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_1517514
_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         'C12 H12 Tc, F6 P'
_chemical_formula_sum            'C12 H12 F6 P Tc'
_chemical_formula_weight         399.19
_chemical_name_common            '[Tc(benzol)2]PF6'
_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                 94.232(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8831(7)
_cell_length_b                   9.8745(5)
_cell_length_c                   9.7190(6)
_cell_measurement_reflns_used    2629
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.4940
_cell_measurement_theta_min      2.5600
_cell_volume                     1328.73(13)
_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, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7418
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.8239
_exptl_absorpt_correction_T_min  0.7193
_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    1.995
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.0818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                2139
_reflns_number_total             3296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02461c2.cif
_cod_data_source_block           c:[tc(benzene)2](pf6)
_cod_depositor_comments
'Adding full bibliography for 1517514--1517518.cif.'
_cod_original_cell_volume        1328.74(13)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1517514