C-H Bond Activation of Coordinated Pyridine: Ortho-Pyridyl-Ditechnetiumhydridocarbonyl Metal Cyclus. Crystal Structure and Dynamic Behavior in Solution
Maaz Zuhayra; Ulf Lützen; Arne Lützen; Laszlo Papp; Eberhard Henze; Gernot Friedrichs; Franz Oberdorfer; Inorganic Chemistry 47 (2008) 10177–10182; doi:10.1021/ic8015063

data_4306692
_publ_section_title
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C-H Bond Activation of Coordinated Pyridine:
Ortho-Pyridyl-Ditechnetiumhydridocarbonyl Metal Cyclus. Crystal Structure
and Dynamic Behavior in Solution
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10177
_journal_page_last               10182
_journal_paper_doi               10.1021/ic8015063
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C18 H10 N2 O8 Tc2'
_chemical_formula_weight         578.28
_chemical_name_systematic
Di-\m-Carbonyl-bis(pyridino-tricarbonyltechnetium)
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.116(16)
_cell_length_b                   10.359(8)
_cell_length_c                   12.148(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2280(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2614
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.255
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1128
_exptl_crystal_recrystallization_method 'Acetone/Ether 1:1'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(10)
_refine_ls_extinction_coef       0.0028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_obs          0.0516
_refine_ls_shift/esd_max         0.087
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1457
_refine_ls_wR_factor_obs         0.1377
_reflns_number_observed          2265
_reflns_number_total             2614
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic8015063_si_002_1.cif
_cod_data_source_block           zupi
_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^)+(0.1026P)^2^+0.0000P] 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^)+(0.1026P)^2^+0.0000P] 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        2279.7(33)
_cod_database_code               4306692