Metal-Metal Multiply Bonded Complexes of Technetium. 5.1 Tris and Tetrakis(formamidinato) Complexes of Ditechnetium
F. Albert Cotton; Steven C. Haefner; Alfred P. Sattelberger; Inorganic Chemistry 35 (1996) 7350–7357; doi:10.1021/ic960535m

data_4323990
_publ_section_title
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 Metal-Metal Multiply Bonded Complexes of Technetium. 5.1 Tris and
 Tetrakis(formamidinato) Complexes of Ditechnetium
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7350
_journal_page_last               7357
_journal_paper_doi               10.1021/ic960535m
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C45 H45 Cl2 N6 Tc2'
_chemical_formula_structural     'Tc2 Cl2 (C15 H15 N2)3'
_chemical_formula_sum            'C45 H45 Cl2 N6 Tc2'
_chemical_formula_weight         936.77
_chemical_name_systematic
; 
 Dichloro tris(\m-di-p-tolylformamidinate) ditechnetium (II,III) 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.142(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1853(15)
_cell_length_b                   15.6371(15)
_cell_length_c                   17.8116(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      30
_cell_volume                     4232.3(6)
_computing_cell_refinement       TEXSAN
_computing_data_collection       TEXSAN'
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'RIGAKU AFC5R'
_diffrn_measurement_method       \q-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           Cu
_diffrn_radiation_wavelength     1.54060
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6545
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        15
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.766
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   'empirical (\y scans)'
_exptl_crystal_colour            red/purple
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.148
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         5748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_obs          0.0452
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+9.1691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1274
_refine_ls_wR_factor_obs         0.1171
_reflns_number_observed          5095
_reflns_number_total             6295
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960535m_2.cif
_cod_data_source_block           1a
_cod_depositor_comments
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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^)+(0.0505P)^2^+9.1691P] 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^)+(0.0505P)^2^+9.1691P] 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_database_code               4323990