#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/54/2225422.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_2225422
loop_
_publ_author_name
'Xie, Jiang-Bo'
_publ_section_title
;
 Poly[(dimethylformamide)(μ₄-2,2'-sulfanediyldibenzoato)nickel(II)]
;
_journal_coeditor_code           BG2334
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m368
_journal_paper_doi               10.1107/S1600536810007749
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C14 H8 O4 S) (C3 H7 N O)]'
_chemical_formula_moiety         'C34 H30 N2 Ni2 O10 S2'
_chemical_formula_sum            'C34 H30 N2 Ni2 O10 S2'
_chemical_formula_weight         808.12
_chemical_name_systematic
;
Poly[(dimethylformamide)(μ₄-2,2'-sulfanediyldibenzoato)nickel(II)]
;
_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                67.2410(10)
_cell_angle_beta                 79.0410(11)
_cell_angle_gamma                71.7960(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5196(2)
_cell_length_b                   10.5240(2)
_cell_length_c                   11.0138(3)
_cell_measurement_reflns_used    2701
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.34
_cell_measurement_theta_min      2.39
_cell_volume                     862.33(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11190
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.7940
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0362
_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)+(0.0295P)²+0.4000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                2553
_reflns_number_total             3350
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg2334.cif
_cod_data_source_block           I
_cod_original_cell_volume        862.33(3)
_cod_database_code               2225422
_cod_database_fobs_code          2225422
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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.37381(4) 0.57945(3) 0.55076(3) 0.03249(12) Uani d . 1 . .
S S1 -0.02998(9) 0.75102(9) 0.29878(7) 0.0481(2) Uani d . 1 . .
O O1 0.2572(2) 0.5904(2) 0.40641(19) 0.0499(5) Uani d . 1 . .
O O2 0.4743(3) 0.4593(2) 0.3200(2) 0.0551(6) Uani d . 1 . .
O O3 -0.3145(3) 0.5998(2) 0.33626(19) 0.0501(5) Uani d . 1 . .
O O4 -0.5286(2) 0.7322(2) 0.4242(2) 0.0521(5) Uani d . 1 . .
O O5 0.1675(3) 0.7125(2) 0.6255(2) 0.0547(6) Uani d . 1 . .
N N1 -0.1056(3) 0.8241(3) 0.6247(3) 0.0535(7) Uani d . 1 . .
C C1 0.3275(4) 0.5360(3) 0.3199(3) 0.0417(7) Uani d . 1 . .
C C2 0.2315(3) 0.5674(3) 0.2057(3) 0.0381(6) Uani d . 1 . .
C C3 0.3089(4) 0.5029(3) 0.1132(3) 0.0501(8) Uani d . 1 . .
H H3 0.4126 0.4380 0.1281 0.060 Uiso calc R 1 . .
C C4 0.2369(4) 0.5317(4) 0.0004(3) 0.0561(8) Uani d . 1 . .
H H4 0.2922 0.4894 -0.0614 0.067 Uiso calc R 1 . .
C C5 0.0810(4) 0.6248(3) -0.0189(3) 0.0553(8) Uani d . 1 . .
H H5 0.0308 0.6456 -0.0948 0.066 Uiso calc R 1 . .
C C6 -0.0010(4) 0.6872(3) 0.0722(3) 0.0494(8) Uani d . 1 . .
H H6 -0.1072 0.7477 0.0582 0.059 Uiso calc R 1 . .
C C7 0.0723(3) 0.6616(3) 0.1858(3) 0.0411(7) Uani d . 1 . .
C C8 -0.2076(4) 0.8749(3) 0.2161(3) 0.0429(7) Uani d . 1 . .
C C9 -0.1898(4) 1.0066(3) 0.1271(3) 0.0571(9) Uani d . 1 . .
H H9 -0.0855 1.0235 0.1077 0.069 Uiso calc R 1 . .
C C10 -0.3225(5) 1.1122(4) 0.0670(3) 0.0665(10) Uani d . 1 . .
H H10 -0.3077 1.1993 0.0069 0.080 Uiso calc R 1 . .
C C11 -0.4766(4) 1.0887(3) 0.0962(3) 0.0620(9) Uani d . 1 . .
H H11 -0.5668 1.1595 0.0550 0.074 Uiso calc R 1 . .
C C12 -0.4984(4) 0.9601(3) 0.1866(3) 0.0529(8) Uani d . 1 . .
H H12 -0.6039 0.9455 0.2069 0.063 Uiso calc R 1 . .
C C13 -0.3648(3) 0.8520(3) 0.2478(3) 0.0388(7) Uani d . 1 . .
C C14 -0.4029(4) 0.7160(3) 0.3450(3) 0.0399(7) Uani d . 1 . .
C C15 0.0244(4) 0.7207(3) 0.6097(3) 0.0472(7) Uani d . 1 . .
H H15 0.0070 0.6507 0.5859 0.057 Uiso calc R 1 . .
C C16 -0.2706(4) 0.8325(4) 0.5980(4) 0.0821(12) Uani d . 1 . .
H H16A -0.2647 0.7545 0.5709 0.123 Uiso calc R 1 . .
H H16B -0.3115 0.9213 0.5289 0.123 Uiso calc R 1 . .
H H16C -0.3440 0.8271 0.6765 0.123 Uiso calc R 1 . .
C C17 -0.0867(4) 0.9353(4) 0.6631(4) 0.0730(11) Uani d . 1 . .
H H17A 0.0279 0.9356 0.6498 0.110 Uiso calc R 1 . .
H H17B -0.1239 0.9177 0.7546 0.110 Uiso calc R 1 . .
H H17C -0.1515 1.0264 0.6103 0.110 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
O2 Ni1 O4 2_666 1_655 90.48(9) ?
O2 Ni1 O3 2_666 2_566 88.17(9) ?
O4 Ni1 O3 1_655 2_566 168.24(8) ?
O2 Ni1 O1 2_666 . 168.07(8) ?
O4 Ni1 O1 1_655 . 89.02(9) ?
O3 Ni1 O1 2_566 . 89.89(8) ?
O2 Ni1 O5 2_666 . 97.16(8) ?
O4 Ni1 O5 1_655 . 97.19(8) ?
O3 Ni1 O5 2_566 . 94.56(8) ?
O1 Ni1 O5 . . 94.73(8) ?
O2 Ni1 Ni1 2_666 2_666 84.58(6) ?
O4 Ni1 Ni1 1_655 2_666 81.54(6) ?
O3 Ni1 Ni1 2_566 2_666 86.70(6) ?
O1 Ni1 Ni1 . 2_666 83.56(6) ?
O5 Ni1 Ni1 . 2_666 177.88(6) ?
C7 S1 C8 . . 102.75(13) ?
C1 O1 Ni1 . . 123.11(19) ?
C1 O2 Ni1 . 2_666 123.63(19) ?
C14 O3 Ni1 . 2_566 119.78(18) ?
C14 O4 Ni1 . 1_455 125.92(19) ?
C15 O5 Ni1 . . 120.6(2) ?
C15 N1 C17 . . 120.9(3) ?
C15 N1 C16 . . 120.9(3) ?
C17 N1 C16 . . 118.2(3) ?
O2 C1 O1 . . 124.9(3) ?
O2 C1 C2 . . 117.1(3) ?
O1 C1 C2 . . 118.0(3) ?
C3 C2 C7 . . 119.1(3) ?
C3 C2 C1 . . 117.4(3) ?
C7 C2 C1 . . 123.5(3) ?
C4 C3 C2 . . 122.1(3) ?
C4 C3 H3 . . 118.9 ?
C2 C3 H3 . . 118.9 ?
C3 C4 C5 . . 118.5(3) ?
C3 C4 H4 . . 120.7 ?
C5 C4 H4 . . 120.7 ?
C6 C5 C4 . . 120.9(3) ?
C6 C5 H5 . . 119.6 ?
C4 C5 H5 . . 119.6 ?
C5 C6 C7 . . 121.2(3) ?
C5 C6 H6 . . 119.4 ?
C7 C6 H6 . . 119.4 ?
C6 C7 C2 . . 118.1(3) ?
C6 C7 S1 . . 120.9(2) ?
C2 C7 S1 . . 121.0(2) ?
C9 C8 C13 . . 118.9(3) ?
C9 C8 S1 . . 117.6(2) ?
C13 C8 S1 . . 123.1(2) ?
C10 C9 C8 . . 121.5(3) ?
C10 C9 H9 . . 119.2 ?
C8 C9 H9 . . 119.2 ?
C11 C10 C9 . . 119.6(3) ?
C11 C10 H10 . . 120.2 ?
C9 C10 H10 . . 120.2 ?
C10 C11 C12 . . 120.1(3) ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
C11 C12 C13 . . 120.9(3) ?
C11 C12 H12 . . 119.6 ?
C13 C12 H12 . . 119.6 ?
C8 C13 C12 . . 119.0(3) ?
C8 C13 C14 . . 124.6(3) ?
C12 C13 C14 . . 116.4(2) ?
O3 C14 O4 . . 126.0(3) ?
O3 C14 C13 . . 118.5(2) ?
O4 C14 C13 . . 115.4(3) ?
O5 C15 N1 . . 123.4(3) ?
O5 C15 H15 . . 118.3 ?
N1 C15 H15 . . 118.3 ?
N1 C16 H16A . . 109.5 ?
N1 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
N1 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N1 C17 H17A . . 109.5 ?
N1 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
N1 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
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
Ni1 O2 2_666 1.947(2) ?
Ni1 O4 1_655 1.9695(19) ?
Ni1 O3 2_566 1.9751(19) ?
Ni1 O1 . 1.9790(19) ?
Ni1 O5 . 2.129(2) ?
Ni1 Ni1 2_666 2.6374(6) ?
S1 C7 . 1.781(3) ?
S1 C8 . 1.786(3) ?
O1 C1 . 1.259(3) ?
O2 C1 . 1.258(3) ?
O3 C14 . 1.249(3) ?
O4 C14 . 1.258(3) ?
O5 C15 . 1.236(3) ?
N1 C15 . 1.325(4) ?
N1 C17 . 1.450(4) ?
N1 C16 . 1.460(4) ?
C1 C2 . 1.504(4) ?
C2 C3 . 1.391(4) ?
C2 C7 . 1.405(4) ?
C3 C4 . 1.375(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.379(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.373(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.400(4) ?
C6 H6 . 0.9300 ?
C8 C9 . 1.389(4) ?
C8 C13 . 1.390(4) ?
C9 C10 . 1.371(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.368(5) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.379(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.391(4) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.507(4) ?
C15 H15 . 0.9300 ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
