Activation of [^99(m)^TcO4]^-^ by phosphonium cations
Henrik Braband; Michael Benz; Yuji Tooyama; Roger Alberto; Chem.Commun. 50 (2014) 4126–; doi:10.1039/C4CC00718B

data_7112213
_publ_section_title
;
 Activation of [^99(m)^TcO4]^-^ by phosphonium cations
;
_journal_name_full               Chem.Commun.
_journal_page_first              4126
_journal_paper_doi               10.1039/C4CC00718B
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         2(C6H15N3TcO3),Br4O5Tc2,CH2Cl2
_chemical_formula_sum            'C13 H32 Br4 Cl2 N6 O11 Tc4'
_chemical_formula_weight         1230.99
_chemical_name_common            '[TcO3(Me3tach)][TcO4]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.775(3)
_cell_angle_beta                 97.616(2)
_cell_angle_gamma                96.984(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6731(3)
_cell_length_b                   12.5422(4)
_cell_length_c                   13.5332(3)
_cell_measurement_reflns_used    15426
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.8391
_cell_measurement_theta_min      2.7845
_cell_volume                     1662.62(9)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34931
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    6.650
_exptl_absorpt_correction_T_max  0.3977
_exptl_absorpt_correction_T_min  0.1957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         10118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0284P)^2^+1.6613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                9012
_reflns_number_total             10118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00718b2.cif
_cod_data_source_block           c:\hb040313
_cod_original_cell_volume        1662.62(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112213