New Metal-Rich Sulfides Ni6SnS2 and Ni9Sn2S2 with a 2D Metal Framework: Synthesis, Crystal Structure, and Bonding
Alexey I. Baranov; Anna A. Isaeva; Lars A. Kloo; Boris A. Popovkin; Inorganic Chemistry 42 (2003) 6667–6672; doi:10.1021/ic034349+

data_4327466
_publ_contact_author
;
        Boris A. Popovkin
        Inorganic Synthesis Laboratory
        Moscow State University
        Leninskie Gory
        119992 Moscow
        Russia
;
_publ_contact_author_email       popovkin@inorg.chem.msu.ru
_publ_contact_author_fax         '7 095 939-0171'
_publ_contact_author_phone       '7 095 939-3339'
_publ_section_title
;
 New Metal-Rich Sulfides Ni6SnS2 and Ni9Sn2S2 with a 2D Metal Framework:
 Synthesis, Crystal Structure, and Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6667
_journal_page_last               6672
_journal_paper_doi               10.1021/ic034349+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'Ni6 Sn S2'
_chemical_formula_sum            'Ni12 S4 Sn2'
_chemical_formula_weight         1070.14
_chemical_name_common            'nickel tin sulphide'
_chemical_name_systematic        'nickel tin sulphide'
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.6500(5)
_cell_length_b                   3.6500(5)
_cell_length_c                   18.141(2)
_cell_measurement_reflns_used    446
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.44
_cell_measurement_theta_min      4.50
_cell_volume                     241.68(5)
_computing_cell_refinement       'KappaCCD (Nonius)'
_computing_data_collection       'KappaCCD (Nonius)'
_computing_data_reduction        Denzo
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56090
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            994
_diffrn_reflns_theta_full        38.44
_diffrn_reflns_theta_max         38.44
_diffrn_reflns_theta_min         4.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    14.932
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_process_details   ScalePack
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    7.353
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.255
_refine_diff_density_min         -4.504
_refine_diff_density_rms         0.664
_refine_ls_extinction_coef       0.007(3)
_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   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0486
_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/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                253
_reflns_number_total             447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343492Bsi20030625_063749_1.cif
_cod_data_source_block           612
_cod_original_cell_volume        241.68(6)
_cod_database_code               4327466