Fluoridonitrosyl Complexes of Technetium(I) and Technetium(II). Synthesis, Characterization, Reactions, and DFT Calculations.
Balasekaran, Samundeeswari Mariappan; Spandl, Johann; Hagenbach, Adelheid; Köhler, Klaus; Drees, Markus; Abram, Ulrich; Inorganic chemistry 53 (2014) 5117–5128; doi:10.1021/ic500229r

data_4338315
_publ_section_title
;
 Fluoridonitrosyl Complexes of Technetium(I) and Technetium(II).
 Synthesis, Characterization, Reactions, and DFT Calculations.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5117
_journal_page_last               5128
_journal_paper_doi               10.1021/ic500229r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C2 H12 F3 N5 O3 Tc, C2 H F3 O2, C2 F3 O2  '
_chemical_formula_sum            'C6 H13 F9 N5 O7 Tc'
_chemical_formula_weight         536.21
_chemical_name_systematic
;
tetrammine(trifluoroacetato)nitrosyltechnetium(I) trifluoroacetate 
trifluoroacetic acid solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.640(10)
_cell_angle_beta                 100.090(10)
_cell_angle_gamma                98.180(10)
_cell_formula_units_Z            2
_cell_length_a                   7.1330(10)
_cell_length_b                   9.3230(10)
_cell_length_c                   14.1980(10)
_cell_measurement_reflns_used    13222
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      3.36
_cell_volume                     902.01(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ortep
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10086
_diffrn_reflns_theta_full        29.20
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.025(2)
_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_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4235
_reflns_number_total             4834
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500229r_si_002.cif
_cod_data_source_block           Tc(NO)(ammine)4_triflate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338309--4338316.cif.
;
_cod_original_cell_volume        902.01(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338315