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_4347799
_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, 2NiC7H25N5O1, 4H2O'
_chemical_formula_sum            'C14 H58 N10 Ni2 O6 S6 Sn2'
_chemical_formula_weight         1009.86
_chemical_name_common            '[Ni(tren)(ma)(H2O)]2[Sn2S6]*4H2O'
_chemical_name_systematic
; 
 '[Ni(C6H18N4)(CH5N)(H2O)]2[Sn2S6]*4H2O'
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.833(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1715(3)
_cell_length_b                   10.5384(3)
_cell_length_c                   15.8594(5)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.05
_cell_volume                     1827.45(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f 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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28097
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.751
_exptl_absorpt_correction_T_max  0.7169
_exptl_absorpt_correction_T_min  0.5922
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0025(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   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0261
_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/[\s^2^(Fo^2^)+(0.0437P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                3760
_reflns_number_total             4371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00625_si_003.cif
_cod_data_source_block           jh1331
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347799