#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:17:42 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223747 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/01/7700188.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_7700188
loop_
_publ_author_name
'Gupta, Anand'
'Deka, Rajesh'
'Sarkar, Arup'
'Singh, Harkesh B.'
'Butcher, Ray J.'
_publ_section_title
;
 Oxidation behavior of intramolecularly coordinated unsymmetrical
 diorganotellurides: isolation of novel tetraorganoditelluronic acids,
 [RR'Te(μ-O)(OH)₂]₂.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10979
_journal_page_last               10985
_journal_paper_doi               10.1039/c9dt01926j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H46 N2 O6 Te2'
_chemical_formula_sum            'C34 H46 N2 O6 Te2'
_chemical_formula_weight         833.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-11 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                103.832(2)
_cell_angle_beta                 114.891(2)
_cell_angle_gamma                91.144(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3292(2)
_cell_length_b                   9.5482(2)
_cell_length_c                   10.8122(2)
_cell_measurement_reflns_used    12351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1850
_cell_measurement_theta_min      2.4220
_cell_volume                     840.33(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxt (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18117
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         31.193
_diffrn_reflns_theta_min         2.430
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0336P)²+0.4222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4501
_reflns_number_total             4956
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01926j2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7700187--7700190.cif.'
_cod_database_code               7700188
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Te Te 0.15306(2) 0.09476(2) 0.61770(2) 0.01911(6) Uani 1 1 d . .
O1 O 0.0720(2) 0.25154(18) 0.53205(18) 0.0243(4) Uani 1 1 d . .
H1 H 0.1095 0.3319 0.5939 0.036 Uiso 1 1 calc R U
O2 O 0.2095(2) -0.07637(18) 0.68810(18) 0.0252(4) Uani 1 1 d . .
H2 H 0.1476 -0.1505 0.6277 0.038 Uiso 1 1 calc R U
O3 O 0.07143(19) -0.03138(18) 0.42479(17) 0.0210(3) Uani 1 1 d . .
N1 N 0.2042(3) 0.5056(2) 0.7127(2) 0.0251(4) Uani 1 1 d . .
C1 C 0.1791(3) 0.2185(3) 0.8228(2) 0.0223(5) Uani 1 1 d . .
C2 C 0.1192(3) 0.1405(3) 0.8884(3) 0.0280(5) Uani 1 1 d . .
H2A H 0.0730 0.0417 0.8423 0.034 Uiso 1 1 calc R U
C3 C 0.1262(3) 0.2054(4) 1.0198(3) 0.0361(6) Uani 1 1 d . .
H3A H 0.0859 0.1511 1.0641 0.043 Uiso 1 1 calc R U
C4 C 0.1915(3) 0.3487(3) 1.0863(3) 0.0357(6) Uani 1 1 d . .
H4A H 0.1960 0.3937 1.1765 0.043 Uiso 1 1 calc R U
C5 C 0.2506(3) 0.4270(3) 1.0219(3) 0.0309(6) Uani 1 1 d . .
H5A H 0.2955 0.5259 1.0690 0.037 Uiso 1 1 calc R U
C6 C 0.2462(3) 0.3649(3) 0.8895(2) 0.0226(5) Uani 1 1 d . .
C7 C 0.3209(3) 0.4580(3) 0.8311(3) 0.0248(5) Uani 1 1 d . .
H7A H 0.3866 0.5451 0.9082 0.030 Uiso 1 1 calc R U
H7B H 0.3929 0.4021 0.7989 0.030 Uiso 1 1 calc R U
C9 C 0.1017(4) 0.5990(3) 0.7554(3) 0.0364(6) Uani 1 1 d . .
H9A H 0.0464 0.5468 0.7941 0.055 Uiso 1 1 calc R U
H9B H 0.0231 0.6253 0.6730 0.055 Uiso 1 1 calc R U
H9C H 0.1669 0.6875 0.8280 0.055 Uiso 1 1 calc R U
C10 C 0.2870(4) 0.5797(3) 0.6526(3) 0.0372(6) Uani 1 1 d . .
H10A H 0.3506 0.5134 0.6201 0.056 Uiso 1 1 calc R U
H10B H 0.3573 0.6660 0.7251 0.056 Uiso 1 1 calc R U
H10C H 0.2085 0.6093 0.5723 0.056 Uiso 1 1 calc R U
C11 C 0.3913(3) 0.1429(3) 0.6402(3) 0.0224(5) Uani 1 1 d . .
C12 C 0.5245(3) 0.1397(3) 0.7666(3) 0.0263(5) Uani 1 1 d . .
C13 C 0.6763(3) 0.1807(3) 0.7814(3) 0.0344(6) Uani 1 1 d . .
H13A H 0.7664 0.1806 0.8665 0.041 Uiso 1 1 calc R U
C14 C 0.6999(4) 0.2211(3) 0.6770(4) 0.0407(7) Uani 1 1 d . .
H14A H 0.8046 0.2500 0.6904 0.049 Uiso 1 1 calc R U
C15 C 0.5703(4) 0.2193(3) 0.5531(3) 0.0376(7) Uani 1 1 d . .
H15A H 0.5873 0.2442 0.4799 0.045 Uiso 1 1 calc R U
C16 C 0.4148(3) 0.1823(3) 0.5309(3) 0.0276(5) Uani 1 1 d . .
C17 C 0.5173(3) 0.0936(3) 0.8882(3) 0.0352(6) Uani 1 1 d . .
H17A H 0.6251 0.0856 0.9553 0.053 Uiso 1 1 calc R U
H17B H 0.4504 -0.0010 0.8518 0.053 Uiso 1 1 calc R U
H17C H 0.4715 0.1662 0.9363 0.053 Uiso 1 1 calc R U
C18 C 0.2846(4) 0.1848(3) 0.3894(3) 0.0348(6) Uani 1 1 d . .
H18A H 0.3300 0.1819 0.3220 0.052 Uiso 1 1 calc R U
H18B H 0.2359 0.2742 0.4003 0.052 Uiso 1 1 calc R U
H18C H 0.2032 0.1001 0.3538 0.052 Uiso 1 1 calc R U
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
O1 Te O3 86.56(7) . .
O1 Te O2 173.11(7) . .
O3 Te O2 88.83(7) . .
O1 Te O3 86.67(7) . 2_556
O3 Te O3 78.08(7) . 2_556
O2 Te O3 87.37(7) . 2_556
O1 Te C1 92.59(8) . .
O3 Te C1 164.58(8) . .
O2 Te C1 90.49(8) . .
O3 Te C1 86.50(8) 2_556 .
O1 Te C11 94.37(8) . .
O3 Te C11 94.97(8) . .
O2 Te C11 91.12(8) . .
O3 Te C11 172.91(7) 2_556 .
C1 Te C11 100.45(9) . .
O1 Te Te 85.64(5) . 2_556
O3 Te Te 39.53(5) . 2_556
O2 Te Te 87.54(5) . 2_556
O3 Te Te 38.55(5) 2_556 2_556
C1 Te Te 125.05(6) . 2_556
C11 Te Te 134.48(6) . 2_556
Te O1 H1 109.5 . .
Te O2 H2 109.5 . .
Te O3 Te 101.92(7) . 2_556
C9 N1 C10 110.8(2) . .
C9 N1 C7 111.9(2) . .
C10 N1 C7 109.7(2) . .
C2 C1 C6 120.1(2) . .
C2 C1 Te 113.93(18) . .
C6 C1 Te 125.98(18) . .
C3 C2 C1 120.6(3) . .
C3 C2 H2A 119.7 . .
C1 C2 H2A 119.7 . .
C4 C3 C2 119.9(3) . .
C4 C3 H3A 120.1 . .
C2 C3 H3A 120.1 . .
C3 C4 C5 119.9(3) . .
C3 C4 H4A 120.1 . .
C5 C4 H4A 120.1 . .
C4 C5 C6 121.8(3) . .
C4 C5 H5A 119.1 . .
C6 C5 H5A 119.1 . .
C5 C6 C1 117.7(2) . .
C5 C6 C7 117.7(2) . .
C1 C6 C7 124.6(2) . .
N1 C7 C6 113.7(2) . .
N1 C7 H7A 108.8 . .
C6 C7 H7A 108.8 . .
N1 C7 H7B 108.8 . .
C6 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N1 C10 H10A 109.5 . .
N1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 C16 119.9(2) . .
C12 C11 Te 119.74(18) . .
C16 C11 Te 120.30(18) . .
C13 C12 C11 118.2(3) . .
C13 C12 C17 116.2(2) . .
C11 C12 C17 125.5(2) . .
C14 C13 C12 122.2(3) . .
C14 C13 H13A 118.9 . .
C12 C13 H13A 118.9 . .
C15 C14 C13 119.1(3) . .
C15 C14 H14A 120.4 . .
C13 C14 H14A 120.4 . .
C14 C15 C16 122.3(3) . .
C14 C15 H15A 118.9 . .
C16 C15 H15A 118.9 . .
C15 C16 C11 118.3(3) . .
C15 C16 C18 116.3(2) . .
C11 C16 C18 125.5(2) . .
C12 C17 H17A 109.5 . .
C12 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C12 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te O1 1.9466(16) .
Te O3 1.9509(16) .
Te O2 1.9540(16) .
Te O3 1.9925(16) 2_556
Te C1 2.158(2) .
Te C11 2.159(2) .
Te Te 3.0629(3) 2_556
O1 H1 0.8400 .
O2 H2 0.8400 .
O3 Te 1.9924(16) 2_556
N1 C9 1.460(3) .
N1 C10 1.463(3) .
N1 C7 1.468(3) .
C1 C2 1.393(3) .
C1 C6 1.403(3) .
C2 C3 1.380(4) .
C2 H2A 0.9500 .
C3 C4 1.373(4) .
C3 H3A 0.9500 .
C4 C5 1.380(4) .
C4 H4A 0.9500 .
C5 C6 1.394(3) .
C5 H5A 0.9500 .
C6 C7 1.513(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.416(3) .
C11 C16 1.419(3) .
C12 C13 1.393(4) .
C12 C17 1.509(4) .
C13 C14 1.374(4) .
C13 H13A 0.9500 .
C14 C15 1.372(5) .
C14 H14A 0.9500 .
C15 C16 1.390(4) .
C15 H15A 0.9500 .
C16 C18 1.508(4) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
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
O1 H1 N1 0.84 1.77 2.609(3) 172.3 .
O2 H2 O1 0.84 2.06 2.831(2) 151.8 2_556
C9 H9B O1 0.98 2.59 3.507(3) 155.5 2_566
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
C6 C1 C2 C3 -0.6(4)
Te C1 C2 C3 -179.5(2)
C1 C2 C3 C4 0.6(4)
C2 C3 C4 C5 -0.3(4)
C3 C4 C5 C6 0.0(4)
C4 C5 C6 C1 0.0(4)
C4 C5 C6 C7 -177.3(2)
C2 C1 C6 C5 0.3(3)
Te C1 C6 C5 179.11(18)
C2 C1 C6 C7 177.3(2)
Te C1 C6 C7 -3.9(3)
C9 N1 C7 C6 63.2(3)
C10 N1 C7 C6 -173.3(2)
C5 C6 C7 N1 -107.9(3)
C1 C6 C7 N1 75.1(3)
C16 C11 C12 C13 2.1(4)
Te C11 C12 C13 -175.82(18)
C16 C11 C12 C17 -177.1(2)
Te C11 C12 C17 5.0(3)
C11 C12 C13 C14 -1.1(4)
C17 C12 C13 C14 178.2(3)
C12 C13 C14 C15 -0.9(4)
C13 C14 C15 C16 2.1(5)
C14 C15 C16 C11 -1.1(4)
C14 C15 C16 C18 -179.9(3)
C12 C11 C16 C15 -1.0(4)
Te C11 C16 C15 176.86(19)
C12 C11 C16 C18 177.6(2)
Te C11 C16 C18 -4.5(3)
