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_4324049
_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
'chemical oxidation of Tc2Cl4(PMe2Ph)4 in the presence of Cl- '
_chemical_formula_moiety         'Tc2, Cl5, (P C8 H11)3'
_chemical_formula_structural     'Tc2, Cl5, (P C8 H11)3'
_chemical_formula_sum            'C24 H33 Cl5 P3 Tc2'
_chemical_formula_weight         787.66
_chemical_name_common
'1,3,6-ditechnetium pentachloro tris(dimethylphenylphosphine)'
_chemical_name_systematic
; 
1,3,6-ditechnetium pentachloro tris(dimethylphenylphosphine)
;
_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                 98.144(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1340(14)
_cell_length_b                   14.4057(13)
_cell_length_c                   19.501(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     3096.3(7)
_computing_cell_refinement       'CAD4 (Enraf Nonius)'
_computing_data_collection       'CAD4 (Enraf Nonius)'
_computing_data_reduction        'SDP  (Enraf Nonius)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4S
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5722
_diffrn_reflns_theta_max         24.90
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.75
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5423
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.131
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0261
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.6994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0806
_refine_ls_wR_factor_obs         0.0659
_reflns_number_observed          4243
_reflns_number_total             5424
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9508583_4.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+1.6994P] 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^)+(0.0331P)^2^+1.6994P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4324049