Electronic and Molecular Structures of trans-Dioxotechnetium(V) Polypyridyl Complexes in the Solid State
Sayandev Chatterjee; Andrew S. Del Negro; Zheming Wang; Matthew K. Edwards; Frances N. Skomurski; Sean E. Hightower; Jeanette A. Krause; Brendan Twamley; B. Patrick Sullivan; Christian Reber; William R. Heineman; Carl J. Seliskar; Samuel A. Bryan; Inorganic Chemistry 50 (2011) 5815–5823; doi:10.1021/ic200747v

data_4325452
_publ_contact_author_address
;     Energy & Environment Directorate
      Pacific northwest National Laboratory
      Richland, WA 99352  USA
;
_publ_contact_author_email       sam.bryan@pnl.gov
_publ_contact_author_name        'Dr. Samuel A. Bryan'
_publ_contact_author_phone       '509 376 6949'
_publ_section_title
;
 Electronic and Molecular Structures of trans-Dioxotechnetium(V)
 Polypyridyl Complexes in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5815
_journal_page_last               5823
_journal_paper_doi               10.1021/ic200747v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C24 H28 n4 O2 Tc, Cl, 2(H2 O)'
_chemical_formula_sum            'C24 H32 Cl O4 Tc n4'
_chemical_formula_weight         573.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.23960(10)
_cell_length_b                   10.23960(10)
_cell_length_c                   42.6378(8)
_cell_measurement_reflns_used    9656
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      67.85
_cell_measurement_theta_min      4.99
_cell_volume                     3871.61(9)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker SMART v5.634'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART6000 CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            31951
_diffrn_reflns_theta_full        68.08
_diffrn_reflns_theta_max         68.08
_diffrn_reflns_theta_min         4.99
_exptl_absorpt_coefficient_mu    5.785
_exptl_absorpt_correction_T_max  0.8016
_exptl_absorpt_correction_T_min  0.5954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2291 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4677
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                4526
_reflns_number_total             4677
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200747v_si_001_3.cif
_cod_data_source_block           2a
_cod_original_formula_sum        'C24 H32 Cl n4 O4 Tc'
_cod_database_code               4325452