A Trigonal-Prismatic Hexanuclear Technetium(II) Bromide Cluster: Solid-State Synthesis and Crystallographic and Electronic Structure
Erik V. Johnstone; Daniel J. Grant; Frederic Poineau; Laura Fox; Paul M. Forster; Longzou Ma; Laura Gagliardi; Kenneth R. Czerwinski; Alfred P. Sattelberger; Inorganic Chemistry 52 (2013) 5660–5662; doi:10.1021/ic400967k

data_4334987
_publ_section_title
;
 A Trigonal-Prismatic Hexanuclear Technetium(II) Bromide Cluster:
 Solid-State Synthesis and Crystallographic and Electronic Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5660
_journal_page_last               5662
_journal_paper_doi               10.1021/ic400967k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Br25 Na Tc12'
_chemical_formula_weight         3196.74
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.6700(10)
_cell_angle_beta                 73.7290(10)
_cell_angle_gamma                87.4880(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5173(5)
_cell_length_b                   10.5233(6)
_cell_length_c                   11.1412(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1064.51(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17149
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    27.238
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Area-Detector Absorption Correction; Siemens Industrial Automation, Inc. 
Madison, WI, 1996
;
_exptl_crystal_density_diffrn    4.987
_exptl_crystal_F_000             1402
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                5858
_reflns_number_total             6456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400967k_si_002.cif
_cod_data_source_block           fp_tcbr2_a_0m_a
_cod_database_code               4334987