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#$Date: 2019-11-23 08:05:57 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232508 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/78/4347801.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_4347801
loop_
_publ_author_name
'Hilbert, Jessica'
'Näther, Christian'
'Weihrich, Richard'
'Bensch, Wolfgang'
_publ_section_title
;
 Room-Temperature Synthesis of Thiostannates from {[Ni(tren)]2[Sn2S6]}n.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7859
_journal_page_last               7865
_journal_paper_doi               10.1021/acs.inorgchem.6b00625
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'Sn2S6, 2NiC9H28N6, 2H2O'
_chemical_formula_sum            'C18 H60 N12 Ni2 O2 S6 Sn2'
_chemical_formula_weight         1023.94
_chemical_name_common            '[Ni(tren)(1,2-dap)]2[Sn2S6]*2H2O'
_chemical_name_systematic
;
 '[Ni(C6H18N4)(C3H10N2)]2[Sn2S6]*2H2O'
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 113.263(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9264(3)
_cell_length_b                   10.1627(3)
_cell_length_c                   15.6585(4)
_cell_measurement_reflns_used    4120
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      1.74
_cell_volume                     1889.78(9)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean '\f scans'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'Stoe Imaging Plate Diffraction System'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26578
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.005
_diffrn_reflns_theta_min         1.740
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  0.7825
_exptl_absorpt_correction_T_min  0.4488
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0390P)²+0.1858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3712
_reflns_number_total             4120
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00625_si_004.cif
_cod_data_source_block           jh1538
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347801
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.12227(2) 0.56526(2) 0.50126(2) 0.02261(6) Uani 1 1 d . . . . .
S1 S 0.21625(5) 0.46317(8) 0.41897(5) 0.03877(16) Uani 1 1 d . . . . .
S2 S 0.21737(5) 0.74666(6) 0.58912(4) 0.03058(14) Uani 1 1 d . . . . .
S3 S 0.07769(5) 0.40541(6) 0.59896(4) 0.02957(14) Uani 1 1 d . . . . .
Ni1 Ni 0.46868(2) 0.35154(3) 0.73560(2) 0.02258(8) Uani 1 1 d . . . . .
N1 N 0.58899(16) 0.50110(19) 0.79908(13) 0.0257(4) Uani 1 1 d . . . . .
C1 C 0.6777(2) 0.4356(3) 0.87839(18) 0.0333(6) Uani 1 1 d . . . . .
H1A H 0.7324 0.5017 0.9170 0.040 Uiso 1 1 calc R U . . .
H1B H 0.7186 0.3719 0.8553 0.040 Uiso 1 1 calc R U . . .
C2 C 0.6252(2) 0.3645(3) 0.93645(17) 0.0365(6) Uani 1 1 d . . . . .
H2A H 0.6818 0.3058 0.9816 0.044 Uiso 1 1 calc R U . . .
H2B H 0.6007 0.4293 0.9718 0.044 Uiso 1 1 calc R U . . .
N2 N 0.52773(17) 0.2862(2) 0.87604(14) 0.0296(4) Uani 1 1 d . . . . .
H1N H 0.4713 0.2931 0.8967 0.035 Uiso 1 1 calc R U . . .
H2N H 0.5478 0.1999 0.8790 0.035 Uiso 1 1 calc R U . . .
C3 C 0.5351(2) 0.6103(3) 0.82985(19) 0.0332(5) Uani 1 1 d . . . . .
H3A H 0.5190 0.6839 0.7850 0.040 Uiso 1 1 calc R U . . .
H3B H 0.5883 0.6428 0.8911 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4260(2) 0.5683(3) 0.8376(2) 0.0353(6) Uani 1 1 d . . . . .
H4A H 0.4431 0.5147 0.8944 0.042 Uiso 1 1 calc R U . . .
H4B H 0.3832 0.6469 0.8421 0.042 Uiso 1 1 calc R U . . .
N3 N 0.35805(17) 0.4906(2) 0.75477(15) 0.0321(5) Uani 1 1 d . . . . .
H3N H 0.3282 0.5437 0.7041 0.038 Uiso 1 1 calc R U . . .
H4N H 0.3008 0.4491 0.7638 0.038 Uiso 1 1 calc R U . . .
C5 C 0.6289(2) 0.5474(3) 0.72808(19) 0.0347(6) Uani 1 1 d . . . . .
H5A H 0.6825 0.4829 0.7213 0.042 Uiso 1 1 calc R U . . .
H5B H 0.6684 0.6325 0.7476 0.042 Uiso 1 1 calc R U . . .
C6 C 0.5291(2) 0.5638(3) 0.63577(19) 0.0380(6) Uani 1 1 d . . . . .
H6A H 0.4793 0.6347 0.6408 0.046 Uiso 1 1 calc R U . . .
H6B H 0.5559 0.5885 0.5868 0.046 Uiso 1 1 calc R U . . .
N4 N 0.46594(19) 0.4388(2) 0.61077(15) 0.0334(5) Uani 1 1 d . . . . .
H5N H 0.4984 0.3838 0.5827 0.040 Uiso 1 1 calc R U . . .
H6N H 0.3937 0.4542 0.5707 0.040 Uiso 1 1 calc R U . . .
N11 N 0.56147(16) 0.1895(2) 0.70968(14) 0.0286(4) Uani 1 1 d . . . . .
H7N H 0.6104 0.2193 0.6853 0.034 Uiso 0.62 1 calc R U P A 1
H8N H 0.6009 0.1452 0.7632 0.034 Uiso 0.62 1 calc R U P A 1
H9N H 0.5766 0.2073 0.6588 0.034 Uiso 0.38 1 calc R U P B 2
H10N H 0.6281 0.1787 0.7593 0.034 Uiso 0.38 1 calc R U P B 2
C11 C 0.4728(4) 0.1015(4) 0.6409(4) 0.0319(9) Uani 0.62 1 d . . P C 1
H11 H 0.4427 0.1423 0.5776 0.038 Uiso 0.62 1 calc R U P C 1
C12 C 0.3795(4) 0.0844(5) 0.6756(4) 0.0348(11) Uani 0.62 1 d . . P C 1
H12A H 0.3176 0.0314 0.6308 0.042 Uiso 0.62 1 calc R U P C 1
H12B H 0.4086 0.0381 0.7362 0.042 Uiso 0.62 1 calc R U P C 1
C11' C 0.4929(6) 0.0668(6) 0.6939(6) 0.0295(13) Uani 0.38 1 d . . P C 2
H11' H 0.4945 0.0297 0.7536 0.035 Uiso 0.38 1 calc R U P C 2
C12' C 0.3767(7) 0.1091(9) 0.6310(7) 0.0347(18) Uani 0.38 1 d . . P C 2
H12C H 0.3248 0.0329 0.6141 0.042 Uiso 0.38 1 calc R U P C 2
H12D H 0.3774 0.1482 0.5732 0.042 Uiso 0.38 1 calc R U P C 2
N12 N 0.33833(18) 0.2136(2) 0.68594(18) 0.0387(5) Uani 1 1 d . . . . .
H11N H 0.3032 0.2085 0.7261 0.046 Uiso 0.62 1 calc R U P C 1
H12N H 0.2868 0.2409 0.6299 0.046 Uiso 0.62 1 calc R U P C 1
H13N H 0.3270 0.1749 0.7340 0.046 Uiso 0.38 1 calc R U P C 2
H14N H 0.2731 0.2529 0.6479 0.046 Uiso 0.38 1 calc R U P C 2
C13 C 0.5272(3) -0.0356(3) 0.6385(3) 0.0584(9) Uani 1 1 d . . . . .
H13A H 0.4706 -0.0934 0.5942 0.088 Uiso 0.62 1 calc R U P C 1
H13B H 0.5901 -0.0239 0.6193 0.088 Uiso 0.62 1 calc R U P C 1
H13C H 0.5548 -0.0752 0.7006 0.088 Uiso 0.62 1 calc R U P C 1
H13D H 0.4803 -0.1143 0.6298 0.088 Uiso 0.38 1 calc R U P C 2
H13E H 0.5167 0.0010 0.5778 0.088 Uiso 0.38 1 calc R U P C 2
H13F H 0.6065 -0.0591 0.6726 0.088 Uiso 0.38 1 calc R U P C 2
O1 O 0.65416(19) 0.2665(2) 0.56698(16) 0.0508(5) Uani 1 1 d . . . . .
H1O1 H 0.6911 0.3369 0.5774 0.076 Uiso 1 1 d R U . . .
H2O1 H 0.6746 0.2424 0.5247 0.076 Uiso 1 1 d R U . . .
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'
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_3
S1 Sn1 S2 114.08(2) .
S1 Sn1 S3 110.60(3) .
S2 Sn1 S3 110.72(2) .
S1 Sn1 S3 110.31(2) 3_566
S2 Sn1 S3 117.16(2) 3_566
S3 Sn1 S3 91.81(2) 3_566
Sn1 S3 Sn1 88.185(19) 3_566
N12 Ni1 N3 90.58(9) .
N12 Ni1 N1 171.43(9) .
N3 Ni1 N1 82.31(8) .
N12 Ni1 N2 94.73(9) .
N3 Ni1 N2 92.78(8) .
N1 Ni1 N2 80.91(8) .
N12 Ni1 N4 102.62(10) .
N3 Ni1 N4 94.87(9) .
N1 Ni1 N4 82.84(8) .
N2 Ni1 N4 160.93(8) .
N12 Ni1 N11 81.11(8) .
N3 Ni1 N11 171.68(8) .
N1 Ni1 N11 105.94(7) .
N2 Ni1 N11 87.55(8) .
N4 Ni1 N11 87.38(8) .
C5 N1 C1 113.0(2) .
C5 N1 C3 110.7(2) .
C1 N1 C3 111.8(2) .
C5 N1 Ni1 106.56(15) .
C1 N1 Ni1 104.68(15) .
C3 N1 Ni1 109.63(15) .
N1 C1 C2 109.7(2) .
N2 C2 C1 110.1(2) .
C2 N2 Ni1 111.17(15) .
N1 C3 C4 112.5(2) .
N3 C4 C3 109.2(2) .
C4 N3 Ni1 106.35(15) .
N1 C5 C6 109.5(2) .
N4 C6 C5 109.3(2) .
C6 N4 Ni1 107.89(16) .
C11' N11 Ni1 109.2(3) .
C11 N11 Ni1 105.22(19) .
N11 C11 C12 107.3(4) .
N11 C11 C13 108.8(3) .
C12 C11 C13 109.5(4) .
N12 C12 C11 108.4(4) .
N11 C11' C12' 104.2(6) .
N11 C11' C13 112.1(5) .
C12' C11' C13 105.2(6) .
C11' C12' N12 106.6(6) .
C12 N12 Ni1 111.8(2) .
C12' N12 Ni1 106.0(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S1 2.3343(7) .
Sn1 S2 2.3380(6) .
Sn1 S3 2.4512(6) .
Sn1 S3 2.4553(6) 3_566
S3 Sn1 2.4553(6) 3_566
Ni1 N12 2.091(2) .
Ni1 N3 2.115(2) .
Ni1 N1 2.1204(19) .
Ni1 N2 2.129(2) .
Ni1 N4 2.134(2) .
Ni1 N11 2.167(2) .
N1 C5 1.475(3) .
N1 C1 1.475(3) .
N1 C3 1.488(3) .
C1 C2 1.515(4) .
C2 N2 1.475(3) .
C3 C4 1.524(4) .
C4 N3 1.475(3) .
C5 C6 1.519(4) .
C6 N4 1.477(4) .
N11 C11' 1.493(7) .
N11 C11 1.516(5) .
C11 C12 1.517(7) .
C11 C13 1.567(5) .
C12 N12 1.449(6) .
C11' C12' 1.497(11) .
C11' C13 1.528(8) .
C12' N12 1.566(9) .
