From TcVIIto TcI; facile syntheses of bis-arene complexes [99(m)Tc(arene)2]+from pertechnetate
Benz, Michael; Braband, Henrik; Schmutz, Paul; Halter, Jonathan; Alberto, Roger; Chem. Sci. 6 (2015) 165–; doi:10.1039/C4SC02461C

data_1517515
_publ_section_title
;
 From TcVIIto TcI; facile syntheses of bis-arene complexes
 [99(m)Tc(arene)2]+from pertechnetate
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              165
_journal_paper_doi               10.1039/C4SC02461C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C14 H16 Tc, F6 P '
_chemical_formula_sum            'C14 H16 F6 P Tc'
_chemical_formula_weight         427.24
_chemical_name_common            '[Tc(toluene)2]PF6'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.474(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7559(8)
_cell_length_b                   11.0030(8)
_cell_length_c                   8.9353(8)
_cell_measurement_reflns_used    1610
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.2960
_cell_measurement_theta_min      2.9280
_cell_volume                     754.20(12)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5202
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.9062
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0403P)^2^+0.0475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                1125
_reflns_number_total             1545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02461c2.cif
_cod_data_source_block           meb211113
_cod_depositor_comments
'Adding full bibliography for 1517514--1517518.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1517515