Synthesis and Characterization of Technetiumtetrakis(acetonitrile)bis(triphenylphosphine) Cationic Complexes
Evan Freiberg; William M. Davis; Alan Davison; Alun G. Jones; Inorganic Chemistry 41 (2002) 3337–3339; doi:10.1021/ic020017d

data_4318149
_publ_section_title
;
 Synthesis and Characterization of
 Technetiumtetrakis(acetonitrile)bis(triphenylphosphine) Cationic
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3337
_journal_page_last               3339
_journal_paper_doi               10.1021/ic020017d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[Tc(CH3CN)4(PPh3)2](PF6)2'
_chemical_formula_sum            'C50 H42 F12 N4 O2 P4 Tc'
_chemical_formula_weight         1180.76
_chemical_name_systematic        ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   16.6859(19)
_cell_length_b                   16.5534(18)
_cell_length_c                   20.086(2)
_cell_measurement_temperature    183(2)
_cell_volume                     5547.9(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18129
_diffrn_reflns_theta_full        21.50
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0009(3)
_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   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+1.9730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                1929
_reflns_number_total             3181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020017d_1.cif
_cod_data_source_block           01018tr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5547.8(11)
_cod_database_code               4318149