Metal-Metal Multiply-Bonded Complexes of Technetium. 3.1 Preparation and Characterization of Phosphine Complexes of Technetium Possessing a Metal-Metal Bond Order of 3.5
F. Albert Cotton; Steven C. Haefner; Alfred P. Sattelberger; Inorganic Chemistry 35 (1996) 1831–1838; doi:10.1021/ic9508583

data_4324048
_publ_section_title
;
 Metal-Metal Multiply-Bonded Complexes of Technetium. 3.1 Preparation and
 Characterization of Phosphine Complexes of Technetium Possessing a
 Metal-Metal Bond Order of 3.5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1831
_journal_page_last               1838
_journal_paper_doi               10.1021/ic9508583
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source
'cold CH3CN solution with 4:1 diethyl ether and thf'
_chemical_formula_moiety
'C32 H44 Cl4 P4 Tc 1+, F6 P 1-, 0.5(C4 H8 O) '
_chemical_formula_structural
'(Tc Cl2 ((C H3)2 (C6 H5) P)2)2 (P F6) (C4 H8 O)0.5'
_chemical_formula_sum            'C34 H48 Cl4 F6 O0.5 P5 Tc2'
_chemical_formula_weight         1071.37
_chemical_name_common
'Ditechnetium tetrachloro tetra(dimethylphenylphosphine) hexafluorophosphate'
_chemical_name_systematic
; 
 Ditechnetium tetrachloro tetra(dimethylphenylphosphine) hexafluorophosphate 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.04(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.580(3)
_cell_length_b                   33.327(3)
_cell_length_c                   13.861(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      30
_cell_volume                     4561.5(18)
_computing_cell_refinement       TEXSAN
_computing_data_collection       TEXSAN
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'AFC5R (Rigaku) '
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6089
_diffrn_reflns_theta_max         55.00
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        9%
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.171
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    n/a
_exptl_crystal_description       acicular
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.667
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         5682
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_obs          0.0504
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+10.7174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1545
_refine_ls_wR_factor_obs         0.1412
_reflns_number_observed          4719
_reflns_number_total             5726
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9508583_3.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+10.7174P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+10.7174P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4561.7(15)
_cod_original_formula_sum        'C34 H48 Cl4 F6 O0.50 P5 Tc2'
_cod_database_code               4324048