Synthesis of a Novel Class of trigonal Bipyramidal Nitrido Tc(V) Complexes with Phosphino-Thiol Ligands. Crystal Structure of [99gTc(N)(L1)2] [L1= 2-(Diphenylphosphino)ethanethiolato] and [99gTc(N)(L5)2] [L5= 2-(Ditolylphosphino)propanethiolato]
Cristina Bolzati; Alessandra Boschi; Licia Uccelli; Erica Malagò; Giuliano Bandoli; Francesco Tisato; Fiorenzo Refosco; Roberto Pasqualini; Adriano Duatti; Inorganic Chemistry 38 (1999) 4473–4479; doi:10.1021/ic9903477

data_4322275
_publ_section_title
;
 Synthesis of a Novel Class of trigonal Bipyramidal Nitrido Tc(V)
 Complexes with Phosphino-Thiol Ligands. Crystal Structure of
 [99gTc(N)(L1)2] [L1= 2-(Diphenylphosphino)ethanethiolato] and
 [99gTc(N)(L5)2] [L5= 2-(Ditolylphosphino)propanethiolato]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4473
_journal_page_last               4479
_journal_paper_doi               10.1021/ic9903477
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H28 N P2 S2 Tc'
_chemical_formula_weight         602.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.06(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.837(16)
_cell_length_b                   7.327(6)
_cell_length_c                   31.521(20)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      7.8
_cell_volume                     5353(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet Siemens R3m/V'
_diffrn_measurement_method       omega-2theta
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            4787
_diffrn_reflns_theta_max         20.05
_diffrn_reflns_theta_min         2.60
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00000(10)
_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_all   1.060
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         2511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_obs          0.0572
_refine_ls_shift/esd_max         -3.924
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+119.4638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1532
_refine_ls_wR_factor_obs         0.1404
_reflns_number_observed          2057
_reflns_number_total             2513
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9903477_1.cif
_cod_data_source_block           1_IC9903477_March30,1999
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+119.4638P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+119.4638P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5353.1(65)
_cod_database_code               4322275