Metal-Metal Multiply-Bonded Complexes of Technetium. 4.1Photodissociation of the Tc\τbTc Triple Bond in [Tc2(CH3CN)10][BF4]4
F. Albert Cotton; Steven C. Haefner; Alfred P. Sattelberger; Journal of the American Chemical Society 118 (1996) 5486–5487; doi:10.1021/ja9604727

data_4117150
_publ_section_title
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 Metal-Metal Multiply-Bonded Complexes of Technetium. 4.1Photodissociation
 of the Tc\\tbTc Triple Bond in [Tc2(CH3CN)10][BF4]4
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5486
_journal_page_last               5487
_journal_paper_doi               10.1021/ja9604727
_journal_volume                  118
_journal_year                    1996
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C12 H18 N6 Tc, (B F4)2'
_chemical_formula_structural     '(Tc (N C2 H3)6) (B F4)2'
_chemical_formula_sum            'C12 H18 B2 F8 N6 Tc'
_chemical_formula_weight         517.94
_chemical_name_systematic
; 
 Technetium(ii) hexakis(acetonitrile) bis tetrafluoroborate 
;
_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                 92.058(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1750(9)
_cell_length_b                   8.3775(7)
_cell_length_c                   16.256(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      19
_cell_volume                     1112.6(2)
_computing_cell_refinement       'CAD4 (Enraf Nonius)'
_computing_data_collection       'CAD4 (Enraf Nonius)'
_computing_data_reduction        SDP
_computing_molecular_graphics    ORTEP
_computing_publication_material  'Microsoft Word'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4-S'
_diffrn_measurement_method       \w-2\q
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2091
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.9428
_exptl_absorpt_correction_type   'empirical (\y scan)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       'well-shaped block'
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.139
_refine_ls_goodness_of_fit_obs   1.187
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_restrained_S_obs      1.187
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_obs          0.0498
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.9908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1422
_refine_ls_wR_factor_obs         0.1345
_reflns_number_observed          1622
_reflns_number_total             1947
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9604727.cif
_cod_data_source_block           FAC1822
_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^)+(0.0850P)^2^+0.9908P] 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^)+(0.0850P)^2^+0.9908P] 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               4117150