High-Valent Technetium Complexes with the [99TcO3]+ Core from in Situ Prepared Mixed Anhydrides of [99TcO4]- and Their Reactivities
Yuji Tooyama; Henrik Braband; Bernhard Spingler; Ulrich Abram; Roger Alberto; Inorganic Chemistry 47 (2008) 257–264; doi:10.1021/ic701908q

data_4304405
_publ_section_title
;
High-Valent Technetium Complexes with the [99TcO3]+ Core from in Situ
Prepared Mixed Anhydrides of [99TcO4]- and Their Reactivities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              257
_journal_page_last               264
_journal_paper_doi               10.1021/ic701908q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '[ReO3(tpzm*)]'
_chemical_formula_sum            'C16 H22 N6 O7 Re2'
_chemical_formula_weight         782.80
_chemical_name_common            '[ReO3(tpzm*)]'
_chemical_name_systematic
;
(Tris((3,5-dimethyl)pyrazol-1-yl)methan)-trioxo-rhenium(VII) perrhenat
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   15.2111(2)
_cell_length_b                   12.8651(2)
_cell_length_c                   22.0324(3)
_cell_measurement_reflns_used    14902
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.4481
_cell_measurement_theta_min      2.2768
_cell_volume                     4311.57(11)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '/o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43528
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    11.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.902
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                3433
_reflns_number_total             5091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701908q-file006.cif
_cod_data_source_block           yt1007
_cod_database_code               4304405