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_4315258
_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         'C16 H32 Mg O12 Tc2'
_chemical_formula_sum            'C16 H32 Mg O12 Tc2'
_chemical_formula_weight         636.73
_chemical_name_common            Mg(OTcO3)2(THF)4
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.322(5)
_cell_length_b                   16.501(8)
_cell_length_c                   14.416(7)
_cell_measurement_reflns_used    134
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.77
_cell_measurement_theta_min      3.68
_cell_volume                     2455(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.2547
_diffrn_reflns_av_sigmaI/netI    0.2635
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8703
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        .1
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8459
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XRED 32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.747
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.747
_refine_ls_R_factor_all          0.2090
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                838
_reflns_number_total             2164
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic1001094_si_002_1.cif
_cod_data_source_block           eotcgrig
_cod_database_code               4315258