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_4320991
_publ_contact_author_address
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Department of Chemistry
University of Nebraska-Lincoln, Lincoln, NE 68588-0304
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_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
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 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
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_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         'C27 H23 P S3 Sn'
_chemical_formula_sum            'C27 H23 P S3 Sn'
_chemical_formula_weight         593.29
_chemical_name_common
Phenyl[tris(2-thio-5-methylphenyl-k3S)phosphine-kP]tin
_chemical_name_systematic
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  Phenyl[tris(2-thio-5-methylphenyl-k3S)phosphine-kP]tin 
 
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_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                 91.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.641(2)
_cell_length_b                   15.354(3)
_cell_length_c                   15.384(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64
_cell_measurement_theta_min      50
_cell_volume                     2512.2(8)
_computing_cell_refinement       'CAD4 Express (Enraf-Nonius, 1988)'
_computing_data_collection       'CAD4 Express (Enraf-Nonius, 1988)'
_computing_data_reduction        'HELENA/PLATON (Spek, 1990)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  counter
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_max         69.91
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        <5
_diffrn_standards_interval_time  60
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    11.119
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.323
_refine_diff_density_min         -2.115
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.00195(14)
_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   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0778P)^2^+2.3501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                4363
_reflns_number_total             4757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991371n_3.cif
_cod_data_source_block           jm027a,2
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Monoclinic P' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2512.2(9)
_cod_database_code               4320991