#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:07:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179232 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/52/4315259.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4315259
loop_
_publ_author_name
'Elisabeth Oehlke'
'Roger Alberto'
'Ulrich Abram'
_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/[σ²(Fo²)+(0.0798P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc1 Tc 0.19295(4) 0.32236(3) 0.25933(3) 0.04042(12) Uani 1 1 d . . .
Cl1 Cl 0.16831(19) 0.49679(12) 0.17423(13) 0.0628(3) Uani 1 1 d . . .
Cl2 Cl 0.34267(18) 0.24013(15) 0.13529(14) 0.0709(4) Uani 1 1 d . . .
Cl3 Cl 0.14408(17) 0.11910(11) 0.29695(12) 0.0580(3) Uani 1 1 d . . .
O1 O 0.3591(4) 0.4001(4) 0.3883(3) 0.0607(9) Uani 1 1 d . . .
O2 O 0.0024(4) 0.3674(3) 0.3242(3) 0.0412(6) Uani 1 1 d . . .
O3 O -0.0559(4) 0.2196(3) 0.0846(3) 0.0474(7) Uani 1 1 d . . .
C31 C -0.2163(8) 0.1411(7) 0.0784(5) 0.0745(16) Uani 1 1 d . . .
H31A H -0.2517 0.1866 0.1443 0.089 Uiso 1 1 calc R . .
H31B H -0.1981 0.0566 0.0893 0.089 Uiso 1 1 calc R . .
C32 C -0.2620(8) 0.1798(6) -0.1169(5) 0.0660(13) Uani 1 1 d . . .
H32A H -0.2919 0.1182 -0.1993 0.079 Uiso 1 1 calc R . .
H32B H -0.2964 0.2609 -0.1262 0.079 Uiso 1 1 calc R . .
C33 C -0.3527(7) 0.1211(6) -0.0446(6) 0.0713(15) Uani 1 1 d . . .
H33A H -0.4449 0.1652 -0.0357 0.086 Uiso 1 1 calc R . .
H33B H -0.4044 0.0277 -0.0871 0.086 Uiso 1 1 calc R . .
C34 C -0.0715(7) 0.2066(6) -0.0428(4) 0.0633(13) Uani 1 1 d . . .
H34A H -0.0225 0.1344 -0.0736 0.076 Uiso 1 1 calc R . .
H34B H -0.0102 0.2874 -0.0474 0.076 Uiso 1 1 calc R . .
O4 O -0.1658(6) 0.2285(3) 0.4142(4) 0.0677(10) Uani 1 1 d . . .
C41 C -0.2098(13) 0.0930(6) 0.4009(10) 0.114(3) Uani 1 1 d . . .
H41A H -0.2641 0.0425 0.3129 0.136 Uiso 1 1 calc R . .
H41B H -0.1044 0.0636 0.4379 0.136 Uiso 1 1 calc R . .
C42 C -0.3254(15) 0.0723(7) 0.4598(11) 0.123(4) Uani 1 1 d . . .
H42A H -0.2783 0.0279 0.5212 0.148 Uiso 1 1 calc R . .
H42B H -0.4373 0.0168 0.3988 0.148 Uiso 1 1 calc R . .
C43 C -0.3498(10) 0.2008(6) 0.5216(7) 0.0794(18) Uani 1 1 d . . .
H43A H -0.2918 0.2245 0.6117 0.095 Uiso 1 1 calc R . .
H43B H -0.4735 0.1997 0.5005 0.095 Uiso 1 1 calc R . .
C44 C -0.2672(9) 0.2944(5) 0.4714(7) 0.0749(18) Uani 1 1 d . . .
H44A H -0.3569 0.3200 0.4109 0.090 Uiso 1 1 calc R . .
H44B H -0.1936 0.3734 0.5387 0.090 Uiso 1 1 calc R . .
O5 O -0.2103(6) 0.5141(4) 0.2570(4) 0.0755(12) Uani 1 1 d . . .
C51 C -0.2749(8) 0.5881(6) 0.3423(5) 0.0667(14) Uani 1 1 d . . .
H51A H -0.1897 0.6124 0.4274 0.080 Uiso 1 1 calc R . .
H51B H -0.3836 0.5368 0.3374 0.080 Uiso 1 1 calc R . .
C52 C -0.3047(13) 0.7065(7) 0.3053(8) 0.101(2) Uani 1 1 d . . .
H52A H -0.4240 0.7153 0.2924 0.121 Uiso 1 1 calc R . .
H52B H -0.2241 0.7850 0.3695 0.121 Uiso 1 1 calc R . .
C53 C -0.275(2) 0.6896(13) 0.1923(12) 0.176(7) Uani 1 1 d . . .
H53A H -0.1684 0.7507 0.2067 0.211 Uiso 1 1 calc R . .
H53B H -0.3725 0.7067 0.1300 0.211 Uiso 1 1 calc R . .
C54 C -0.2602(15) 0.5524(11) 0.1483(7) 0.130(4) Uani 1 1 d . . .
H54A H -0.3716 0.4966 0.0869 0.156 Uiso 1 1 calc R . .
H54B H -0.1720 0.5481 0.1116 0.156 Uiso 1 1 calc R . .
H21 H -0.062(8) 0.307(6) 0.356(6) 0.074(18) Uiso 1 1 d . . .
H22 H -0.061(9) 0.412(6) 0.304(6) 0.070(19) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tc1 O2 96.80(15) . . ?
O1 Tc1 O3 175.43(15) . . ?
O2 Tc1 O3 78.66(12) . . ?
O1 Tc1 Cl2 99.11(13) . . ?
O2 Tc1 Cl2 164.08(9) . . ?
O3 Tc1 Cl2 85.43(9) . . ?
O1 Tc1 Cl1 97.87(14) . . ?
O2 Tc1 Cl1 88.52(9) . . ?
O3 Tc1 Cl1 81.59(8) . . ?
Cl2 Tc1 Cl1 89.49(6) . . ?
O1 Tc1 Cl3 97.97(14) . . ?
O2 Tc1 Cl3 87.43(9) . . ?
O3 Tc1 Cl3 82.45(8) . . ?
Cl2 Tc1 Cl3 90.18(5) . . ?
Cl1 Tc1 Cl3 164.01(5) . . ?
Tc1 O2 H21 123(3) . . ?
Tc1 O2 H22 127(5) . . ?
H21 O2 H22 104(6) . . ?
C34 O3 C31 107.4(4) . . ?
C34 O3 Tc1 125.2(3) . . ?
C31 O3 Tc1 126.9(3) . . ?
O3 C31 C33 107.9(4) . . ?
O3 C31 H31A 110.1 . . ?
C33 C31 H31A 110.1 . . ?
O3 C31 H31B 110.1 . . ?
C33 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
C34 C32 C33 105.8(4) . . ?
C34 C32 H32A 110.6 . . ?
C33 C32 H32A 110.6 . . ?
C34 C32 H32B 110.6 . . ?
C33 C32 H32B 110.6 . . ?
H32A C32 H32B 108.7 . . ?
C31 C33 C32 106.0(5) . . ?
C31 C33 H33A 110.5 . . ?
C32 C33 H33A 110.5 . . ?
C31 C33 H33B 110.5 . . ?
C32 C33 H33B 110.5 . . ?
H33A C33 H33B 108.7 . . ?
O3 C34 C32 105.7(4) . . ?
O3 C34 H34A 110.6 . . ?
C32 C34 H34A 110.6 . . ?
O3 C34 H34B 110.6 . . ?
C32 C34 H34B 110.6 . . ?
H34A C34 H34B 108.7 . . ?
C44 O4 C41 109.0(4) . . ?
C42 C41 O4 109.4(5) . . ?
C42 C41 H41A 109.8 . . ?
O4 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
O4 C41 H41B 109.8 . . ?
H41A C41 H41B 108.2 . . ?
C41 C42 C43 108.6(5) . . ?
C41 C42 H42A 110.0 . . ?
C43 C42 H42A 110.0 . . ?
C41 C42 H42B 110.0 . . ?
C43 C42 H42B 110.0 . . ?
H42A C42 H42B 108.3 . . ?
C42 C43 C44 103.9(5) . . ?
C42 C43 H43A 111.0 . . ?
C44 C43 H43A 111.0 . . ?
C42 C43 H43B 111.0 . . ?
C44 C43 H43B 111.0 . . ?
H43A C43 H43B 109.0 . . ?
O4 C44 C43 107.0(4) . . ?
O4 C44 H44A 110.3 . . ?
C43 C44 H44A 110.3 . . ?
O4 C44 H44B 110.3 . . ?
C43 C44 H44B 110.3 . . ?
H44A C44 H44B 108.6 . . ?
C54 O5 C51 108.7(5) . . ?
O5 C51 C52 106.1(5) . . ?
O5 C51 H51A 110.5 . . ?
C52 C51 H51A 110.5 . . ?
O5 C51 H51B 110.5 . . ?
C52 C51 H51B 110.5 . . ?
H51A C51 H51B 108.7 . . ?
C53 C52 C51 106.2(6) . . ?
C53 C52 H52A 110.5 . . ?
C51 C52 H52A 110.5 . . ?
C53 C52 H52B 110.5 . . ?
C51 C52 H52B 110.5 . . ?
H52A C52 H52B 108.7 . . ?
C52 C53 C54 107.9(7) . . ?
C52 C53 H53A 110.1 . . ?
C54 C53 H53A 110.1 . . ?
C52 C53 H53B 110.1 . . ?
C54 C53 H53B 110.1 . . ?
H53A C53 H53B 108.4 . . ?
O5 C54 C53 103.9(7) . . ?
O5 C54 H54A 111.0 . . ?
C53 C54 H54A 111.0 . . ?
O5 C54 H54B 111.0 . . ?
C53 C54 H54B 111.0 . . ?
H54A C54 H54B 109.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 O1 1.620(3) . ?
Tc1 O2 2.037(3) . ?
Tc1 O3 2.290(3) . ?
Tc1 Cl2 2.3162(12) . ?
Tc1 Cl1 2.3366(13) . ?
Tc1 Cl3 2.3429(12) . ?
O2 H21 1.01(7) . ?
O2 H22 0.77(6) . ?
O3 C34 1.448(6) . ?
O3 C31 1.450(6) . ?
C31 C33 1.468(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C34 1.480(8) . ?
C32 C33 1.510(8) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
O4 C44 1.404(6) . ?
O4 C41 1.407(6) . ?
C41 C42 1.389(10) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.468(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.491(8) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
O5 C54 1.401(8) . ?
O5 C51 1.423(6) . ?
C51 C52 1.467(9) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.418(12) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.472(14) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H21 O4 1.01(7) 1.56(7) 2.561(4) 173(6) .
O2 H22 O5 0.77(6) 1.80(6) 2.574(4) 180(8) .
