#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:47:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179424 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/21/4332184.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332184
loop_
_publ_author_name
'Wang, Lei'
'Zhang, Bin'
'Zhang, Jingping'
_publ_section_title
;
 Preparation and Crystal Structure of Dual-Functional Precursor Complex
 Bis(acetylacetonato)nickel(II) with 4-Pyridyltetrathiafulvalene
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6860
_journal_page_last               6863
_journal_paper_doi               10.1021/ic060095r
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C32 H28 N2 Ni O4 S8'
_chemical_formula_weight         819.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 97.2040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3220(5)
_cell_length_b                   8.5055(5)
_cell_length_c                   28.6082(18)
_cell_measurement_temperature    293(2)
_cell_volume                     1767.58(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            9625
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.9558
_exptl_absorpt_correction_T_min  0.6287
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0429
_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)+(0.0740P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                2885
_reflns_number_total             3451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060095rsup1.cif
_cod_data_source_block           0207
_cod_database_code               4332184
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ni Ni 0.5000 0.0000 0.0000 0.03844(16) Uani 1 2 d S
O1 O 0.6868(2) 0.0878(2) 0.05162(6) 0.0452(4) Uani 1 1 d .
O2 O 0.3375(2) 0.18993(19) 0.00128(6) 0.0443(4) Uani 1 1 d .
S1 S 0.03696(11) -0.49747(9) 0.23226(3) 0.0616(2) Uani 1 1 d .
S2 S -0.14315(9) -0.26546(9) 0.16527(2) 0.0485(2) Uani 1 1 d .
S3 S -0.24462(10) -0.42374(9) 0.30605(3) 0.0574(2) Uani 1 1 d .
S4 S -0.45430(9) -0.20920(9) 0.23801(3) 0.0523(2) Uani 1 1 d .
N N 0.3559(3) -0.1080(2) 0.05060(7) 0.0411(5) Uani 1 1 d .
C1 C 0.8359(4) 0.2674(4) 0.10595(11) 0.0682(9) Uani 1 1 d .
H1A H 0.8465 0.1940 0.1317 0.068 Uiso 1 1 calc R
H1B H 0.8161 0.3711 0.1176 0.068 Uiso 1 1 calc R
H1C H 0.9471 0.2661 0.0914 0.068 Uiso 1 1 calc R
C2 C 0.6745(4) 0.2213(3) 0.06991(9) 0.0436(6) Uani 1 1 d .
C3 C 0.5274(4) 0.3257(3) 0.06026(10) 0.0548(7) Uani 1 1 d .
H3 H 0.5346 0.4189 0.0774 0.055 Uiso 1 1 calc R
C4 C 0.3711(4) 0.3054(3) 0.02776(9) 0.0430(6) Uani 1 1 d .
C5 C 0.2255(5) 0.4318(4) 0.02272(12) 0.0675(9) Uani 1 1 d .
H5A H 0.1155 0.3917 0.0049 0.067 Uiso 1 1 calc R
H5B H 0.2692 0.5207 0.0067 0.067 Uiso 1 1 calc R
H5C H 0.1991 0.4634 0.0534 0.067 Uiso 1 1 calc R
C6 C 0.1760(4) -0.0856(3) 0.05296(9) 0.0508(7) Uani 1 1 d .
H6 H 0.1121 -0.0192 0.0308 0.051 Uiso 1 1 calc R
C7 C 0.0799(3) -0.1538(3) 0.08570(9) 0.0471(6) Uani 1 1 d .
H7 H -0.0451 -0.1336 0.0853 0.047 Uiso 1 1 calc R
C8 C 0.1710(3) -0.2540(3) 0.11971(9) 0.0400(6) Uani 1 1 d .
C9 C 0.3587(3) -0.2776(3) 0.11706(8) 0.0428(6) Uani 1 1 d .
H9 H 0.4263 -0.3435 0.1387 0.043 Uiso 1 1 calc R
C10 C 0.4436(3) -0.2047(3) 0.08299(8) 0.0438(6) Uani 1 1 d .
H10 H 0.5684 -0.2233 0.0823 0.044 Uiso 1 1 calc R
C11 C 0.0812(3) -0.3254(3) 0.15693(9) 0.0413(6) Uani 1 1 d .
C12 C 0.1558(4) -0.4336(3) 0.18721(10) 0.0521(7) Uani 1 1 d .
H12 H 0.2714 -0.4746 0.1841 0.052 Uiso 1 1 calc R
C13 C -0.1436(3) -0.3639(3) 0.21950(9) 0.0431(6) Uani 1 1 d .
C14 C -0.2662(3) -0.3360(3) 0.24996(9) 0.0434(6) Uani 1 1 d .
C15 C -0.5304(5) -0.2341(4) 0.29261(11) 0.0652(9) Uani 1 1 d .
H15 H -0.6348 -0.1824 0.3001 0.065 Uiso 1 1 calc R
C16 C -0.4347(5) -0.3296(4) 0.32333(12) 0.0689(9) Uani 1 1 d .
H16 H -0.4688 -0.3452 0.3532 0.069 Uiso 1 1 calc R
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_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Ni O2 180.00(11) . 3_655
O2 Ni O1 92.15(7) . .
O2 Ni O1 87.85(7) 3_655 .
O2 Ni O1 87.85(7) . 3_655
O2 Ni O1 92.15(7) 3_655 3_655
O1 Ni O1 180.00(7) . 3_655
O2 Ni N 89.39(7) . .
O2 Ni N 90.61(7) 3_655 .
O1 Ni N 90.58(7) . .
O1 Ni N 89.42(7) 3_655 .
O2 Ni N 90.61(7) . 3_655
O2 Ni N 89.39(7) 3_655 3_655
O1 Ni N 89.42(7) . 3_655
O1 Ni N 90.58(7) 3_655 3_655
N Ni N 180.00(15) . 3_655
C2 O1 Ni 123.99(16) . .
C4 O2 Ni 124.91(16) . .
C12 S1 C13 94.50(13) . .
C13 S2 C11 94.94(12) . .
C16 S3 C14 94.63(15) . .
C15 S4 C14 94.73(15) . .
C6 N C10 116.1(2) . .
C6 N Ni 123.54(17) . .
C10 N Ni 120.33(16) . .
O1 C2 C3 125.8(2) . .
O1 C2 C1 115.1(2) . .
C3 C2 C1 119.0(2) . .
C4 C3 C2 127.0(2) . .
O2 C4 C3 126.0(2) . .
O2 C4 C5 114.8(2) . .
C3 C4 C5 119.2(2) . .
N C6 C7 124.5(2) . .
C6 C7 C8 119.5(2) . .
C7 C8 C9 115.8(2) . .
C7 C8 C11 123.0(2) . .
C9 C8 C11 121.2(2) . .
C10 C9 C8 120.7(2) . .
N C10 C9 123.3(2) . .
C12 C11 C8 125.4(2) . .
C12 C11 S2 115.1(2) . .
C8 C11 S2 119.53(18) . .
C11 C12 S1 119.8(2) . .
C14 C13 S1 121.8(2) . .
C14 C13 S2 124.0(2) . .
S1 C13 S2 114.07(15) . .
C13 C14 S4 123.6(2) . .
C13 C14 S3 121.6(2) . .
S4 C14 S3 114.74(15) . .
C16 C15 S4 117.9(3) . .
C15 C16 S3 118.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni O2 2.0094(16) .
Ni O2 2.0094(16) 3_655
Ni O1 2.0255(16) .
Ni O1 2.0255(16) 3_655
Ni N 2.106(2) .
Ni N 2.106(2) 3_655
O1 C2 1.258(3) .
O2 C4 1.246(3) .
S1 C12 1.730(3) .
S1 C13 1.746(3) .
S2 C13 1.763(3) .
S2 C11 1.765(2) .
S3 C16 1.731(3) .
S3 C14 1.759(3) .
S4 C15 1.736(3) .
S4 C14 1.749(3) .
N C6 1.341(3) .
N C10 1.341(3) .
C1 C2 1.519(4) .
C2 C3 1.397(4) .
C3 C4 1.392(4) .
C4 C5 1.508(4) .
C6 C7 1.369(4) .
C7 C8 1.398(3) .
C8 C9 1.400(3) .
C8 C11 1.453(4) .
C9 C10 1.368(3) .
C11 C12 1.333(4) .
C13 C14 1.348(4) .
C15 C16 1.330(5) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5B C3 0.96 2.88 3.774(5) 154.9 3_665
C10 H10 S2 0.93 3.00 3.630(3) 126.8 1_655
C16 H16 C2 0.93 2.87 3.734(4) 154.5 2_545
