#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:52:03 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058143.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_7058143
loop_
_publ_author_name
'Shayapov, Vladimir R.'
'Usoltsev, Andrey N.'
'Adonin, Sergey A.'
'Sokolov, Maxim N.'
'Samsonenko, Denis G.'
'Fedin, Vladimir P.'
_publ_section_title
;
 Thermochromism of bromotellurates(iv): experimental insights
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3927
_journal_paper_doi               10.1039/C9NJ00320G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C14 H20.5 Br6 N2 O0.25 Te'
_chemical_formula_weight         827.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-11-12 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.188(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3224(4)
_cell_length_b                   13.0117(4)
_cell_length_c                   23.4808(7)
_cell_measurement_reflns_used    6114
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      3.94
_cell_volume                     4668.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12214
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.936
_diffrn_reflns_theta_min         3.398
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.356
_exptl_crystal_description       block
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0165P)²+30.3550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4778
_reflns_number_total             5127
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj00320g2.cif
_cod_data_source_block           AU289
_cod_depositor_comments
'Adding full bibliography for 7058143--7058147.cif.'
_cod_original_formula_sum        'C14 H20.50 Br6 N2 O0.25 Te'
_cod_database_code               7058143
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.124
_shelx_estimated_absorpt_t_max   0.160
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 1.000000 0.49076(3) 0.250000 0.01154(8) Uani 1 2 d S T P . .
Br11 Br 0.97613(3) 0.34076(3) 0.32628(2) 0.02105(10) Uani 1 1 d . . . . .
Br12 Br 0.99337(3) 0.63894(3) 0.32998(2) 0.01938(9) Uani 1 1 d . . . . .
Br13 Br 0.82523(3) 0.49581(3) 0.22732(2) 0.02134(10) Uani 1 1 d . . . . .
Te2 Te 0.500000 0.500000 0.500000 0.01464(8) Uani 1 2 d S . P . .
Br21 Br 0.44350(3) 0.64692(4) 0.56978(2) 0.02755(11) Uani 1 1 d . . . . .
Br22 Br 0.44088(3) 0.60718(4) 0.40648(2) 0.02953(11) Uani 1 1 d . . . . .
Br23 Br 0.65558(3) 0.59619(3) 0.49718(2) 0.02355(10) Uani 1 1 d . . . . .
N1 N 0.8475(2) 0.4701(3) 0.53771(15) 0.0129(7) Uani 0.5 1 d . . P A 1
C1 C 0.8475(2) 0.4701(3) 0.53771(15) 0.0129(7) Uani 0.5 1 d . . P A 2
C11 C 0.8193(3) 0.3579(4) 0.4543(2) 0.0288(10) Uani 1 1 d . . . . .
H11A H 0.836041 0.353782 0.414842 0.043 Uiso 1 1 calc R U . B 1
H11B H 0.755360 0.357671 0.454395 0.043 Uiso 1 1 calc R U . B 1
H11C H 0.843264 0.298584 0.475910 0.043 Uiso 1 1 calc R U . B 1
C12 C 0.8547(2) 0.4546(3) 0.48118(16) 0.0195(8) Uani 0.5 1 d . . P A 1
N12 N 0.8547(2) 0.4546(3) 0.48118(16) 0.0195(8) Uani 0.5 1 d . . P A 2
C13 C 0.8934(3) 0.5287(3) 0.44976(18) 0.0220(9) Uani 1 1 d . . . . .
H13 H 0.898937 0.517893 0.410177 0.026 Uiso 1 1 calc R U . A 1
C14 C 0.9241(3) 0.6186(4) 0.47508(19) 0.0231(9) Uani 1 1 d . . . . .
H14 H 0.949612 0.670303 0.453015 0.028 Uiso 1 1 calc R U . . .
C15 C 0.9174(3) 0.6326(3) 0.53304(19) 0.0217(9) Uani 1 1 d . . . . .
H15 H 0.939262 0.693409 0.551418 0.026 Uiso 1 1 calc R U . . .
C16 C 0.8787(3) 0.5573(3) 0.56361(17) 0.0184(8) Uani 1 1 d . . . . .
H16 H 0.873673 0.566450 0.603382 0.022 Uiso 1 1 calc R U . A 1
C17 C 0.8018(3) 0.3934(3) 0.57129(19) 0.0228(9) Uani 1 1 d . . . . .
H17A H 0.802194 0.416269 0.611078 0.034 Uiso 1 1 calc R U . A 1
H17B H 0.831791 0.327036 0.569722 0.034 Uiso 1 1 calc R U . A 1
H17C H 0.741237 0.386081 0.555339 0.034 Uiso 1 1 calc R U . A 1
N2 N 0.7630(3) 0.7571(3) 0.2615(2) 0.0312(10) Uani 0.5 1 d . . P C 1
C2 C 0.7630(3) 0.7571(3) 0.2615(2) 0.0312(10) Uani 0.5 1 d . . P C 2
C21 C 0.8884(3) 0.8718(5) 0.2740(3) 0.0426(14) Uani 1 1 d . . . . .
H21A H 0.860639 0.925231 0.249506 0.064 Uiso 1 1 calc R U . D 1
H21B H 0.925535 0.828719 0.251571 0.064 Uiso 1 1 calc R U . D 1
H21C H 0.924205 0.903986 0.305404 0.064 Uiso 1 1 calc R U . D 1
C22 C 0.8205(3) 0.8079(3) 0.29750(18) 0.0275(9) Uani 0.5 1 d . . P C 1
N22 N 0.8205(3) 0.8079(3) 0.29750(18) 0.0275(9) Uani 0.5 1 d . . P C 2
C23 C 0.8155(3) 0.8015(4) 0.3550(2) 0.0343(12) Uani 1 1 d . . . . .
H23 H 0.856692 0.837853 0.379541 0.041 Uiso 1 1 calc R U . C 1
C24 C 0.7531(3) 0.7444(4) 0.3780(2) 0.0367(13) Uani 1 1 d . . . . .
H24 H 0.750516 0.740454 0.418199 0.044 Uiso 1 1 calc R U . . .
C25 C 0.6936(4) 0.6922(4) 0.3420(3) 0.0405(13) Uani 1 1 d . . . . .
H25 H 0.649148 0.651888 0.357206 0.049 Uiso 1 1 calc R U . . .
C26 C 0.6988(4) 0.6989(4) 0.2834(2) 0.0362(12) Uani 1 1 d . . . . .
H26 H 0.657795 0.663081 0.258400 0.043 Uiso 1 1 calc R U . C 1
C27 C 0.7682(4) 0.7668(4) 0.1987(2) 0.0392(13) Uani 1 1 d . . . . .
H27A H 0.723012 0.723880 0.178974 0.059 Uiso 1 1 calc R U . C 1
H27B H 0.826037 0.744328 0.188480 0.059 Uiso 1 1 calc R U . C 1
H27C H 0.759001 0.838743 0.187409 0.059 Uiso 1 1 calc R U . C 1
O1W O 0.500000 0.5967(7) 0.250000 0.042(3) Uani 0.5 2 d S T P . .
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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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
Br11 Te1 Br11 87.06(2) . 2_755 yes
Br11 Te1 Br12 92.353(13) 2_755 2_755 ?
Br11 Te1 Br12 92.354(13) . . yes
Br11 Te1 Br12 174.195(13) . 2_755 yes
Br11 Te1 Br12 174.195(13) 2_755 . ?
Br11 Te1 Br13 88.156(14) 2_755 2_755 ?
Br11 Te1 Br13 88.157(14) . . yes
Br11 Te1 Br13 93.875(14) . 2_755 yes
Br11 Te1 Br13 93.874(15) 2_755 . ?
Br12 Te1 Br12 88.80(2) . 2_755 yes
Br13 Te1 Br12 86.120(14) . 2_755 yes
Br13 Te1 Br12 86.120(14) 2_755 . ?
Br13 Te1 Br12 91.878(14) 2_755 2_755 ?
Br13 Te1 Br12 91.879(14) . . yes
Br13 Te1 Br13 177.20(2) . 2_755 yes
Br21 Te2 Br21 180.0 . 5_666 yes
Br21 Te2 Br22 88.599(15) 5_666 . ?
Br21 Te2 Br22 88.599(16) . 5_666 yes
Br21 Te2 Br22 91.401(15) 5_666 5_666 ?
Br21 Te2 Br22 91.401(16) . . yes
Br22 Te2 Br22 180.0 5_666 . yes
Br23 Te2 Br21 89.459(14) 5_666 . ?
Br23 Te2 Br21 89.460(14) . 5_666 yes
Br23 Te2 Br21 90.541(14) . . yes
Br23 Te2 Br21 90.541(14) 5_666 5_666 ?
Br23 Te2 Br22 89.140(14) . . yes
Br23 Te2 Br22 89.141(14) 5_666 5_666 ?
Br23 Te2 Br22 90.859(14) 5_666 . ?
Br23 Te2 Br22 90.861(14) . 5_666 yes
Br23 Te2 Br23 180.0 5_666 . yes
C12 N1 C16 120.8(4) . . ?
C12 N1 C17 119.9(4) . . ?
C16 N1 C17 119.3(3) . . ?
N12 C1 C16 120.8(4) . . ?
N12 C1 C17 119.9(4) . . ?
C16 C1 C17 119.3(3) . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
N1 C12 C11 119.1(4) . . ?
N1 C12 C13 119.4(4) . . ?
C13 C12 C11 121.5(4) . . ?
C1 N12 C11 119.1(4) . . ?
C1 N12 C13 119.4(4) . . ?
C13 N12 C11 121.5(4) . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.7(4) . . ?
N12 C13 C14 120.7(4) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.2(4) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 120.5 . . ?
C16 C15 C14 119.0(4) . . ?
C16 C15 H15 120.5 . . ?
N1 C16 C15 120.9(4) . . ?
N1 C16 H16 119.6 . . ?
C1 C16 C15 120.9(4) . . ?
C15 C16 H16 119.6 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 N2 C26 119.2(5) . . ?
C22 N2 C27 120.0(4) . . ?
C26 N2 C27 120.8(5) . . ?
N22 C2 C26 119.2(5) . . ?
N22 C2 C27 120.0(4) . . ?
C26 C2 C27 120.8(5) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
N2 C22 C21 119.3(4) . . ?
N2 C22 C23 120.7(5) . . ?
C23 C22 C21 119.9(5) . . ?
C2 N22 C21 119.3(4) . . ?
C2 N22 C23 120.7(5) . . ?
C23 N22 C21 119.9(5) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.5(5) . . ?
C24 C23 N22 121.5(5) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.8(5) . . ?
C25 C24 H24 120.6 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.6(5) . . ?
C26 C25 H25 120.2 . . ?
N2 C26 C25 120.1(5) . . ?
N2 C26 H26 119.9 . . ?
C2 C26 C25 120.1(5) . . ?
C25 C26 H26 119.9 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
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
Te1 Br11 2.6920(5) . yes
Te1 Br11 2.6921(5) 2_755 ?
Te1 Br12 2.6987(5) . yes
Te1 Br12 2.6987(5) 2_755 ?
Te1 Br13 2.6927(4) . yes
Te1 Br13 2.6927(4) 2_755 ?
Te2 Br21 2.7010(4) . yes
Te2 Br21 2.7010(4) 5_666 ?
Te2 Br22 2.7013(5) . yes
Te2 Br22 2.7013(5) 5_666 ?
Te2 Br23 2.6976(4) . yes
Te2 Br23 2.6976(4) 5_666 ?
N1 C12 1.355(5) . ?
N1 C16 1.358(5) . ?
N1 C17 1.479(5) . ?
C1 N12 1.355(5) . ?
C1 C16 1.358(5) . ?
C1 C17 1.479(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C12 1.493(6) . ?
C11 N12 1.493(6) . ?
C12 C13 1.374(6) . ?
N12 C13 1.374(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.375(6) . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 C22 1.349(6) . ?
N2 C26 1.371(7) . ?
N2 C27 1.486(6) . ?
C2 N22 1.349(6) . ?
C2 C26 1.371(7) . ?
C2 C27 1.486(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C22 1.470(7) . ?
C21 N22 1.470(7) . ?
C22 C23 1.360(6) . ?
N22 C23 1.360(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.352(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.377(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(8) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
