Reactivity of the [M(PS)2](+) Building Block (M = Re(III) and (99m)Tc(III); PS = Phosphinothiolate) toward Isopropylxanthate and Pyridine-2-thiolate.
Salvarese, Nicola; Dolmella, Alessandro; Refosco, Fiorenzo; Bolzati, Cristina; Inorganic chemistry 54 (2015) 1634–1644; doi:10.1021/ic502632h

data_4342057
_publ_section_title
;
 Reactivity of the [M(PS)2](+) Building Block (M = Re(III) and
 (99m)Tc(III); PS = Phosphinothiolate) toward Isopropylxanthate and
 Pyridine-2-thiolate.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1634
_journal_page_last               1644
_journal_paper_doi               10.1021/ic502632h
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C33 H32 N P2 Re S3'
_chemical_formula_sum            'C33 H32 N P2 Re S3'
_chemical_formula_weight         786.92
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_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_date             2013-05-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6997(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.21123(12)
_cell_length_b                   12.79865(17)
_cell_length_c                   24.1186(3)
_cell_measurement_reflns_used    21784
_cell_measurement_temperature    243.1(1)
_cell_measurement_theta_max      29.4017
_cell_measurement_theta_min      2.2317
_cell_volume                     3141.46(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      243.1(1)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
  1 omega -103.00  -55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.6805  179.0000  -60.0000 48

  2 omega   47.00  101.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805  179.0000   60.0000 54

  3 omega  -39.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805    0.0000 -120.0000 113

  4 omega   -5.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805   77.0000  150.0000 59

  5 omega  -61.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.6805  -77.0000    0.0000 65

  6 omega   -8.00   95.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805   77.0000  -60.0000 103

  7 omega   34.00  103.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805  179.0000 -150.0000 69

  8 omega  -51.00   23.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805  -38.0000 -150.0000 74

  9 omega   -7.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805   38.0000  -90.0000 100

 10 omega   34.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805  179.0000  120.0000 27

 11 omega    2.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805   77.0000   90.0000 65

 12 omega  -42.00   18.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805  -38.0000  150.0000 60

 13 omega   47.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6805 -134.0000  -56.0000 40
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0692944000
_diffrn_orient_matrix_UB_12      -0.0004219000
_diffrn_orient_matrix_UB_13      -0.0055297000
_diffrn_orient_matrix_UB_21      0.0020221000
_diffrn_orient_matrix_UB_22      0.0521677000
_diffrn_orient_matrix_UB_23      -0.0098232000
_diffrn_orient_matrix_UB_31      0.0071561000
_diffrn_orient_matrix_UB_32      -0.0187001000
_diffrn_orient_matrix_UB_33      -0.0272719000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51398
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         29.47
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0.0(1)
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.612
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0191P)^2^+3.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                7246
_reflns_number_total             8146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502632h_si_002.cif
_cod_data_source_block           exp_204_abs
_cod_depositor_comments          'Adding full bibliography for 4342057.cif.'
_cod_database_code               4342057