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_4318150
_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][Zn2Cl6]0.5'
_chemical_formula_sum            'C44 H42 Cl3 N4 P2 Tc Zn'
_chemical_formula_weight         958.48
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.412(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.593(4)
_cell_length_b                   13.922(3)
_cell_length_c                   22.152(5)
_cell_measurement_temperature    183(2)
_cell_volume                     4411.5(18)
_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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14060
_diffrn_reflns_theta_full        20.99
_diffrn_reflns_theta_max         20.99
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.8580
_exptl_absorpt_correction_T_min  0.6751
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          .05
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0041(4)
_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   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.797
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+4.5004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                3656
_reflns_number_total             4728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020017d_2.cif
_cod_data_source_block           01091t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        4411.6(18)
_cod_database_code               4318150