Probing the Presence of Multiple Metal-Metal Bonds in Technetium Chlorides by X-ray Absorption Spectroscopy: Implications for Synthetic Chemistry
Frederic Poineau; Erik V. Johnstone; Paul M. Forster; Longzou Ma; Alfred P. Sattelberger; Kenneth R. Czerwinski; Inorganic Chemistry 51 (2012) 9563–9570; doi:10.1021/ic3014859

data_4330279
_publ_section_title
;
 Probing the Presence of Multiple Metal-Metal Bonds in Technetium
 Chlorides by X-ray Absorption Spectroscopy: Implications for Synthetic
 Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9563
_journal_page_last               9570
_journal_paper_doi               10.1021/ic3014859
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C19 H42 Cl3.91 N O Tc0.95'
_chemical_formula_weight         532.25
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.214(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1856(10)
_cell_length_b                   14.8529(15)
_cell_length_c                   17.2877(18)
_cell_measurement_temperature    100(2)
_cell_volume                     2614.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35883
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             1113
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.853
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6487
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+2.8873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                5695
_reflns_number_total             6487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014859_si_001.cif
_cod_data_source_block           Tc_acetone
_cod_database_code               4330279