Synthesis, Characterization, and Structures of R3EOTcO3 Complexes (E = C, Si, Ge, Sn, Pb) and Related Compounds
Elisabeth Oehlke; Roger Alberto; Ulrich Abram; Inorganic Chemistry 49 (2010) 3525–3530; doi:10.1021/ic1001094

data_4315259
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin 
      Institute of Chemistry
      Fabeckstrasse 34-36
      D-14195 Berlin
      Germany
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Synthesis, Characterization, and Structures of R3EOTcO3 Complexes (E = C,
 Si, Ge, Sn, Pb) and Related Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3525
_journal_page_last               3530
_journal_paper_doi               10.1021/ic1001094
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C4 H10 Cl3 O3 Tc, 2(C4 H8 O)'
_chemical_formula_sum            'C12 H26 Cl3 O5 Tc'
_chemical_formula_weight         454.68
_chemical_name_common            '[TcOCl3(OH2)(THF)].2THF'
_chemical_name_systematic
;
 Aquatrichlorooxotetrahydofurantechnetium(V)
 tetrahydrofurane solvate
;
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.190(10)
_cell_angle_beta                 109.400(10)
_cell_angle_gamma                97.400(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2940(10)
_cell_length_b                   10.7250(10)
_cell_length_c                   11.911(2)
_cell_measurement_reflns_used    8744
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.01
_cell_volume                     942.9(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10059
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.711
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         5036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                3714
_reflns_number_total             5036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1001094_si_002_2.cif
_cod_data_source_block           eotc1
_cod_database_code               4315259