Room-Temperature Synthesis of Thiostannates from {[Ni(tren)]2[Sn2S6]}n.
Hilbert, Jessica; Näther, Christian; Weihrich, Richard; Bensch, Wolfgang; Inorganic chemistry 55 (2016) 7859–7865; doi:10.1021/acs.inorgchem.6b00625

data_4347801
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0390P)^2^+0.1858P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_shelxl_version_number           2014-3
_shelx_res_checksum              53531
_shelx_hkl_checksum              63249