#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:52:03 +0100 (vie 08 de nov de 2019) $
#$Revision: 224887 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/81/7058147.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_7058147
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            'C12 H18 Br8 N2 O2 Te'
_chemical_formula_weight         989.16
_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                 109.028(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7234(5)
_cell_length_b                   11.0724(5)
_cell_length_c                   12.1082(7)
_cell_measurement_reflns_used    2812
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      3.73
_cell_volume                     1232.36(12)
_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 0.843
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5857
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.874
_diffrn_reflns_theta_min         3.560
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    14.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39721
_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    2.666
_exptl_crystal_description       stick
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2725
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0281
_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)+(0.0122P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2266
_reflns_number_total             2725
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj00320g2.cif
_cod_data_source_block           AU304
_cod_depositor_comments
'Adding full bibliography for 7058143--7058147.cif.'
_cod_database_code               7058147
_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   0.057
_shelx_estimated_absorpt_t_max   0.331
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 1.000000 0.500000 0.01636(9) Uani 1 2 d S . P
Br1 Br 0.25227(4) 1.11657(4) 0.38147(3) 0.02634(11) Uani 1 1 d . . .
Br2 Br 0.63690(4) 1.12047(4) 0.37480(3) 0.02724(11) Uani 1 1 d . . .
Br3 Br 0.42827(4) 0.82685(4) 0.33526(3) 0.02531(11) Uani 1 1 d . . .
N1 N 0.7763(3) 0.4350(3) 0.5309(3) 0.0225(8) Uani 1 1 d . . .
H1 H 0.718904 0.475613 0.560668 0.027 Uiso 1 1 calc R U .
C1 C 0.7846(4) 0.4682(4) 0.4267(3) 0.0201(9) Uani 1 1 d . . .
C2 C 0.8736(4) 0.4061(4) 0.3790(3) 0.0231(9) Uani 1 1 d . . .
H2 H 0.880461 0.429113 0.305392 0.028 Uiso 1 1 calc R U .
C3 C 0.9525(4) 0.3103(4) 0.4393(3) 0.0241(9) Uani 1 1 d . . .
H3 H 1.014351 0.267348 0.406431 0.029 Uiso 1 1 calc R U .
C4 C 0.9444(4) 0.2738(4) 0.5481(3) 0.0225(9) Uani 1 1 d . . .
C5 C 0.8532(4) 0.3416(4) 0.5912(3) 0.0222(9) Uani 1 1 d . . .
H5 H 0.844872 0.321454 0.665077 0.027 Uiso 1 1 calc R U .
C6 C 1.0234(4) 0.1658(4) 0.6124(3) 0.0285(10) Uani 1 1 d . . .
H6A H 1.053717 0.181096 0.696659 0.043 Uiso 1 1 calc R U .
H6B H 1.109307 0.150144 0.589202 0.043 Uiso 1 1 calc R U .
H6C H 0.958789 0.095418 0.593467 0.043 Uiso 1 1 calc R U .
Br4 Br 0.67129(4) 0.60073(4) 0.35686(4) 0.03244(12) Uani 1 1 d . . .
O1 O 0.6137(3) 0.5773(3) 0.6245(2) 0.0362(8) Uani 1 1 d D . .
H1O H 0.627(4) 0.6443(19) 0.596(3) 0.043 Uiso 1 1 d D U .
H2O H 0.659(4) 0.575(3) 0.6966(11) 0.043 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'
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_676 yes
Br2 Te1 Br1 89.021(13) . . yes
Br2 Te1 Br1 89.021(13) 3_676 3_676 ?
Br2 Te1 Br1 90.978(13) 3_676 . ?
Br2 Te1 Br1 90.979(13) . 3_676 yes
Br2 Te1 Br2 180.0 . 3_676 yes
Br2 Te1 Br3 89.528(12) . . yes
Br2 Te1 Br3 89.528(13) 3_676 3_676 ?
Br2 Te1 Br3 90.471(13) . 3_676 yes
Br2 Te1 Br3 90.472(13) 3_676 . ?
Br3 Te1 Br1 88.615(13) 3_676 3_676 ?
Br3 Te1 Br1 88.615(14) . . yes
Br3 Te1 Br1 91.385(14) . 3_676 yes
Br3 Te1 Br1 91.385(14) 3_676 . ?
Br3 Te1 Br3 180.0 . 3_676 yes
C1 N1 H1 119.0 . . ?
C1 N1 C5 121.9(3) . . ?
C5 N1 H1 119.0 . . ?
N1 C1 C2 119.9(4) . . ?
N1 C1 Br4 115.8(3) . . ?
C2 C1 Br4 124.3(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 121.9(3) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C6 122.8(3) . . ?
C5 C4 C3 115.8(4) . . ?
C5 C4 C6 121.3(3) . . ?
N1 C5 C4 121.5(3) . . ?
N1 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H1O O1 H2O 110.7(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 2.6970(4) . yes
Te1 Br1 2.6970(4) 3_676 ?
Te1 Br2 2.6768(4) . yes
Te1 Br2 2.6768(4) 3_676 ?
Te1 Br3 2.6896(4) . yes
Te1 Br3 2.6896(4) 3_676 ?
N1 H1 0.8800 . ?
N1 C1 1.342(4) . ?
N1 C5 1.344(5) . ?
C1 C2 1.372(5) . ?
C1 Br4 1.864(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.404(5) . ?
C4 C5 1.387(5) . ?
C4 C6 1.495(5) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
O1 H1O 0.843(10) . ?
O1 H2O 0.841(10) . ?
