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_4325451
_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         'C20 H20 n4 O2 Tc, Cl, 2(H2 O)'
_chemical_formula_sum            'C20 H24 Cl O4 Tc n4'
_chemical_formula_weight         517.88
_chemical_name_common            '[(py)4TcO2][Cl].2H2O'
_chemical_name_systematic
; 
 ? 
;
_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                 115.4840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4168(4)
_cell_length_b                   11.9421(4)
_cell_length_c                   15.3310(5)
_cell_measurement_reflns_used    5797
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.39
_cell_volume                     2217.41(12)
_computing_cell_refinement       'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics
'SHELXTL v6.14 and DIAMOND v3.2e (Brandenburg, 2010)'
_computing_publication_material  'SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'SHELXTL  v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14048
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_correction_T_min  0.8064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2511 Friedel pairs'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.7016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                4884
_reflns_number_total             5060
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200747v_si_001_2.cif
_cod_data_source_block           1a
_cod_original_formula_sum        'C20 H24 Cl n4 O4 Tc'
_cod_database_code               4325451