#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:29:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179143 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/04/4310476.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_4310476
loop_
_publ_author_name
'Christopher A. Dodds'
'Alan R. Kennedy'
'John Reglinski'
'Mark D. Spicer'
_publ_section_title
;
 Pushing the Frontiers of Hard and Soft Scorpionate Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              394
_journal_page_last               395
_journal_paper_doi               10.1021/ic035167i
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 B2 N12 S6 Te1'
_chemical_formula_sum            'C26 H34 B2 Cl6 N12 S6 Te'
_chemical_formula_weight         1068.93
_chemical_name_common            Te(Tm)2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-08-07T12:47:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.6840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1347(2)
_cell_length_b                   19.4830(3)
_cell_length_c                   15.2672(3)
_cell_measurement_reflns_used    14876
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     4334.21(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0489773
_diffrn_orient_matrix_UB_12      0.0107306
_diffrn_orient_matrix_UB_13      -0.0306689
_diffrn_orient_matrix_UB_21      -0.0286564
_diffrn_orient_matrix_UB_22      -0.0328225
_diffrn_orient_matrix_UB_23      -0.0499674
_diffrn_orient_matrix_UB_31      -0.0386041
_diffrn_orient_matrix_UB_32      0.0379787
_diffrn_orient_matrix_UB_33      -0.0345182
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32215
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.079
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0319P)²+8.5439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                7333
_reflns_number_total             9553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035167isi20031008_095828.cif
_cod_data_source_block           '[Te(Tm)2].2CHCl3'
_cod_database_code               4310476
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'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_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
C12 C 0.0904(3) 0.1513(3) 0.6922(3) 0.0484(12) Uani 1 1 d . . .
H12A H 0.1127 0.1987 0.6996 0.073 Uiso 1 1 calc R . .
H12B H 0.1328 0.1218 0.7363 0.073 Uiso 1 1 calc R . .
H12C H 0.0294 0.149 0.7027 0.073 Uiso 1 1 calc R . .
C17 C 0.3329(2) 0.05305(19) 0.0316(2) 0.0253(8) Uani 1 1 d . . .
C18 C 0.4534(2) 0.1032(2) 0.0031(3) 0.0317(9) Uani 1 1 d . . .
H18 H 0.4897 0.1314 -0.0242 0.038 Uiso 1 1 calc R . .
C19 C 0.4853(3) 0.0611(2) 0.0740(3) 0.0343(9) Uani 1 1 d . . .
H19 H 0.5478 0.054 0.1061 0.041 Uiso 1 1 calc R . .
C20 C 0.4144(3) -0.0165(2) 0.1676(3) 0.0404(10) Uani 1 1 d . . .
H20A H 0.4405 0.0077 0.225 0.061 Uiso 1 1 calc R . .
H20B H 0.4531 -0.0561 0.1634 0.061 Uiso 1 1 calc R . .
H20C H 0.3524 -0.0324 0.1653 0.061 Uiso 1 1 calc R . .
C23 C 0.3886(3) 0.1767(3) -0.2981(3) 0.0507(12) Uani 1 1 d . . .
H23 H 0.4134 0.2037 -0.3376 0.061 Uiso 1 1 calc R . .
C24 C 0.3770(3) 0.0651(3) -0.3828(3) 0.0518(13) Uani 1 1 d . . .
H24A H 0.3482 0.0203 -0.3799 0.078 Uiso 1 1 calc R . .
H24B H 0.4422 0.0586 -0.3783 0.078 Uiso 1 1 calc R . .
H24C H 0.347 0.0875 -0.4406 0.078 Uiso 1 1 calc R . .
C25 C -0.0250(3) 0.3532(2) 0.3374(3) 0.0344(9) Uani 1 1 d . . .
H25 H -0.0108 0.3078 0.3686 0.041 Uiso 1 1 calc R . .
C26 C 0.2033(4) 0.3563(3) 0.6293(4) 0.0703(17) Uani 1 1 d . . .
H26 H 0.1632 0.3205 0.5914 0.084 Uiso 1 1 calc R . .
N9 N 0.35851(19) 0.09867(16) -0.0236(2) 0.0261(7) Uani 1 1 d . . .
N10 N 0.4104(2) 0.03001(16) 0.0914(2) 0.0293(7) Uani 1 1 d . . .
S5 S 0.22349(7) 0.02551(5) 0.02538(6) 0.0290(2) Uani 1 1 d . . .
Cl1 Cl -0.06590(9) 0.40902(7) 0.40751(8) 0.0579(3) Uani 1 1 d . . .
Cl2 Cl 0.07588(7) 0.38667(6) 0.31742(8) 0.0459(3) Uani 1 1 d . . .
Cl3 Cl -0.10982(7) 0.34155(6) 0.23368(7) 0.0400(2) Uani 1 1 d . . .
Cl4 Cl 0.20722(14) 0.34108(10) 0.74458(13) 0.0985(6) Uani 1 1 d . . .
Cl5 Cl 0.31273(13) 0.34897(11) 0.61284(14) 0.1001(6) Uani 1 1 d . . .
Cl6 Cl 0.15363(15) 0.43553(9) 0.59733(15) 0.1213(8) Uani 1 1 d . . .
H1A H -0.025 0.1867 0.3317 0.013(8) Uiso 1 1 d . . .
H2A H 0.2279 0.1178 -0.1189 0.014(8) Uiso 1 1 d . . .
C1 C 0.0715(2) 0.05447(18) 0.2443(2) 0.0239(7) Uani 1 1 d . . .
C2 C -0.0677(2) 0.0619(2) 0.2633(3) 0.0307(8) Uani 1 1 d . . .
H2 H -0.1182 0.0768 0.2843 0.037 Uiso 1 1 calc R . .
C3 C -0.0691(3) 0.0099(2) 0.2049(3) 0.0317(9) Uani 1 1 d . . .
H3 H -0.1203 -0.0181 0.1766 0.038 Uiso 1 1 calc R . .
C4 C 0.0476(3) -0.0452(2) 0.1369(3) 0.0385(10) Uani 1 1 d . . .
H4A H 0.0508 -0.0233 0.08 0.058 Uiso 1 1 calc R . .
H4B H 0.0036 -0.0832 0.1232 0.058 Uiso 1 1 calc R . .
H4C H 0.1083 -0.0629 0.1691 0.058 Uiso 1 1 calc R . .
C5 C 0.1383(2) 0.22661(18) 0.2746(2) 0.0242(8) Uani 1 1 d . . .
C6 C 0.2040(3) 0.2056(2) 0.4196(3) 0.0331(9) Uani 1 1 d . . .
H6 H 0.214 0.189 0.48 0.04 Uiso 1 1 calc R . .
C7 C 0.2628(3) 0.2446(2) 0.3884(3) 0.0382(10) Uani 1 1 d . . .
H7 H 0.3216 0.2601 0.4224 0.046 Uiso 1 1 calc R . .
C8 C 0.2587(3) 0.3004(2) 0.2388(3) 0.0418(11) Uani 1 1 d . . .
H8A H 0.2501 0.2775 0.1799 0.063 Uiso 1 1 calc R . .
H8B H 0.3244 0.3079 0.2666 0.063 Uiso 1 1 calc R . .
H8C H 0.2268 0.3447 0.2297 0.063 Uiso 1 1 calc R . .
C9 C 0.0491(2) 0.1655(2) 0.5243(2) 0.0289(8) Uani 1 1 d . . .
C10 C 0.1006(3) 0.0658(2) 0.4858(3) 0.0382(10) Uani 1 1 d . . .
H10 H 0.1157 0.0299 0.4504 0.046 Uiso 1 1 calc R . .
C11 C 0.1173(3) 0.0664(2) 0.5766(3) 0.0417(10) Uani 1 1 d . . .
H11 H 0.146 0.0309 0.6171 0.05 Uiso 1 1 calc R . .
C13 C 0.2150(2) 0.24642(19) -0.0481(2) 0.0264(8) Uani 1 1 d . . .
C14 C 0.3646(3) 0.2597(2) -0.0295(3) 0.0324(9) Uani 1 1 d . . .
H14 H 0.4263 0.251 -0.0299 0.039 Uiso 1 1 calc R . .
C15 C 0.3341(3) 0.3162(2) 0.0036(3) 0.0358(9) Uani 1 1 d . . .
H15 H 0.3701 0.3546 0.0303 0.043 Uiso 1 1 calc R . .
C16 C 0.1811(3) 0.3572(2) 0.0183(3) 0.0429(11) Uani 1 1 d . . .
H16A H 0.1408 0.3785 -0.0361 0.064 Uiso 1 1 calc R . .
H16B H 0.218 0.3927 0.057 0.064 Uiso 1 1 calc R . .
H16C H 0.1437 0.3334 0.0522 0.064 Uiso 1 1 calc R . .
C21 C 0.3330(2) 0.0871(2) -0.2375(2) 0.0293(8) Uani 1 1 d . . .
C22 C 0.3679(3) 0.1984(2) -0.2225(3) 0.0421(10) Uani 1 1 d . . .
H22 H 0.3755 0.2439 -0.1992 0.051 Uiso 1 1 calc R . .
B1 B 0.0397(3) 0.1539(2) 0.3540(3) 0.0254(9) Uiso 1 1 d . . .
B2 B 0.2933(3) 0.1416(2) -0.1009(3) 0.0264(9) Uiso 1 1 d . . .
N1 N 0.02001(19) 0.09028(15) 0.28793(19) 0.0245(6) Uani 1 1 d . . .
N2 N 0.0179(2) 0.00519(15) 0.1941(2) 0.0269(7) Uani 1 1 d . . .
N3 N 0.12656(19) 0.19411(16) 0.34828(19) 0.0255(7) Uani 1 1 d . . .
N4 N 0.2215(2) 0.25758(16) 0.2983(2) 0.0302(7) Uani 1 1 d . . .
N5 N 0.0574(2) 0.12712(16) 0.4525(2) 0.0292(7) Uani 1 1 d . . .
N6 N 0.0851(2) 0.12785(18) 0.6003(2) 0.0348(8) Uani 1 1 d . . .
N7 N 0.2904(2) 0.21607(16) -0.0632(2) 0.0277(7) Uani 1 1 d . . .
N8 N 0.2415(2) 0.30815(16) -0.0085(2) 0.0315(7) Uani 1 1 d . . .
N11 N 0.3336(2) 0.14318(16) -0.1843(2) 0.0291(7) Uani 1 1 d . . .
N12 N 0.3672(2) 0.10788(19) -0.3075(2) 0.0391(8) Uani 1 1 d . . .
S1 S 0.18474(6) 0.06910(5) 0.24607(6) 0.02527(19) Uani 1 1 d . . .
S2 S 0.06310(6) 0.22752(5) 0.16757(6) 0.0275(2) Uani 1 1 d . . .
S3 S 0.00613(7) 0.24617(6) 0.52323(7) 0.0369(2) Uani 1 1 d . . .
S4 S 0.10552(6) 0.21458(6) -0.06948(7) 0.0314(2) Uani 1 1 d . . .
S6 S 0.29723(7) 0.00648(5) -0.22169(6) 0.0303(2) Uani 1 1 d . . .
Te1 Te 0.148233(15) 0.131509(12) 0.091066(15) 0.02272(7) Uani 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 0 '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'
N N 0.0061 0.0033 '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'
Te Te -0.5308 1.6751 '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'
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
N9 C17 N10 107.2(3) . . ?
N9 C17 S5 127.3(3) . . ?
N10 C17 S5 125.5(3) . . ?
C19 C18 N9 108.5(4) . . ?
C18 C19 N10 106.9(3) . . ?
C22 C23 N12 107.1(4) . . ?
Cl1 C25 Cl2 110.0(2) . . ?
Cl1 C25 Cl3 109.7(2) . . ?
Cl2 C25 Cl3 110.3(2) . . ?
Cl6 C26 Cl5 112.9(4) . . ?
Cl6 C26 Cl4 109.0(3) . . ?
Cl5 C26 Cl4 110.5(3) . . ?
C17 N9 C18 108.0(3) . . ?
C17 N9 B2 126.5(3) . . ?
C18 N9 B2 125.5(3) . . ?
C17 N10 C19 109.5(3) . . ?
C17 N10 C20 125.7(3) . . ?
C19 N10 C20 124.6(3) . . ?
C17 S5 Te1 103.85(12) . . ?
N1 C1 N2 108.0(3) . . ?
N1 C1 S1 127.6(3) . . ?
N2 C1 S1 124.4(3) . . ?
C3 C2 N1 108.8(3) . . ?
C2 C3 N2 106.5(3) . . ?
N3 C5 N4 108.1(3) . . ?
N3 C5 S2 126.7(3) . . ?
N4 C5 S2 125.2(3) . . ?
C7 C6 N3 108.2(4) . . ?
C6 C7 N4 107.0(3) . . ?
N6 C9 N5 106.7(3) . . ?
N6 C9 S3 125.0(3) . . ?
N5 C9 S3 128.2(3) . . ?
C11 C10 N5 108.1(4) . . ?
C10 C11 N6 107.3(4) . . ?
N8 C13 N7 107.5(3) . . ?
N8 C13 S4 124.0(3) . . ?
N7 C13 S4 128.5(3) . . ?
C15 C14 N7 108.4(3) . . ?
C14 C15 N8 107.3(4) . . ?
N11 C21 N12 106.6(3) . . ?
N11 C21 S6 127.5(3) . . ?
N12 C21 S6 125.9(3) . . ?
C23 C22 N11 108.4(4) . . ?
N5 B1 N3 107.3(3) . . ?
N5 B1 N1 108.1(3) . . ?
N3 B1 N1 112.2(3) . . ?
N11 B2 N9 108.8(3) . . ?
N11 B2 N7 109.9(3) . . ?
N9 B2 N7 107.0(3) . . ?
C1 N1 C2 107.3(3) . . ?
C1 N1 B1 133.5(3) . . ?
C2 N1 B1 119.2(3) . . ?
C1 N2 C3 109.5(3) . . ?
C1 N2 C4 125.5(3) . . ?
C3 N2 C4 125.1(3) . . ?
C5 N3 C6 107.9(3) . . ?
C5 N3 B1 126.1(3) . . ?
C6 N3 B1 125.9(3) . . ?
C5 N4 C7 108.9(3) . . ?
C5 N4 C8 125.3(3) . . ?
C7 N4 C8 125.7(3) . . ?
C9 N5 C10 108.3(3) . . ?
C9 N5 B1 124.7(3) . . ?
C10 N5 B1 125.9(3) . . ?
C9 N6 C11 109.6(3) . . ?
C9 N6 C12 124.0(4) . . ?
C11 N6 C12 126.4(3) . . ?
C13 N7 C14 107.6(3) . . ?
C13 N7 B2 125.0(3) . . ?
C14 N7 B2 127.0(3) . . ?
C13 N8 C15 109.3(3) . . ?
C13 N8 C16 125.0(3) . . ?
C15 N8 C16 125.7(4) . . ?
C21 N11 C22 108.3(3) . . ?
C21 N11 B2 122.2(3) . . ?
C22 N11 B2 129.3(3) . . ?
C21 N12 C23 109.5(4) . . ?
C21 N12 C24 125.8(4) . . ?
C23 N12 C24 124.6(4) . . ?
C1 S1 Te1 95.60(12) . . ?
C5 S2 Te1 97.65(12) . . ?
C13 S4 Te1 93.36(12) . . ?
S1 Te1 S5 88.44(3) . . ?
S1 Te1 S2 86.50(3) . . ?
S5 Te1 S2 173.27(3) . . ?
S1 Te1 S4 173.44(3) . . ?
S5 Te1 S4 97.80(3) . . ?
S2 Te1 S4 87.43(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
C12 N6 1.457(5) . ?
C17 N9 1.351(5) . ?
C17 N10 1.354(5) . ?
C17 S5 1.718(4) . ?
C18 C19 1.341(5) . ?
C18 N9 1.385(5) . ?
C19 N10 1.372(5) . ?
C20 N10 1.463(5) . ?
C23 C22 1.343(6) . ?
C23 N12 1.377(6) . ?
C24 N12 1.459(5) . ?
C25 Cl1 1.752(4) . ?
C25 Cl2 1.761(4) . ?
C25 Cl3 1.763(4) . ?
C26 Cl6 1.728(5) . ?
C26 Cl5 1.747(6) . ?
C26 Cl4 1.770(7) . ?
N9 B2 1.562(5) . ?
S5 Te1 2.6805(10) . ?
C1 N1 1.349(5) . ?
C1 N2 1.353(4) . ?
C1 S1 1.730(4) . ?
C2 C3 1.346(5) . ?
C2 N1 1.393(5) . ?
C3 N2 1.374(5) . ?
C4 N2 1.464(5) . ?
C5 N3 1.343(5) . ?
C5 N4 1.355(5) . ?
C5 S2 1.721(4) . ?
C6 C7 1.351(6) . ?
C6 N3 1.385(4) . ?
C7 N4 1.371(5) . ?
C8 N4 1.455(5) . ?
C9 N6 1.356(4) . ?
C9 N5 1.362(5) . ?
C9 S3 1.698(4) . ?
C10 C11 1.341(6) . ?
C10 N5 1.390(5) . ?
C11 N6 1.378(5) . ?
C13 N8 1.357(5) . ?
C13 N7 1.359(5) . ?
C13 S4 1.716(4) . ?
C14 C15 1.344(6) . ?
C14 N7 1.391(5) . ?
C15 N8 1.372(5) . ?
C16 N8 1.457(5) . ?
C21 N11 1.360(5) . ?
C21 N12 1.369(4) . ?
C21 S6 1.700(4) . ?
C22 N11 1.390(5) . ?
B1 N5 1.546(5) . ?
B1 N3 1.553(5) . ?
B1 N1 1.575(5) . ?
B2 N11 1.553(5) . ?
B2 N7 1.566(5) . ?
S1 Te1 2.5841(9) . ?
S2 Te1 2.7088(10) . ?
S4 Te1 2.8616(10) . ?
