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_4330280
_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            'C35 H78 Cl14 N2 O0 Tc2'
_chemical_formula_weight         1221.11
_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                 92.090(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.815(3)
_cell_length_b                   14.7166(19)
_cell_length_c                   16.908(2)
_cell_measurement_temperature    100(2)
_cell_volume                     5424.6(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62464
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6210
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.259
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         11059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+90.0866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                8338
_reflns_number_total             11059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3014859_si_002.cif
_cod_data_source_block           Tc_CH2Cl2
_cod_original_cell_volume        5424.7(12)
_cod_database_code               4330280