#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321341.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_4321341
loop_
_publ_author_name
'Gregory E. D. Mullen'
'Philip J. Blower'
'Daniel J. Price'
'Anne K. Powell'
'Mark J. Howard'
'Michael J. Went'
_publ_section_title
;
 Trithiacyclononane as a Ligand for Potential Technetium and Rhenium
 Radiopharmaceuticals: Synthesis of [M(9S3)(SC2H4SC2H4S)][BF4] (M =99Tc,
 Re, 188Re) via C-S Bond Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4093
_journal_page_last               4098
_journal_paper_doi               10.1021/ic991240m
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        gm
_chemical_formula_moiety         'Tc S6 C10 H20 B F4'
_chemical_formula_structural     'Tc [(SCH2CH2)3] [S(CH2CH2S)2] BF4'
_chemical_formula_sum            'C10 H20 B F4 S6 Tc'
_chemical_formula_weight         517.43
_chemical_melting_point          ?
_chemical_name_systematic
; Technetium(3+)[1,4,7-trithiacyclononane][2,2'-thiodiethanethiolate(2-)]
tetraflouroborate(-)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL + manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.233(2)
_cell_length_b                   14.341(2)
_cell_length_c                   20.726(3)
_cell_measurement_reflns_used    595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.62
_cell_volume                     3636.0(9)
_computing_cell_refinement
' Denzo and Scalepack from The HKL Programme Suite'
_computing_data_collection       'MSC Raxis II control software'
_computing_data_reduction        'SHELX97 and SHELXPRO'
_computing_molecular_graphics    SHELXTL+XP
_computing_publication_material  SHELXTL+XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku Raxis IIc''
_diffrn_measurement_method       'image plate oscilation photographs'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29143
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_type   none
_exptl_crystal_colour
;
Red in transmission - metallic-green in reflection
;
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0055(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.988
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_obs          0.0358
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0679P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0935
_refine_ls_wR_factor_obs         0.0876
_reflns_number_observed          4230
_reflns_number_total             5223
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991240m.cif
_cod_data_source_block           gm01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Orthorhombic' changed to 'orthorhombic' according to the built-in
table from CIF Core dictionary named 'cif_core.dic' version 2.4.1
from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321341
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tc1 Tc 0.376275(14) 0.257627(11) 0.464494(8) 0.03462(8) Uani 1 d . .
S1 S 0.27988(5) 0.40332(4) 0.43904(3) 0.04526(14) Uani 1 d . .
S2 S 0.25136(5) 0.19888(4) 0.37936(3) 0.04400(13) Uani 1 d . .
S3 S 0.49551(4) 0.29598(4) 0.37555(3) 0.04206(13) Uani 1 d . .
S4 S 0.42544(5) 0.10676(4) 0.47207(3) 0.04420(14) Uani 1 d . .
S5 S 0.25297(5) 0.23155(4) 0.54982(3) 0.04100(13) Uani 1 d . .
S6 S 0.47779(5) 0.34331(4) 0.53471(3) 0.04817(15) Uani 1 d . .
C1 C 0.1522(2) 0.3680(2) 0.40014(14) 0.0545(6) Uani 1 d . .
H11 H 0.1226(25) 0.4344(25) 0.3811(15) 0.075(10) Uiso 1 d . .
H12 H 0.1057(25) 0.3425(23) 0.4363(14) 0.062(8) Uiso 1 d . .
C2 C 0.1693(2) 0.2957(2) 0.34854(13) 0.0552(6) Uani 1 d . .
H21 H 0.2074(24) 0.3253(20) 0.3102(14) 0.062(8) Uiso 1 d . .
H22 H 0.0979(25) 0.2709(19) 0.3355(15) 0.056(8) Uiso 1 d . .
C3 C 0.3475(2) 0.1777(2) 0.31312(13) 0.0538(6) Uani 1 d . .
H31 H 0.2995(28) 0.1693(23) 0.2731(16) 0.078(10) Uiso 1 d . .
H32 H 0.3946(26) 0.1212(23) 0.3288(16) 0.072(9) Uiso 1 d . .
C4 C 0.4273(2) 0.2560(2) 0.30093(13) 0.0507(6) Uani 1 d . .
H41 H 0.3910(23) 0.3021(23) 0.2816(13) 0.054(8) Uiso 1 d . .
H42 H 0.4873(25) 0.2316(19) 0.2738(13) 0.053(8) Uiso 1 d . .
C5 C 0.4740(2) 0.4224(2) 0.36962(14) 0.0512(5) Uani 1 d . .
H51 H 0.5004(24) 0.4335(21) 0.3307(16) 0.067(9) Uiso 1 d . .
H52 H 0.5126(26) 0.4514(22) 0.4101(14) 0.071(9) Uiso 1 d . .
C6 C 0.3564(2) 0.4544(2) 0.37145(14) 0.0537(6) Uani 1 d . .
H61 H 0.3092(21) 0.4379(17) 0.3296(13) 0.051(7) Uiso 1 d . .
H62 H 0.3532(25) 0.5245(24) 0.3773(15) 0.072(9) Uiso 1 d . .
C7 C 0.3609(2) 0.0614(2) 0.54584(12) 0.0439(5) Uani 1 d . .
H71 H 0.4068(23) 0.0711(20) 0.5838(14) 0.056(7) Uiso 1 d . .
H72 H 0.3490(22) -0.0136(20) 0.5385(12) 0.047(7) Uiso 1 d . .
C8 C 0.2514(2) 0.10454(15) 0.55961(12) 0.0439(5) Uani 1 d . .
H81 H 0.2209(25) 0.0981(20) 0.6055(15) 0.067(9) Uiso 1 d . .
H82 H 0.1967(19) 0.0806(15) 0.5293(10) 0.032(5) Uiso 1 d . .
C9 C 0.3300(3) 0.2662(2) 0.62216(13) 0.0520(6) Uani 1 d . .
H91 H 0.3767(21) 0.2211(20) 0.6342(14) 0.045(7) Uiso 1 d . .
H92 H 0.2704(26) 0.2677(19) 0.6585(15) 0.061(8) Uiso 1 d . .
C10 C 0.3928(2) 0.3546(2) 0.60796(13) 0.0546(6) Uani 1 d . .
H101 H 0.4478(27) 0.3680(22) 0.6473(16) 0.073(10) Uiso 1 d . .
H102 H 0.3483(27) 0.4118(24) 0.6020(15) 0.072(9) Uiso 1 d . .
B1 B 0.6147(3) 0.0368(2) 0.29043(15) 0.0583(7) Uani 1 d . .
F1 F 0.5360(2) -0.0291(2) 0.29676(12) 0.1251(10) Uani 1 d . .
F2 F 0.6185(2) 0.08946(15) 0.34455(10) 0.1022(8) Uani 1 d . .
F3 F 0.5939(2) 0.09077(13) 0.23664(9) 0.0818(5) Uani 1 d . .
F4 F 0.7103(3) -0.0115(2) 0.28167(13) 0.1408(12) Uani 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
S4 Tc1 S6 109.20(3) . . ?
S4 Tc1 S5 88.06(2) . . ?
S6 Tc1 S5 87.42(2) . . ?
S4 Tc1 S3 96.36(2) . . ?
S6 Tc1 S3 92.04(2) . . ?
S5 Tc1 S3 175.47(2) . . ?
S4 Tc1 S1 163.89(2) . . ?
S6 Tc1 S1 86.56(2) . . ?
S5 Tc1 S1 89.36(2) . . ?
S3 Tc1 S1 86.12(2) . . ?
S4 Tc1 S2 83.55(2) . . ?
S6 Tc1 S2 167.13(2) . . ?
S5 Tc1 S2 94.91(2) . . ?
S3 Tc1 S2 84.63(2) . . ?
S1 Tc1 S2 80.82(2) . . ?
C1 S1 C6 102.10(13) . . ?
C1 S1 Tc1 105.59(9) . . ?
C6 S1 Tc1 104.96(8) . . ?
C2 S2 C3 102.50(13) . . ?
C2 S2 Tc1 109.19(9) . . ?
C3 S2 Tc1 101.17(9) . . ?
C5 S3 C4 100.70(13) . . ?
C5 S3 Tc1 100.93(9) . . ?
C4 S3 Tc1 107.18(9) . . ?
C7 S4 Tc1 106.46(8) . . ?
C8 S5 C9 100.58(12) . . ?
C8 S5 Tc1 104.35(8) . . ?
C9 S5 Tc1 103.97(10) . . ?
C10 S6 Tc1 105.42(9) . . ?
C2 C1 S1 112.7(2) . . ?
C1 C2 S2 110.6(2) . . ?
C4 C3 S2 114.6(2) . . ?
C3 C4 S3 112.5(2) . . ?
C6 C5 S3 115.7(2) . . ?
C5 C6 S1 112.6(2) . . ?
C8 C7 S4 113.2(2) . . ?
C7 C8 S5 112.3(2) . . ?
C10 C9 S5 109.2(2) . . ?
C9 C10 S6 111.9(2) . . ?
F2 B1 F1 109.5(3) . . ?
F2 B1 F4 111.3(3) . . ?
F1 B1 F4 105.4(3) . . ?
F2 B1 F3 111.3(3) . . ?
F1 B1 F3 109.8(3) . . ?
F4 B1 F3 109.5(3) . . ?
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 S4 2.2512(6) . ?
Tc1 S6 2.2738(6) . ?
Tc1 S5 2.3542(6) . ?
Tc1 S3 2.4142(6) . ?
Tc1 S1 2.4565(6) . ?
Tc1 S2 2.4815(6) . ?
S1 C1 1.829(3) . ?
S1 C6 1.837(3) . ?
S2 C2 1.828(3) . ?
S2 C3 1.833(3) . ?
S3 C5 1.836(2) . ?
S3 C4 1.849(3) . ?
S4 C7 1.840(2) . ?
S5 C8 1.833(2) . ?
S5 C9 1.839(3) . ?
S6 C10 1.847(3) . ?
C1 C2 1.504(4) . ?
C3 C4 1.509(4) . ?
C5 C6 1.510(4) . ?
C7 C8 1.503(3) . ?
C9 C10 1.511(4) . ?
B1 F2 1.353(4) . ?
B1 F1 1.355(4) . ?
B1 F4 1.372(4) . ?
B1 F3 1.381(3) . ?
