Reactivity of a Tin(II) (Iminophosphinoyl)(thiophosphinoyl)methanediide Complex Toward Sulfur: Synthesis and 119Sn Mössbauer Spectroscopic Studies of [{(μ-S)SnC(PPh2=NSiMe3)(PPh2=S)}3Sn(μ3-S)]
Jia-Yi Guo; Hong-Wei Xi; Israel Nowik; Rolfe H. Herber; Yongxin Li; Kok Hwa Lim; Cheuk-Wai So; Inorganic Chemistry 51 (2012) 3996–4001; doi:10.1021/ic2019633

data_4328736
_publ_section_title
;
 Reactivity of a Tin(II) (Iminophosphinoyl)(thiophosphinoyl)methanediide
 Complex Toward Sulfur: Synthesis and 119Sn M\"ossbauer Spectroscopic
 Studies of [{(\m-S)SnC(PPh2=NSiMe3)(PPh2=S)}3Sn(\m3-S)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3996
_journal_page_last               4001
_journal_paper_doi               10.1021/ic2019633
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C108 H87 D24 N3 P6 S7 Si3 Sn4'
_chemical_formula_weight         2444.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.672(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4619(10)
_cell_length_b                   33.693(2)
_cell_length_c                   19.8683(12)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.42
_cell_volume                     11008.0(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1185
_diffrn_reflns_av_sigmaI/netI    0.1024
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            147130
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.8897
_exptl_absorpt_correction_T_min  0.7959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.860
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1235
_refine_ls_number_reflns         27312
_refine_ls_number_restraints     404
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0698P)^2^+103.8710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2238
_reflns_number_gt                17689
_reflns_number_total             27312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019633_si_002.cif
_cod_data_source_block           scw542
_cod_original_cell_volume        11008.1(12)
_cod_database_code               4328736