ?
C7 C6 H6A 108.3 . . ?
S1 C6 H6A 108.3 . . ?
C7 C6 H6B 108.3 . . ?
S1 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
N4 C7 C10 121.1(3) . . ?
N4 C7 C6 120.6(3) . . ?
C10 C7 C6 118.2(3) . . ?
N4 C8 C9 121.7(3) . . ?
N4 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
N3 C9 C8 122.0(3) . . ?
N3 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
N3 C10 C7 122.4(3) . . ?
N3 C10 H10 118.8 . . ?
C7 C10 H10 118.8 . . ?
C1 N1 C4 117.2(3) . . ?
C1 N1 Ni1 123.7(2) . . ?
C4 N1 Ni1 118.8(2) . . ?
C3 N2 C2 115.8(3) . . ?
C10 N3 C9 116.1(3) . . ?
C10 N3 Ni1 120.6(2) . 4_565 ?
C9 N3 Ni1 123.0(2) . 4_565 ?
C7 N4 C8 116.5(3) . . ?
C7 N4 Ni1 119.3(2) . . ?
C8 N4 Ni1 123.6(2) . . ?
O52 N5 O53 121.0(3) . . ?
O52 N5 O51 120.4(3) . . ?
O53 N5 O51 118.5(3) . . ?
O63 N6 O62 121.0(3) . . ?
O63 N6 O61 118.2(3) . . ?
O62 N6 O61 120.8(3) . . ?
O51 Ni1 O61 91.01(10) . . ?
O51 Ni1 N1 176.48(9) . . ?
O61 Ni1 N1 86.95(10) . . ?
O51 Ni1 N4 95.55(10) . . ?
O61 Ni1 N4 97.85(10) . . ?
N1 Ni1 N4 87.58(11) . . ?
O51 Ni1 N3 86.19(10) . 4_666 ?
O61 Ni1 N3 86.85(10) . 4_666 ?
N1 Ni1 N3 90.83(11) . 4_666 ?
N4 Ni1 N3 174.95(11) . 4_666 ?
O51 Ni1 S1 97.55(7) . . ?
O61 Ni1 S1 170.93(7) . . ?
N1 Ni1 S1 84.36(8) . . ?
N4 Ni1 S1 84.37(8) . . ?
N3 Ni1 S1 90.70(8) 4_666 . ?
N5 O51 Ni1 125.6(2) . . ?
N6 O61 Ni1 131.8(2) . . ?
C5 S1 C6 102.56(17) . . ?
C5 S1 Ni1 96.37(12) . . ?
C6 S1 Ni1 98.30(11) . . ?
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 N1 1.342(4) . ?
C1 C2 1.378(5) . ?
C1 H1 0.9500 . ?
C2 N2 1.341(5) . ?
C2 H2 0.9500 . ?
C3 N2 1.325(5) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.350(4) . ?
C4 C5 1.502(5) . ?
C5 S1 1.813(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.495(5) . ?
C6 S1 1.817(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.338(4) . ?
C7 C10 1.390(5) . ?
C8 N4 1.354(4) . ?
C8 C9 1.377(5) . ?
C8 H8 0.9500 . ?
C9 N3 1.343(4) . ?
C9 H9 0.9500 . ?
C10 N3 1.338(4) . ?
C10 H10 0.9500 . ?
N1 Ni1 2.100(3) . ?
N3 Ni1 2.125(3) 4_565 ?
N4 Ni1 2.113(3) . ?
N5 O52 1.237(4) . ?
N5 O53 1.238(4) . ?
N5 O51 1.273(4) . ?
N6 O63 1.241(4) . ?
N6 O62 1.249(4) . ?
N6 O61 1.259(4) . ?
Ni1 O51 2.043(2) . ?
Ni1 O61 2.070(2) . ?
Ni1 N3 2.125(3) 4_666 ?
Ni1 S1 2.3886(10) . ?
