Synthesis, Characterization, Crystal Structures, and Reactions of Trigonal Bipyramidal Tin(IV) Complexes Containing a Tetradentate Tripodal Tristhiolatophosphine Ligand. Use in the One-Step Synthesis of an Iron(IV) Complex
Kerry A. (Fusie) Clark; T. Adrian George; Tom J. Brett; Charles R. Ross; Richard K. Shoemaker; Inorganic Chemistry 39 (2000) 2252–2253; doi:10.1021/ic991371n

data_4320990
_publ_contact_author_address
;
Department of Chemistry
University of Nebraska-Lincoln, Lincoln, NE 68588-0304
;
_publ_contact_author_email       tageorge@unlserve.unl.edu
_publ_contact_author_name        'George, T. Adrian'
_publ_contact_author_phone       1(402)4723513
_publ_section_title
;
 Synthesis, Characterization, Crystal Structures, and Reactions of
 Trigonal Bipyramidal Tin(IV) Complexes Containing a Tetradentate Tripodal
 Tristhiolatophosphine Ligand. Use in the One-Step Synthesis of an
 Iron(IV) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2252
_journal_page_last               2253
_journal_paper_doi               10.1021/ic991371n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C33 H41 P S3 Si3 Sn'
_chemical_formula_sum            'C33 H41 P S3 Si3 Sn'
_chemical_formula_weight         767.77
_chemical_name_common
Phenyl[tris(2-thio-3-trimethylsilylphenyl-k3S)phosphine-kP]tin
_chemical_name_systematic
; 
 Phenyl[tris(2-thio-3-trimethylsilylphenyl-k3S)phosphine-kP]tin 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.86(3)
_cell_angle_beta                 107.21(3)
_cell_angle_gamma                90.75(3)
_cell_formula_units_Z            2
_cell_length_a                   10.111(2)
_cell_length_b                   14.737(3)
_cell_length_c                   15.342(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1990.8(10)
_computing_cell_refinement       MARXDS
_computing_data_collection       MARDC
_computing_data_reduction        MARXDS
_computing_molecular_graphics    XP
_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 0.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  'MARResearch imaging plate'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14905
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         4.25
_exptl_absorpt_coefficient_mu    0.949
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .3
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.073(5)
_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   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+1.1376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                5679
_reflns_number_total             6552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991371n_2.cif
_cod_data_source_block           ni289b,3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1990.8(7)
_cod_database_code               4320990