#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:30:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180224 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111014.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111014
loop_
_publ_author_name
'Schatte, Gabriele'
'Chivers, Tristram'
'Jaska, Cory'
'Sandblom, Nicole'
_publ_section_title
;
 Cycloaddition reaction of tert-butyl isocyanate and a tellurium diimide
 dimer: extended helical structure of the ureato telluroxide
 {[OC(μ-NBut)2TeO]2(thf)}∞
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1657
_journal_paper_doi               10.1039/b004137h
_journal_year                    2000
_chemical_formula_moiety         'C18 H36 N4 O4 Te2, C4 H8 O'
_chemical_formula_sum            'C22 H44 N4 O5 Te2'
_chemical_formula_weight         699.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5941(7)
_cell_length_b                   15.5941(7)
_cell_length_c                   12.4867(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    193(2)
_cell_volume                     3036.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (1.05) in WinGX-1.62'
_computing_publication_material  WinGX-1.62
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13101
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_T_max  0.7580
_exptl_absorpt_correction_T_min  0.6304
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, V 2.01, Software for Area-Detector Absorption
  Corrections; Bruker AXS Inc., Madison, WI, 2000. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2593
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0164
_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)+(0.0250P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                2410
_reflns_number_total             2593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004137hsup1.cif
_cod_data_source_block           cal9972
_cod_database_code               7111014
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -z+1/2'
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
Te1 Te 0.380993(9) 0.248016(11) 0.041491(13) 0.03481(6) Uani 1 1 d . . .
O1 O 0.31073(14) 0.03641(13) 0.16748(17) 0.0520(6) Uani 1 1 d . . .
O2 O 0.29835(12) 0.32649(12) 0.09620(15) 0.0392(4) Uani 1 1 d . . .
N1 N 0.36600(16) 0.17490(15) 0.18026(18) 0.0442(6) Uani 1 1 d . . .
N2 N 0.31574(14) 0.13582(13) 0.02493(17) 0.0352(5) Uani 1 1 d . . .
C1 C 0.32907(18) 0.10736(19) 0.1316(2) 0.0402(7) Uani 1 1 d . . .
C10 C 0.3814(2) 0.1843(2) 0.2970(3) 0.0539(8) Uani 1 1 d . . .
C11 C 0.4435(3) 0.1157(2) 0.3347(3) 0.0738(11) Uani 1 1 d . . .
H11A H 0.4207 0.0590 0.3166 0.089 Uiso 1 1 calc R . .
H11B H 0.4508 0.1201 0.4125 0.089 Uiso 1 1 calc R . .
H11C H 0.4990 0.1239 0.2995 0.089 Uiso 1 1 calc R . .
C12 C 0.2974(3) 0.1787(4) 0.3572(3) 0.0939(15) Uani 1 1 d . . .
H12A H 0.2586 0.2238 0.3320 0.113 Uiso 1 1 calc R . .
H12B H 0.3080 0.1861 0.4340 0.113 Uiso 1 1 calc R . .
H12C H 0.2712 0.1225 0.3446 0.113 Uiso 1 1 calc R . .
C13 C 0.4211(3) 0.2721(2) 0.3140(3) 0.0859(14) Uani 1 1 d . . .
H13A H 0.4740 0.2767 0.2719 0.103 Uiso 1 1 calc R . .
H13B H 0.4344 0.2799 0.3901 0.103 Uiso 1 1 calc R . .
H13C H 0.3806 0.3165 0.2909 0.103 Uiso 1 1 calc R . .
C20 C 0.30551(18) 0.07358(17) -0.0662(2) 0.0368(6) Uani 1 1 d . . .
C21 C 0.38383(18) 0.01592(18) -0.0733(2) 0.0434(7) Uani 1 1 d . . .
H21A H 0.4350 0.0510 -0.0861 0.052 Uiso 1 1 calc R . .
H21B H 0.3765 -0.0248 -0.1324 0.052 Uiso 1 1 calc R . .
H21C H 0.3905 -0.0157 -0.0060 0.052 Uiso 1 1 calc R . .
C22 C 0.22514(17) 0.0208(2) -0.0448(3) 0.0516(8) Uani 1 1 d . . .
H22A H 0.2335 -0.0139 0.0198 0.062 Uiso 1 1 calc R . .
H22B H 0.2141 -0.0169 -0.1060 0.062 Uiso 1 1 calc R . .
H22C H 0.1762 0.0593 -0.0345 0.062 Uiso 1 1 calc R . .
C23 C 0.2940(2) 0.12392(19) -0.1701(2) 0.0448(7) Uani 1 1 d . . .
H23A H 0.2443 0.1620 -0.1636 0.054 Uiso 1 1 calc R . .
H23B H 0.2848 0.0839 -0.2295 0.054 Uiso 1 1 calc R . .
H23C H 0.3455 0.1582 -0.1839 0.054 Uiso 1 1 calc R . .
O1S O 0.4138(4) 0.4733(5) -0.0528(6) 0.135(3) Uani 0.50 1 d PDU A -1
C1S C 0.4959(8) 0.4486(11) -0.0854(11) 0.101(5) Uani 0.50 1 d PDU A -1
H11S H 0.5193 0.4894 -0.1385 0.122 Uiso 0.50 1 calc PR A -1
H12S H 0.4950 0.3905 -0.1172 0.122 Uiso 0.50 1 calc PR A -1
C2S C 0.5498(9) 0.4499(9) 0.0196(11) 0.125(5) Uani 0.50 1 d PDU A -1
H21S H 0.5615 0.3907 0.0445 0.150 Uiso 0.50 1 calc PR A -1
H22S H 0.6051 0.4796 0.0080 0.150 Uiso 0.50 1 calc PR A -1
C3S C 0.4984(10) 0.4953(12) 0.0965(12) 0.132(5) Uani 0.50 1 d PDU A -1
H31S H 0.5323 0.5412 0.1314 0.158 Uiso 0.50 1 calc PR A -1
H32S H 0.4767 0.4558 0.1523 0.158 Uiso 0.50 1 calc PR A -1
C4S C 0.4230(7) 0.5341(9) 0.0307(11) 0.095(4) Uani 0.50 1 d PDU A -1
H41S H 0.3702 0.5384 0.0743 0.114 Uiso 0.50 1 calc PR A -1
H42S H 0.4378 0.5915 0.0023 0.114 Uiso 0.50 1 calc PR A -1
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'
N N 0.0061 0.0033 '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'
Te Te -0.5308 1.6751 '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
O2 Te1 N2 104.52(9) . .
O2 Te1 O2 77.10(8) . 6
N2 Te1 O2 92.08(8) . 6
O2 Te1 N1 88.71(9) . .
N2 Te1 N1 63.81(9) . .
O2 Te1 N1 148.18(9) 6 .
O2 Te1 C1 100.16(8) . .
N2 Te1 C1 32.98(9) . .
O2 Te1 C1 123.51(8) 6 .
N1 Te1 C1 31.05(9) . .
O2 Te1 Te1 40.51(5) . 6
N2 Te1 Te1 101.89(6) . 6
O2 Te1 Te1 36.65(5) 6 6
N1 Te1 Te1 124.48(7) . 6
C1 Te1 Te1 120.00(6) . 6
Te1 O2 Te1 102.84(8) . 6
C1 N1 C10 126.2(3) . .
C1 N1 Te1 95.79(17) . .
C10 N1 Te1 138.0(2) . .
C1 N2 C20 121.6(2) . .
C1 N2 Te1 95.76(17) . .
C20 N2 Te1 133.23(17) . .
O1 C1 N1 129.9(3) . .
O1 C1 N2 126.2(3) . .
N1 C1 N2 104.0(2) . .
O1 C1 Te1 173.2(2) . .
N1 C1 Te1 53.16(14) . .
N2 C1 Te1 51.27(13) . .
N1 C10 C12 110.0(3) . .
N1 C10 C13 107.0(3) . .
C12 C10 C13 109.6(3) . .
N1 C10 C11 109.8(3) . .
C12 C10 C11 110.9(3) . .
C13 C10 C11 109.4(3) . .
N2 C20 C21 109.9(2) . .
N2 C20 C22 107.7(2) . .
C21 C20 C22 110.6(2) . .
N2 C20 C23 108.9(2) . .
C21 C20 C23 110.4(2) . .
C22 C20 C23 109.3(2) . .
C1S O1S C4S 107.8(8) . .
O1S C1S C2S 104.2(10) . .
C3S C2S C1S 105.6(8) . .
C2S C3S C4S 105.0(9) . .
O1S C4S C3S 101.8(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 O2 1.9040(17) .
Te1 N2 2.034(2) .
Te1 O2 2.0723(18) 6
Te1 N1 2.087(2) .
Te1 C1 2.595(3) .
Te1 Te1 3.1103(3) 6
O1 C1 1.227(3) .
O2 Te1 2.0723(18) 6
N1 C1 1.345(4) .
N1 C10 1.485(4) .
N2 C1 1.420(3) .
N2 C20 1.504(3) .
C10 C12 1.513(5) .
C10 C13 1.517(5) .
C10 C11 1.517(4) .
C20 C21 1.519(4) .
C20 C22 1.523(4) .
C20 C23 1.527(4) .
O1S C1S 1.397(12) .
O1S C4S 1.417(10) .
C1S C2S 1.558(14) .
C2S C3S 1.437(18) .
C3S C4S 1.557(14) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N2 Te1 O2 Te1 -91.41(10) . 6
O2 Te1 O2 Te1 -2.61(11) 6 6
N1 Te1 O2 Te1 -153.90(10) . 6
C1 Te1 O2 Te1 -124.90(9) . 6
O2 Te1 N1 C1 112.32(18) . .
N2 Te1 N1 C1 5.43(16) . .
O2 Te1 N1 C1 49.7(3) 6 .
Te1 Te1 N1 C1 92.03(17) 6 .
O2 Te1 N1 C10 -64.4(3) . .
N2 Te1 N1 C10 -171.3(3) . .
O2 Te1 N1 C10 -127.0(3) 6 .
C1 Te1 N1 C10 -176.7(4) . .
Te1 Te1 N1 C10 -84.7(3) 6 .
O2 Te1 N2 C1 -86.32(16) . .
O2 Te1 N2 C1 -163.53(16) 6 .
N1 Te1 N2 C1 -5.14(15) . .
Te1 Te1 N2 C1 -127.90(15) 6 .
O2 Te1 N2 C20 128.9(2) . .
O2 Te1 N2 C20 51.7(2) 6 .
N1 Te1 N2 C20 -149.9(3) . .
C1 Te1 N2 C20 -144.8(3) . .
Te1 Te1 N2 C20 87.3(2) 6 .
C10 N1 C1 O1 -10.5(5) . .
Te1 N1 C1 O1 172.2(3) . .
C10 N1 C1 N2 170.1(3) . .
Te1 N1 C1 N2 -7.2(2) . .
C10 N1 C1 Te1 177.3(3) . .
C20 N2 C1 O1 -21.6(4) . .
Te1 N2 C1 O1 -172.0(3) . .
C20 N2 C1 N1 157.9(2) . .
Te1 N2 C1 N1 7.4(2) . .
C20 N2 C1 Te1 150.5(3) . .
O2 Te1 C1 N1 -69.98(18) . .
N2 Te1 C1 N1 -171.0(3) . .
O2 Te1 C1 N1 -151.16(16) 6 .
Te1 Te1 C1 N1 -107.95(16) 6 .
O2 Te1 C1 N2 101.04(16) . .
O2 Te1 C1 N2 19.87(19) 6 .
N1 Te1 C1 N2 171.0(3) . .
Te1 Te1 C1 N2 63.08(17) 6 .
C1 N1 C10 C12 -58.8(4) . .
Te1 N1 C10 C12 117.2(4) . .
C1 N1 C10 C13 -177.8(3) . .
Te1 N1 C10 C13 -1.9(5) . .
C1 N1 C10 C11 63.5(4) . .
Te1 N1 C10 C11 -120.5(3) . .
C1 N2 C20 C21 -57.8(3) . .
Te1 N2 C20 C21 79.9(3) . .
C1 N2 C20 C22 62.7(3) . .
Te1 N2 C20 C22 -159.6(2) . .
C1 N2 C20 C23 -178.9(2) . .
Te1 N2 C20 C23 -41.2(3) . .
C4S O1S C1S C2S 34.8(13) . .
O1S C1S C2S C3S -13.9(18) . .
C1S C2S C3S C4S -9.9(19) . .
C1S O1S C4S C3S -40.6(12) . .
C2S C3S C4S O1S 30.0(17) . .
