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_4308514
_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_sum            'C4 Cl4 N2 O6 Tc2'
_chemical_formula_weight         509.86
_chemical_name_systematic
; 
 ditechnetium(I)-hexachloro-tetracarbonyl-dinitrosyl 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 105.80(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.82(3)
_cell_length_b                   6.103(6)
_cell_length_c                   12.151(16)
_cell_measurement_temperature    293(2)
_cell_volume                     1343(3)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'PICKER STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            707
_diffrn_reflns_theta_full        49.92
_diffrn_reflns_theta_max         49.92
_diffrn_reflns_theta_min         4.88
_exptl_absorpt_coefficient_mu    24.267
_exptl_absorpt_correction_T_max  .304
_exptl_absorpt_correction_T_min  .125
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          .09
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         707
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                691
_reflns_number_total             707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049599ksi20041013_083251_1.cif
_cod_data_source_block           tec2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4308514