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_4322276
_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            'C34 H40 N P2 S2 Tc'
_chemical_formula_weight         686.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.615(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0899(12)
_cell_length_b                   14.3874(15)
_cell_length_c                   11.0872(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1620.9(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2395
_diffrn_reflns_theta_max         23.06
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0025(12)
_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   1.066
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_obs          0.0603
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+7.0183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1802
_refine_ls_wR_factor_obs         0.1646
_reflns_number_observed          1778
_reflns_number_total             2263
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9903477_2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+7.0183P] 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^)+(0.0968P)^2^+7.0183P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322276