New Approach to the Chemistry of Technetium(V) and Rhenium(V) Phenylimido Complexes: Novel [M(NPh)PNP]3+ Metal Fragments (M = Tc, Re; PNP = Aminodiphosphine) Suitable for the Synthesis of Stable Mixed-Ligand Compounds
Marina Porchia; Francesco Tisato; Fiorenzo Refosco; Cristina Bolzati; Mario Cavazza-Ceccato; Giuliano Bandoli; Alessandro Dolmella; Inorganic Chemistry 44 (2005) 4766–4776; doi:10.1021/ic048486y

data_4309060
_publ_contact_author_email       tisato@icis.cnr.it
_publ_contact_author_name        'Francesco Tisato'
_publ_section_title
;
New Approach to the Chemistry of Technetium(V) and Rhenium(V) Phenylimido
Complexes: Novel [M(NPh)PNP]3+ Metal Fragments (M = Tc, Re; PNP =
Aminodiphosphine) Suitable for the Synthesis of Stable Mixed-Ligand
Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4766
_journal_page_last               4776
_journal_paper_doi               10.1021/ic048486y
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C34.5 H35 Cl4 N2 P2 Tc'
_chemical_formula_weight         779.38
_chemical_name_systematic
;
?
;
_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                 107.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.106(3)
_cell_length_b                   12.117(2)
_cell_length_c                   20.481(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      8.0
_cell_volume                     3580.2(13)
_computing_cell_refinement       'P3/P4 ver.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4 ver.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4 ver.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL NT ver.5.10 (Bruker, 1999)'
_computing_publication_material  'SHELXTL NT ver.5.10 (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT ver.5.10 (Bruker, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nicolet R3m/V diffractometer'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1296
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8101
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
A.C.T. North, D.C. Phillips, F.S. Mathews, Acta Crystallogr.
Sect. A 24 (1968) p. 351.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0000(3)
_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   0.879
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         8101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          2.799
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1558
_reflns_number_gt                3725
_reflns_number_total             8101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048486ysi20050518_100624_3.cif
_cod_data_source_block           2.1/2CH2Cl2
_cod_original_cell_volume        3580.2(12)
_cod_original_formula_sum        'C34.50 H35 Cl4 N2 P2 Tc'
_cod_database_code               4309060