Syntheses and Characterization of Dicarbonyl-Nitrosyl Complexes of Technetium(I) and Rhenium(I) in Aqueous Media: Spectroscopic, Structural, and DFT Analyses
Roger Schibli; Niklaus Marti; Patrick Maurer; Bernhard Spingler; Marie-Line Lehaire; Volker Gramlich; Charles L. Barnes; Inorganic Chemistry 44 (2005) 683–690; doi:10.1021/ic049599k

data_4308516
_publ_section_title
;
Syntheses and Characterization of Dicarbonyl-Nitrosyl Complexes of
Technetium(I) and Rhenium(I) in Aqueous Media: Spectroscopic, Structural,
and DFT Analyses
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              683
_journal_page_last               690
_journal_paper_doi               10.1021/ic049599k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C10 H20 Br3 N2 O3 Re'
_chemical_formula_sum            'C10 H20 Br3 N2 O3 Re'
_chemical_formula_weight         642.21
_chemical_name_systematic
; 
 tetraethylammonium tribromo tricarbonyl rhenate  
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2101(6)
_cell_length_b                   25.1002(12)
_cell_length_c                   8.8348(7)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    183(2)
_cell_volume                     1820.6(2)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f oscillation scan'
_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  0.1083
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6130
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         2.61
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  8
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    13.262
_exptl_absorpt_correction_T_max  0.4646
_exptl_absorpt_correction_T_min  0.0451
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.408
_refine_diff_density_min         -4.212
_refine_diff_density_rms         0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         978
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1321P)^2^+25.7405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                855
_reflns_number_total             978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049599ksi20041013_083251_3.cif
_cod_data_source_block           rs130804
_cod_database_code               4308516