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_1517516
_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         'C18 H24 Tc F6 P'
_chemical_formula_sum            'C18 H24 F6 P Tc'
_chemical_formula_weight         483.34
_chemical_name_common            '[Tc(mesitylene)2]PF6'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2697(5)
_cell_length_b                   13.0695(16)
_cell_length_c                   15.815(6)
_cell_measurement_reflns_used    5887
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.6170
_cell_measurement_theta_min      2.7870
_cell_volume                     1916.0(8)
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12954
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.9077
_exptl_absorpt_correction_T_min  0.6877
_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    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                5484
_reflns_number_total             5851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02461c2.cif
_cod_data_source_block           c:[tc(mesitylene)2](pf6)
_cod_depositor_comments
'Adding full bibliography for 1517514--1517518.cif.'
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               1517516