#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:52:03 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058146.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_7058146
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            'C10 H12 Br6 Cl4 N2 O2 Te'
_chemical_formula_weight         941.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 98.779(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6178(4)
_cell_length_b                   12.9085(6)
_cell_length_c                   10.8436(5)
_cell_measurement_reflns_used    2278
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      3.62
_cell_volume                     1192.14(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.841
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5336
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.847
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72265
_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    2.622
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2627
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0352
_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)+(0.0174P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2283
_reflns_number_total             2627
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj00320g2.cif
_cod_data_source_block           Au282
_cod_depositor_comments
'Adding full bibliography for 7058143--7058147.cif.'
_cod_database_code               7058146
_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   0.191
_shelx_estimated_absorpt_t_max   0.333
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Te1 Te 0.500000 0.500000 1.000000 0.01318(9) Uani 1 2 d S . P
Br1 Br 0.36562(4) 0.39771(3) 0.79433(3) 0.02040(10) Uani 1 1 d . . .
Br2 Br 0.71023(5) 0.34665(3) 1.05688(3) 0.02028(10) Uani 1 1 d . . .
Br3 Br 0.30462(5) 0.40378(3) 1.13348(3) 0.02148(10) Uani 1 1 d . . .
N1 N 0.8784(4) 0.3740(2) 0.6600(3) 0.0208(7) Uani 1 1 d . . .
H1N H 0.918263 0.377224 0.739614 0.025 Uiso 1 1 calc R U .
C1 C 0.9772(5) 0.3721(3) 0.5759(3) 0.0205(8) Uani 1 1 d . . .
H1 H 1.087563 0.373561 0.601856 0.025 Uiso 1 1 calc R U .
C2 C 0.9162(5) 0.3680(3) 0.4517(3) 0.0184(8) Uani 1 1 d . . .
C3 C 0.7557(5) 0.3650(3) 0.4151(3) 0.0216(8) Uani 1 1 d . . .
H3 H 0.712417 0.361999 0.329173 0.026 Uiso 1 1 calc R U .
C4 C 0.6587(5) 0.3664(3) 0.5059(3) 0.0206(8) Uani 1 1 d . . .
C5 C 0.7232(5) 0.3711(3) 0.6292(3) 0.0200(8) Uani 1 1 d . . .
H5 H 0.657697 0.372427 0.692144 0.024 Uiso 1 1 calc R U .
Cl1 Cl 1.04215(12) 0.37030(7) 0.34300(9) 0.0252(2) Uani 1 1 d . . .
Cl2 Cl 0.45901(12) 0.36296(8) 0.46576(9) 0.0304(2) Uani 1 1 d . . .
O1 O 1.0012(4) 0.3972(3) 0.8945(2) 0.0442(9) Uani 1 1 d D . .
H1O H 0.948(3) 0.389(4) 0.953(3) 0.053 Uiso 1 1 d D U .
H2O H 1.0978(14) 0.399(4) 0.923(3) 0.053 Uiso 1 1 d D 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'
Cl Cl 0.1484 0.1585 '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
Br1 Te1 Br1 180.0 . 3_667 yes
Br2 Te1 Br1 88.940(12) . 3_667 yes
Br2 Te1 Br1 88.940(12) 3_667 . ?
Br2 Te1 Br1 91.059(12) 3_667 3_667 ?
Br2 Te1 Br1 91.060(12) . . yes
Br2 Te1 Br2 180.0 . 3_667 yes
Br3 Te1 Br1 89.648(12) . . yes
Br3 Te1 Br1 89.649(12) 3_667 3_667 ?
Br3 Te1 Br1 90.351(12) 3_667 . ?
Br3 Te1 Br1 90.352(12) . 3_667 yes
Br3 Te1 Br2 89.531(12) . . yes
Br3 Te1 Br2 89.532(12) 3_667 3_667 ?
Br3 Te1 Br2 90.468(12) 3_667 . ?
Br3 Te1 Br2 90.469(12) . 3_667 yes
Br3 Te1 Br3 180.0 3_667 . yes
C1 N1 H1N 118.4 . . ?
C5 N1 H1N 118.4 . . ?
C5 N1 C1 123.2(3) . . ?
N1 C1 H1 120.6 . . ?
N1 C1 C2 118.8(4) . . ?
C2 C1 H1 120.6 . . ?
C1 C2 C3 120.1(3) . . ?
C1 C2 Cl1 119.1(3) . . ?
C3 C2 Cl1 120.9(3) . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.8(3) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 Cl2 120.7(3) . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 Cl2 119.5(3) . . ?
N1 C5 C4 119.4(3) . . ?
N1 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
H1O O1 H2O 110.5(17) . . ?
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 Br1 2.6963(4) . yes
Te1 Br1 2.6963(4) 3_667 ?
Te1 Br2 2.6908(4) . yes
Te1 Br2 2.6908(4) 3_667 ?
Te1 Br3 2.6864(4) . yes
Te1 Br3 2.6864(4) 3_667 ?
N1 H1N 0.8800 . ?
N1 C1 1.340(4) . ?
N1 C5 1.328(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.369(5) . ?
C2 C3 1.381(5) . ?
C2 Cl1 1.720(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(5) . ?
C4 C5 1.369(5) . ?
C4 Cl2 1.710(4) . ?
C5 H5 0.9500 . ?
O1 H1O 0.840(10) . ?
O1 H2O 0.843(10) . ?
