#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:38:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180271 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/57/7115787.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_7115787
loop_
_publ_author_name
'Thomas B. Faust'
'Pavel M. Usov'
'Deanna M. D'Alessandro'
'Cameron J. Kepert'
_publ_section_title
;
 Highly unusual interpenetration isomers of electroactive nickel
 bis(dithiolene) coordination frameworks
;
_journal_name_full               Chem.Commun.
_journal_page_first              12772
_journal_paper_doi               10.1039/C4cc05438E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C34 H34 N6 Ni2 O2 S8 Zn, 2(C3 H7 N O)'
_chemical_formula_sum            'C40 H48 N8 Ni2 O4 S8 Zn'
_chemical_formula_weight         1144.13
_chemical_melting_point          ?
_chemical_name_common            '[Zn(Ni(pedt)2)2(dmf)].2dmf'
_chemical_name_systematic
; 
 ? 
;
_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                90.00
_cell_angle_beta                 107.269(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.350(2)
_cell_length_b                   22.346(2)
_cell_length_c                   15.4658(17)
_cell_measurement_temperature    150(2)
_cell_volume                     5065.8(10)
_computing_cell_refinement       'SAINT Ver. 7.60A  (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2009.3-0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.60A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius FR591 Kappa APEX II'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            143043
_diffrn_reflns_theta_full        35.15
_diffrn_reflns_theta_max         35.14
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.6932
_exptl_absorpt_correction_T_min  0.3643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2360
_exptl_crystal_recrystallization_method 'Direct from synthesis'
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         11255
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0355
_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)+(0.0402P)²+8.6728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                8975
_reflns_number_total             11255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05438e2.cif
_cod_data_source_block           cjk13tf20a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7115787
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_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 0.82307(10) 0.18866(7) 0.25847(11) 0.0225(3) Uani 1 1 d . . .
H1 H 0.8261 0.2194 0.3017 0.027 Uiso 1 1 calc R . .
C2 C 0.74480(10) 0.15390(7) 0.23130(11) 0.0224(3) Uani 1 1 d . . .
H2 H 0.6961 0.1608 0.2562 0.027 Uiso 1 1 calc R . .
C3 C 0.73799(9) 0.10859(6) 0.16694(10) 0.0184(2) Uani 1 1 d . . .
C4 C 0.81370(10) 0.10008(7) 0.13501(11) 0.0205(3) Uani 1 1 d . . .
H4 H 0.8128 0.0696 0.0920 0.025 Uiso 1 1 calc R . .
C5 C 0.88996(10) 0.13651(7) 0.16664(11) 0.0201(2) Uani 1 1 d . . .
H5 H 0.9408 0.1297 0.1449 0.024 Uiso 1 1 calc R . .
C6 C 0.65387(10) 0.07298(7) 0.13175(10) 0.0189(2) Uani 1 1 d . . .
C7 C 0.59417(10) 0.06152(7) 0.18027(10) 0.0210(3) Uani 1 1 d . . .
H7 H 0.6073 0.0762 0.2405 0.025 Uiso 1 1 calc R . .
C8 C 0.89625(10) 0.36764(7) 0.25240(11) 0.0223(3) Uani 1 1 d . . .
H8 H 0.9454 0.3755 0.3053 0.027 Uiso 1 1 calc R . .
C9 C 0.82971(10) 0.41127(7) 0.22266(11) 0.0226(3) Uani 1 1 d . . .
H9 H 0.8341 0.4480 0.2545 0.027 Uiso 1 1 calc R . .
C10 C 0.75580(10) 0.40065(7) 0.14498(10) 0.0194(2) Uani 1 1 d . . .
C11 C 0.75400(10) 0.34522(7) 0.10212(11) 0.0219(3) Uani 1 1 d . . .
H11 H 0.7049 0.3355 0.0501 0.026 Uiso 1 1 calc R . .
C12 C 0.82378(10) 0.30471(7) 0.13583(11) 0.0221(3) Uani 1 1 d . . .
H12 H 0.8217 0.2677 0.1050 0.026 Uiso 1 1 calc R . .
C13 C 0.68363(10) 0.44521(7) 0.10972(11) 0.0211(3) Uani 1 1 d . . .
C14 C 0.69607(12) 0.50521(8) 0.12505(14) 0.0298(4) Uani 1 1 d . . .
H14 H 0.7534 0.5195 0.1618 0.036 Uiso 1 1 calc R . .
C15 C 0.99645(17) 0.27816(11) 0.04467(16) 0.0321(4) Uani 0.821(3) 1 d PDU A 1
H15 H 0.9652 0.3151 0.0428 0.038 Uiso 0.821(3) 1 calc PR A 1
C16 C 1.0819(3) 0.21078(14) -0.0221(2) 0.0490(7) Uani 0.821(3) 1 d PU A 1
H16A H 1.0914 0.1904 0.0361 0.074 Uiso 0.821(3) 1 calc PR A 1
H16B H 1.1411 0.2203 -0.0305 0.074 Uiso 0.821(3) 1 calc PR A 1
H16C H 1.0475 0.1846 -0.0712 0.074 Uiso 0.821(3) 1 calc PR A 1
C17 C 1.0184(3) 0.3053(2) -0.0998(3) 0.0718(11) Uani 0.821(3) 1 d PU A 1
H17B H 0.9758 0.2868 -0.1533 0.108 Uiso 0.821(3) 1 calc PR A 1
H17C H 1.0774 0.3116 -0.1108 0.108 Uiso 0.821(3) 1 calc PR A 1
H17A H 0.9938 0.3438 -0.0877 0.108 Uiso 0.821(3) 1 calc PR A 1
C18 C 1.0225(8) 0.2299(5) 0.0570(8) 0.0345(10) Uani 0.179(3) 1 d PDU A 2
H18 H 1.0495 0.1915 0.0718 0.041 Uiso 0.179(3) 1 calc PR A 2
C19 C 0.9571(13) 0.3022(7) -0.0578(11) 0.057(2) Uani 0.179(3) 1 d PU A 2
H19A H 0.9862 0.3386 -0.0268 0.086 Uiso 0.179(3) 1 calc PR A 2
H19B H 0.8990 0.2958 -0.0452 0.086 Uiso 0.179(3) 1 calc PR A 2
H19C H 0.9462 0.3068 -0.1232 0.086 Uiso 0.179(3) 1 calc PR A 2
C20 C 1.0556(13) 0.2208(8) -0.0890(11) 0.0537(19) Uani 0.179(3) 1 d PU A 2
H20A H 1.0795 0.2502 -0.1231 0.081 Uiso 0.179(3) 1 calc PR A 2
H20B H 1.0086 0.1965 -0.1311 0.081 Uiso 0.179(3) 1 calc PR A 2
H20C H 1.1053 0.1948 -0.0547 0.081 Uiso 0.179(3) 1 calc PR A 2
C21 C 0.6544(3) 0.33442(14) 0.2905(3) 0.0695(8) Uani 1 1 d U . .
H21 H 0.6063 0.3423 0.2368 0.083 Uiso 1 1 calc R . .
C22 C 0.7625(3) 0.3730(2) 0.4272(3) 0.0851(9) Uani 1 1 d U . .
H22A H 0.7835 0.3313 0.4317 0.128 Uiso 1 1 calc R . .
H22B H 0.7435 0.3831 0.4805 0.128 Uiso 1 1 calc R . .
H22C H 0.8122 0.3995 0.4240 0.128 Uiso 1 1 calc R . .
C23 C 0.6473(3) 0.43954(15) 0.3274(3) 0.0770(10) Uani 1 1 d U . .
H23A H 0.5951 0.4387 0.2724 0.116 Uiso 1 1 calc R . .
H23B H 0.6937 0.4670 0.3186 0.116 Uiso 1 1 calc R . .
H23C H 0.6271 0.4532 0.3785 0.116 Uiso 1 1 calc R . .
N1 N 0.89516(8) 0.18091(6) 0.22656(9) 0.0189(2) Uani 1 1 d . A .
N2 N 0.89492(8) 0.31491(6) 0.21042(10) 0.0212(2) Uani 1 1 d . A .
N3 N 1.0303(2) 0.26636(13) -0.0228(2) 0.0376(5) Uani 0.821(3) 1 d PU A 1
N4 N 1.0157(14) 0.2520(7) -0.0260(14) 0.0415(11) Uani 0.179(3) 1 d PU A 2
N5 N 0.6855(2) 0.38027(11) 0.3459(2) 0.0645(6) Uani 1 1 d U . .
Ni1 Ni 0.5000 0.0000 0.0000 0.01744(6) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.5000 0.0000 0.02055(6) Uani 1 2 d S . .
O1 O 1.0023(3) 0.24494(12) 0.1096(2) 0.0270(4) Uani 0.821(3) 1 d PDU A 1
O2 O 0.9962(16) 0.2556(8) 0.1144(12) 0.0316(12) Uani 0.179(3) 1 d PDU A 2
O3 O 0.6825(3) 0.28297(12) 0.3028(3) 0.1065(12) Uani 1 1 d . . .
S1 S 0.62777(3) 0.04570(2) 0.02134(3) 0.02538(8) Uani 1 1 d . . .
S2 S 0.49613(3) 0.021259(19) 0.13449(3) 0.02259(8) Uani 1 1 d . . .
S3 S 0.57753(3) 0.420138(18) 0.04352(3) 0.02384(8) Uani 1 1 d . . .
S4 S 0.61007(3) 0.55518(2) 0.07913(4) 0.03351(11) Uani 1 1 d . . .
Zn1 Zn 1.0000 0.247666(10) 0.2500 0.01725(5) 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'
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'
Zn Zn 0.2839 1.4301 '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
N1 C1 C2 123.20(14) . .
C1 C2 C3 119.68(14) . .
C2 C3 C4 116.91(12) . .
C2 C3 C6 121.60(13) . .
C4 C3 C6 121.45(13) . .
C5 C4 C3 119.68(14) . .
N1 C5 C4 123.13(14) . .
C7 C6 C3 123.56(13) . .
C7 C6 S1 118.31(11) . .
C3 C6 S1 118.10(11) . .
C6 C7 S2 121.30(12) . .
N2 C8 C9 123.51(14) . .
C8 C9 C10 119.50(14) . .
C11 C10 C9 116.80(13) . .
C11 C10 C13 121.12(13) . .
C9 C10 C13 122.08(14) . .
C12 C11 C10 119.78(14) . .
N2 C12 C11 123.45(14) . .
C14 C13 C10 123.38(14) . .
C14 C13 S3 118.48(11) . .
C10 C13 S3 118.13(12) . .
C13 C14 S4 121.14(13) . .
O1 C15 N3 124.9(2) . .
O2 C18 N4 124.6(15) . .
O3 C21 N5 125.6(5) . .
C5 N1 C1 117.36(12) . .
C5 N1 Zn1 121.21(10) . .
C1 N1 Zn1 120.28(10) . .
C8 N2 C12 116.94(12) . .
C8 N2 Zn1 124.87(10) . .
C12 N2 Zn1 118.14(10) . .
C15 N3 C17 123.2(3) . .
C15 N3 C16 119.9(3) . .
C17 N3 C16 116.9(3) . .
C18 N4 C19 118.5(17) . .
C18 N4 C20 121.7(15) . .
C19 N4 C20 119.1(16) . .
C21 N5 C23 122.2(4) . .
C21 N5 C22 120.9(3) . .
C23 N5 C22 116.9(3) . .
S1 Ni1 S1 180.0 5_655 .
S1 Ni1 S2 88.137(15) 5_655 .
S1 Ni1 S2 91.862(16) . .
S1 Ni1 S2 91.862(15) 5_655 5_655
S1 Ni1 S2 88.140(15) . 5_655
S2 Ni1 S2 180.0 . 5_655
S3 Ni2 S3 180.000(12) . 5_665
S3 Ni2 S4 91.691(17) . .
S3 Ni2 S4 88.310(17) 5_665 .
S3 Ni2 S4 88.310(17) . 5_665
S3 Ni2 S4 91.690(17) 5_665 5_665
S4 Ni2 S4 180.0 . 5_665
C15 O1 Zn1 140.9(2) . .
C18 O2 Zn1 140.5(14) . .
C6 S1 Ni1 104.51(5) . .
C7 S2 Ni1 104.01(5) . .
C13 S3 Ni2 104.64(5) . .
C14 S4 Ni2 103.90(6) . .
O2 Zn1 O2 170.2(9) 2_755 .
O2 Zn1 N1 95.4(6) 2_755 2_755
O2 Zn1 N1 91.4(5) . 2_755
O2 Zn1 N1 91.4(5) 2_755 .
O2 Zn1 N1 95.4(6) . .
N1 Zn1 N1 91.86(7) 2_755 .
O2 Zn1 N2 81.9(5) 2_755 2_755
O2 Zn1 N2 91.2(6) . 2_755
N1 Zn1 N2 88.63(5) 2_755 2_755
N1 Zn1 N2 173.37(5) . 2_755
O2 Zn1 N2 91.2(6) 2_755 .
O2 Zn1 N2 82.0(5) . .
N1 Zn1 N2 173.37(5) 2_755 .
N1 Zn1 N2 88.64(5) . .
N2 Zn1 N2 91.64(7) 2_755 .
O2 Zn1 O1 175.9(5) 2_755 .
O2 Zn1 O1 6.9(5) . .
N1 Zn1 O1 85.16(9) 2_755 .
N1 Zn1 O1 92.61(11) . .
N2 Zn1 O1 94.02(11) 2_755 .
N2 Zn1 O1 88.21(9) . .
O2 Zn1 O1 6.9(5) 2_755 2_755
O2 Zn1 O1 175.9(5) . 2_755
N1 Zn1 O1 92.61(11) 2_755 2_755
N1 Zn1 O1 85.16(9) . 2_755
N2 Zn1 O1 88.21(9) 2_755 2_755
N2 Zn1 O1 94.02(11) . 2_755
O1 Zn1 O1 176.80(15) . 2_755
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.350(2) .
C1 C2 1.387(2) .
C2 C3 1.402(2) .
C3 C4 1.404(2) .
C3 C6 1.4763(19) .
C4 C5 1.3901(19) .
C5 N1 1.3437(19) .
C6 C7 1.370(2) .
C6 S1 1.7440(15) .
C7 S2 1.7155(15) .
C8 N2 1.343(2) .
C8 C9 1.388(2) .
C9 C10 1.406(2) .
C10 C11 1.401(2) .
C10 C13 1.469(2) .
C11 C12 1.381(2) .
C12 N2 1.3517(19) .
C13 C14 1.365(2) .
C13 S3 1.7392(16) .
C14 S4 1.7136(16) .
C15 O1 1.231(4) .
C15 N3 1.323(4) .
C16 N3 1.471(4) .
C17 N3 1.442(4) .
C18 O2 1.222(9) .
C18 N4 1.35(2) .
C19 N4 1.43(2) .
C20 N4 1.47(3) .
C21 O3 1.223(4) .
C21 N5 1.330(4) .
C22 N5 1.456(5) .
C23 N5 1.443(4) .
N1 Zn1 2.1448(12) .
N2 Zn1 2.1559(12) .
Ni1 S1 2.1479(4) 5_655
Ni1 S1 2.1479(4) .
Ni1 S2 2.1516(4) .
Ni1 S2 2.1516(4) 5_655
Ni2 S3 2.1397(4) .
Ni2 S3 2.1398(4) 5_665
Ni2 S4 2.1553(5) .
Ni2 S4 2.1553(5) 5_665
O1 Zn1 2.183(3) .
O2 Zn1 2.089(16) .
Zn1 O2 2.089(16) 2_755
Zn1 N1 2.1448(12) 2_755
Zn1 N2 2.1559(12) 2_755
Zn1 O1 2.183(3) 2_755
