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_4324047
_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
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_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        'Chemical oxidation of Tc2Cl4(PMe2Ph)4'
_chemical_formula_moiety         'C32 H44 Cl4 P4 Tc 1+, F6 P 1-'
_chemical_formula_structural     '(Tc Cl4 (P (C H3)2 (C6 H5))4)2 (P F6) '
_chemical_formula_sum            'C32 H44 Cl4 F6 P5 Tc2'
_chemical_formula_weight         1035.32
_chemical_name_common
'Ditechnetium tetrachloro tetra(dimethylphenylhosphine) hexafluorophsphate'
_chemical_name_systematic
; 
 Ditechnetium tetrachloro tetra(dimethylphenylhosphine) hexafluorophsphate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 96.393(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.799(4)
_cell_length_b                   18.254(2)
_cell_length_c                   17.945(5)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     4166.5(18)
_computing_cell_refinement       'CAD4 (Enraf Nonius)'
_computing_data_collection       'CAD4 (Enraf Nonius)'
_computing_data_reduction        'SDP  (Enraf Nonius)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'CAD4 (Enraf Nonius)'
_diffrn_measurement_method       'theta-2theta '
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0773
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_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       plate
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    noref
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+3.8567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1493
_refine_ls_wR_factor_obs         0.1239
_reflns_number_observed          3034
_reflns_number_total             4466
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9508583_2.cif
_cod_data_source_block           xl
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+3.8567P] 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^)+(0.0857P)^2^+3.8567P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4166.4(17)
_cod_database_code               4324047