#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035242.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_7035242
loop_
_publ_author_name
'Hilbert, J.'
'Näther, C'
'Bensch, W.'
_publ_section_title
;
 Utilization of mixtures of aromatic N-donor ligands of different
 coordination ability for the solvothermal synthesis of thiostannate
 containing molecules.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11542
_journal_page_last               11550
_journal_paper_doi               10.1039/c5dt01145k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'Sn2S6, Ni2C48H32N8, c10H8N2, H2O'
_chemical_formula_sum            'C58 H42 N10 Ni2 O S6 Sn2'
_chemical_formula_weight         1442.18
_chemical_name_common            '[Ni(phen)2]2Sn2S6*4,4'-bipy*1/2H2O'
_chemical_name_systematic
;
{[Ni(C12H8N2)2]2Sn2S6*C10H8N2*1/2H2O
;
_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
_audit_update_record
;
2015-03-17 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.556(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3431(6)
_cell_length_b                   19.4475(6)
_cell_length_c                   15.0835(5)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.53
_cell_volume                     5355.4(3)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ scans'
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31723
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.903
_exptl_absorpt_correction_T_max  0.7793
_exptl_absorpt_correction_T_min  0.6810
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00052(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0466
_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)+(0.0525P)²+10.8420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                5042
_reflns_number_total             6419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01145k2.cif
_cod_data_source_block           jh483
_cod_depositor_comments
'Adding full bibliography for 7035242--7035243.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7035242
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
Sn1 Sn 0.5000 0.157531(16) 0.2500 0.02958(11) Uani 1 2 d S
Sn2 Sn 0.5000 0.332272(16) 0.2500 0.03130(12) Uani 1 2 d S
S1 S 0.44192(5) 0.08073(5) 0.14682(7) 0.0346(2) Uani 1 1 d .
S2 S 0.41963(5) 0.24454(4) 0.30691(7) 0.0354(2) Uani 1 1 d .
S3 S 0.44765(5) 0.40841(5) 0.14212(7) 0.0355(2) Uani 1 1 d .
Ni1 Ni 0.5000 -0.00824(3) 0.2500 0.03015(16) Uani 1 2 d S
Ni2 Ni 0.5000 0.49756(3) 0.2500 0.03148(17) Uani 1 2 d S
N1 N 0.40819(17) -0.02171(15) 0.3216(2) 0.0341(7) Uani 1 1 d .
N2 N 0.43951(18) -0.08277(15) 0.1708(2) 0.0336(7) Uani 1 1 d .
C1 C 0.4550(2) -0.11132(19) 0.0951(3) 0.0399(9) Uani 1 1 d .
H1 H 0.5013 -0.1020 0.0745 0.048 Uiso 1 1 calc R
C2 C 0.4061(3) -0.1550(2) 0.0438(3) 0.0457(10) Uani 1 1 d .
H2 H 0.4190 -0.1743 -0.0104 0.055 Uiso 1 1 calc R
C3 C 0.3400(3) -0.1688(2) 0.0737(4) 0.0485(11) Uani 1 1 d .
H3 H 0.3062 -0.1978 0.0399 0.058 Uiso 1 1 calc R
C4 C 0.3213(2) -0.1405(2) 0.1543(3) 0.0427(9) Uani 1 1 d .
C5 C 0.2535(3) -0.1538(2) 0.1915(4) 0.0508(11) Uani 1 1 d .
H5 H 0.2182 -0.1831 0.1606 0.061 Uiso 1 1 calc R
C6 C 0.2390(2) -0.1253(2) 0.2696(4) 0.0501(11) Uani 1 1 d .
H6 H 0.1939 -0.1350 0.2930 0.060 Uiso 1 1 calc R
C7 C 0.2910(2) -0.0806(2) 0.3175(3) 0.0420(10) Uani 1 1 d .
C8 C 0.2797(2) -0.0504(2) 0.3993(3) 0.0468(10) Uani 1 1 d .
H8 H 0.2361 -0.0597 0.4265 0.056 Uiso 1 1 calc R
C9 C 0.3317(3) -0.0076(2) 0.4399(3) 0.0476(11) Uani 1 1 d .
H9 H 0.3248 0.0127 0.4958 0.057 Uiso 1 1 calc R
C10 C 0.3952(2) 0.0064(2) 0.3986(3) 0.0396(9) Uani 1 1 d .
H10 H 0.4304 0.0371 0.4269 0.047 Uiso 1 1 calc R
C11 C 0.3572(2) -0.06569(18) 0.2819(3) 0.0335(8) Uani 1 1 d .
C12 C 0.3734(2) -0.09705(18) 0.2004(3) 0.0345(8) Uani 1 1 d .
N21 N 0.59902(17) 0.51048(15) 0.1951(2) 0.0338(7) Uani 1 1 d .
N22 N 0.55166(18) 0.57240(15) 0.3373(2) 0.0347(7) Uani 1 1 d .
C21 C 0.6197(2) 0.4823(2) 0.1219(3) 0.0417(9) Uani 1 1 d .
H21 H 0.5870 0.4520 0.0886 0.050 Uiso 1 1 calc R
C22 C 0.6883(2) 0.4956(2) 0.0915(3) 0.0476(11) Uani 1 1 d .
H22 H 0.7010 0.4751 0.0380 0.057 Uiso 1 1 calc R
C23 C 0.7367(2) 0.5381(2) 0.1391(3) 0.0449(10) Uani 1 1 d .
H23 H 0.7835 0.5469 0.1194 0.054 Uiso 1 1 calc R
C24 C 0.7165(2) 0.5687(2) 0.2175(3) 0.0399(9) Uani 1 1 d .
C25 C 0.7627(2) 0.6138(2) 0.2717(3) 0.0471(10) Uani 1 1 d .
H25 H 0.8103 0.6238 0.2553 0.057 Uiso 1 1 calc R
C26 C 0.7405(3) 0.6430(2) 0.3461(3) 0.0498(11) Uani 1 1 d .
H26 H 0.7729 0.6724 0.3815 0.060 Uiso 1 1 calc R
C27 C 0.6685(2) 0.6300(2) 0.3720(3) 0.0410(9) Uani 1 1 d .
C28 C 0.6403(3) 0.6592(2) 0.4473(3) 0.0472(11) Uani 1 1 d .
H28 H 0.6703 0.6883 0.4861 0.057 Uiso 1 1 calc R
C29 C 0.5701(3) 0.6458(2) 0.4645(3) 0.0443(10) Uani 1 1 d .
H29 H 0.5506 0.6659 0.5145 0.053 Uiso 1 1 calc R
C30 C 0.5272(2) 0.6021(2) 0.4074(3) 0.0391(9) Uani 1 1 d .
H30 H 0.4782 0.5933 0.4196 0.047 Uiso 1 1 calc R
C31 C 0.6214(2) 0.58605(18) 0.3195(3) 0.0337(8) Uani 1 1 d .
C32 C 0.6462(2) 0.55396(18) 0.2423(3) 0.0341(8) Uani 1 1 d .
C41 C 0.2148(2) 0.2504(2) 0.0209(3) 0.0430(9) Uani 1 1 d .
C42 C 0.1496(3) 0.2667(4) -0.0261(4) 0.083(2) Uani 1 1 d .
H42 H 0.1478 0.2779 -0.0875 0.100 Uiso 1 1 calc R
C43 C 0.0860(3) 0.2668(4) 0.0166(4) 0.087(2) Uani 1 1 d .
H43 H 0.0413 0.2773 -0.0180 0.104 Uiso 1 1 calc R
N41 N 0.0831(3) 0.2532(2) 0.1018(3) 0.0632(12) Uani 1 1 d .
C44 C 0.1459(3) 0.2374(3) 0.1465(4) 0.0628(13) Uani 1 1 d .
H44 H 0.1458 0.2269 0.2080 0.075 Uiso 1 1 calc R
C45 C 0.2121(3) 0.2350(3) 0.1099(3) 0.0551(12) Uani 1 1 d .
H45 H 0.2556 0.2228 0.1458 0.066 Uiso 1 1 calc R
O1 O 0.0262(6) 0.2339(6) 0.2718(8) 0.121(5) Uani 0.50 1 d P
H2O1 H 0.0265 0.2424 0.3292 0.181 Uiso 0.50 1 d PR
H1O1 H 0.0119 0.2722 0.2442 0.181 Uiso 0.50 1 d PR
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'
Ni Ni 0.3393 1.1124 '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'
Sn Sn -0.6537 1.4246 '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
S1 Sn1 S1 100.59(5) . 2_655
S1 Sn1 S2 117.27(4) . 2_655
S1 Sn1 S2 115.02(3) 2_655 2_655
S1 Sn1 S2 115.02(3) . .
S1 Sn1 S2 117.28(4) 2_655 .
S2 Sn1 S2 92.78(4) 2_655 .
S3 Sn2 S3 101.36(5) 2_655 .
S3 Sn2 S2 114.57(3) 2_655 .
S3 Sn2 S2 117.52(3) . .
S3 Sn2 S2 117.53(3) 2_655 2_655
S3 Sn2 S2 114.57(3) . 2_655
S2 Sn2 S2 92.30(4) . 2_655
Sn1 S1 Ni1 83.59(4) . .
Sn1 S2 Sn2 87.46(3) . .
Sn2 S3 Ni2 83.13(4) . .
N1 Ni1 N1 165.69(17) 2_655 .
N1 Ni1 N2 91.54(13) 2_655 .
N1 Ni1 N2 78.64(13) . .
N1 Ni1 N2 78.64(13) 2_655 2_655
N1 Ni1 N2 91.54(13) . 2_655
N2 Ni1 N2 93.84(18) . 2_655
N1 Ni1 S1 95.27(9) 2_655 2_655
N1 Ni1 S1 94.64(9) . 2_655
N2 Ni1 S1 173.19(9) . 2_655
N2 Ni1 S1 87.36(9) 2_655 2_655
N1 Ni1 S1 94.64(9) 2_655 .
N1 Ni1 S1 95.27(9) . .
N2 Ni1 S1 87.36(9) . .
N2 Ni1 S1 173.19(9) 2_655 .
S1 Ni1 S1 92.23(5) 2_655 .
N21 Ni2 N21 166.14(17) 2_655 .
N21 Ni2 N22 91.43(13) 2_655 .
N21 Ni2 N22 79.03(13) . .
N21 Ni2 N22 79.03(13) 2_655 2_655
N21 Ni2 N22 91.43(13) . 2_655
N22 Ni2 N22 93.47(18) . 2_655
N21 Ni2 S3 92.71(10) 2_655 .
N21 Ni2 S3 96.87(10) . .
N22 Ni2 S3 175.86(9) . .
N22 Ni2 S3 87.22(9) 2_655 .
N21 Ni2 S3 96.87(10) 2_655 2_655
N21 Ni2 S3 92.71(9) . 2_655
N22 Ni2 S3 87.22(9) . 2_655
N22 Ni2 S3 175.86(9) 2_655 2_655
S3 Ni2 S3 92.39(5) . 2_655
C10 N1 C11 118.0(3) . .
C10 N1 Ni1 128.2(3) . .
C11 N1 Ni1 113.7(3) . .
C1 N2 C12 118.0(3) . .
C1 N2 Ni1 128.8(3) . .
C12 N2 Ni1 112.9(3) . .
N2 C1 C2 123.1(4) . .
C3 C2 C1 118.5(4) . .
C2 C3 C4 120.6(4) . .
C3 C4 C12 116.7(4) . .
C3 C4 C5 124.1(4) . .
C12 C4 C5 119.2(4) . .
C6 C5 C4 121.1(4) . .
C5 C6 C7 120.8(4) . .
C8 C7 C11 117.2(4) . .
C8 C7 C6 123.4(4) . .
C11 C7 C6 119.3(4) . .
C9 C8 C7 119.6(4) . .
C8 C9 C10 119.6(4) . .
N1 C10 C9 122.5(4) . .
N1 C11 C7 123.0(4) . .
N1 C11 C12 117.0(3) . .
C7 C11 C12 120.0(4) . .
N2 C12 C4 123.0(4) . .
N2 C12 C11 117.5(3) . .
C4 C12 C11 119.5(4) . .
C21 N21 C32 118.3(3) . .
C21 N21 Ni2 127.9(3) . .
C32 N21 Ni2 113.8(3) . .
C30 N22 C31 118.2(4) . .
C30 N22 Ni2 129.1(3) . .
C31 N22 Ni2 112.5(3) . .
N21 C21 C22 122.4(4) . .
C23 C22 C21 119.9(4) . .
C22 C23 C24 119.2(4) . .
C23 C24 C32 117.4(4) . .
C23 C24 C25 123.7(4) . .
C32 C24 C25 118.9(4) . .
C26 C25 C24 121.7(4) . .
C25 C26 C27 120.6(4) . .
C31 C27 C28 116.4(4) . .
C31 C27 C26 119.1(4) . .
C28 C27 C26 124.4(4) . .
C29 C28 C27 120.1(4) . .
C28 C29 C30 119.0(4) . .
N22 C30 C29 123.0(4) . .
N22 C31 C27 123.2(4) . .
N22 C31 C32 117.1(3) . .
C27 C31 C32 119.7(4) . .
N21 C32 C24 122.8(4) . .
N21 C32 C31 117.3(3) . .
C24 C32 C31 119.9(4) . .
C42 C41 C45 116.2(4) . .
C42 C41 C41 122.3(5) . 7
C45 C41 C41 121.5(5) . 7
C41 C42 C43 119.6(5) . .
N41 C43 C42 124.6(6) . .
C44 N41 C43 115.6(5) . .
N41 C44 C45 124.3(5) . .
C41 C45 C44 119.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.3382(10) .
Sn1 S1 2.3382(10) 2_655
Sn1 S2 2.4532(9) 2_655
Sn1 S2 2.4532(9) .
Sn2 S3 2.3366(10) 2_655
Sn2 S3 2.3366(10) .
Sn2 S2 2.4630(9) .
Sn2 S2 2.4630(9) 2_655
S1 Ni1 2.4960(11) .
S3 Ni2 2.5047(11) .
Ni1 N1 2.103(3) 2_655
Ni1 N1 2.103(3) .
Ni1 N2 2.122(3) .
Ni1 N2 2.122(3) 2_655
Ni1 S1 2.4960(11) 2_655
Ni2 N21 2.083(3) 2_655
Ni2 N21 2.083(3) .
Ni2 N22 2.124(3) .
Ni2 N22 2.124(3) 2_655
Ni2 S3 2.5047(11) 2_655
N1 C10 1.326(5) .
N1 C11 1.363(5) .
N2 C1 1.324(5) .
N2 C12 1.361(5) .
C1 C2 1.411(6) .
C2 C3 1.360(7) .
C3 C4 1.407(7) .
C4 C12 1.408(6) .
C4 C5 1.436(6) .
C5 C6 1.351(7) .
C6 C7 1.433(6) .
C7 C8 1.400(7) .
C7 C11 1.404(5) .
C8 C9 1.367(7) .
C9 C10 1.400(6) .
C11 C12 1.430(6) .
N21 C21 1.321(5) .
N21 C32 1.360(5) .
N22 C30 1.321(5) .
N22 C31 1.358(5) .
C21 C22 1.404(6) .
C22 C23 1.365(7) .
C23 C24 1.406(6) .
C24 C32 1.406(5) .
C24 C25 1.422(6) .
C25 C26 1.355(7) .
C26 C27 1.436(6) .
C27 C31 1.404(6) .
C27 C28 1.413(6) .
C28 C29 1.363(7) .
C29 C30 1.397(6) .
C31 C32 1.434(6) .
C41 C42 1.368(7) .
C41 C45 1.380(7) .
C41 C41 1.490(9) 7
C42 C43 1.386(8) .
C43 N41 1.317(8) .
N41 C44 1.313(7) .
C44 C45 1.383(7) .
O1 O1 1.11(2) 2
