#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:52:03 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058145.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_7058145
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 H10 Br6 Cl2 N2 Te'
_chemical_formula_weight         836.16
_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   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                74.694(6)
_cell_angle_beta                 70.263(5)
_cell_angle_gamma                83.031(6)
_cell_formula_units_Z            1
_cell_length_a                   7.3223(5)
_cell_length_b                   8.3339(6)
_cell_length_c                   9.0497(6)
_cell_measurement_reflns_used    2463
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      3.93
_cell_volume                     501.05(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.823
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3754
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.052
_diffrn_reflns_theta_min         3.617
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    13.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21008
_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    2.771
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.952
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0352
_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)+(0.0363P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1905
_reflns_number_total             2201
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj00320g2.cif
_cod_data_source_block           AU200Orange
_cod_depositor_comments
'Adding full bibliography for 7058143--7058147.cif.'
_cod_database_code               7058145
_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   0.076
_shelx_estimated_absorpt_t_max   0.341
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
_atom_site_refinement_flags_occupancy
Te1 Te 0.000000 0.500000 0.500000 0.01461(12) Uani 1 2 d S . P
Br1 Br 0.06273(7) 0.16984(6) 0.60041(6) 0.01987(14) Uani 1 1 d . . .
Br3 Br 0.30757(7) 0.51433(6) 0.22841(6) 0.02015(14) Uani 1 1 d . . .
Br5 Br 0.22921(8) 0.56862(7) 0.65329(6) 0.02813(16) Uani 1 1 d . . .
N1 N 0.4186(7) 0.1795(6) 0.7862(5) 0.0318(11) Uani 1 1 d . U .
H1 H 0.447147 0.285011 0.760304 0.038 Uiso 1 1 d R U .
C11 C 0.2846(7) 0.1121(7) 0.9256(6) 0.0229(11) Uani 1 1 d . U .
C12 C 0.2570(7) -0.0545(6) 0.9689(6) 0.0229(11) Uani 1 1 d . U .
H12 H 0.164005 -0.103678 1.068508 0.028 Uiso 1 1 calc R U .
C13 C 0.3664(9) -0.1495(8) 0.8657(7) 0.0430(16) Uani 1 1 d . U .
H13 H 0.347774 -0.265825 0.892543 0.052 Uiso 1 1 calc R U .
C14 C 0.5031(10) -0.0773(9) 0.7233(8) 0.054(2) Uani 1 1 d . U .
H14 H 0.578160 -0.143551 0.651554 0.065 Uiso 1 1 calc R U .
C15 C 0.5306(8) 0.0869(9) 0.6856(7) 0.0454(17) Uani 1 1 d . U .
H15 H 0.627767 0.137042 0.589154 0.055 Uiso 1 1 calc R U .
Cl1 Cl 0.1587(3) 0.24219(19) 1.04334(19) 0.0552(5) Uani 1 1 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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
Br1 Te1 Br1 180.0 . 2_566 yes
Br1 Te1 Br3 88.826(16) . 2_566 yes
Br1 Te1 Br3 88.826(16) 2_566 . ?
Br1 Te1 Br3 91.174(16) . . yes
Br1 Te1 Br3 91.174(16) 2_566 2_566 ?
Br1 Te1 Br5 88.341(16) . 2_566 yes
Br1 Te1 Br5 88.341(16) 2_566 . ?
Br1 Te1 Br5 91.658(16) . . yes
Br1 Te1 Br5 91.659(16) 2_566 2_566 ?
Br3 Te1 Br3 180.0 . 2_566 yes
Br5 Te1 Br3 89.638(16) . 2_566 yes
Br5 Te1 Br3 89.639(16) 2_566 . ?
Br5 Te1 Br3 90.362(16) . . yes
Br5 Te1 Br3 90.362(16) 2_566 2_566 ?
Br5 Te1 Br5 180.0 2_566 . yes
C11 N1 H1 121.7 . . ?
C11 N1 C15 122.0(5) . . ?
C15 N1 H1 116.0 . . ?
N1 C11 C12 120.2(5) . . ?
N1 C11 Cl1 117.0(4) . . ?
C12 C11 Cl1 122.7(4) . . ?
C11 C12 H12 120.8 . . ?
C11 C12 C13 118.4(5) . . ?
C13 C12 H12 120.8 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.2(6) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0(6) . . ?
C15 C14 H14 120.0 . . ?
N1 C15 H15 120.4 . . ?
C14 C15 N1 119.1(5) . . ?
C14 C15 H15 120.4 . . ?
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 2.6950(5) . yes
Te1 Br1 2.6950(5) 2_566 ?
Te1 Br3 2.7016(5) . yes
Te1 Br3 2.7017(5) 2_566 ?
Te1 Br5 2.7005(6) . yes
Te1 Br5 2.7005(6) 2_566 ?
N1 H1 0.8800 . ?
N1 C11 1.339(7) . ?
N1 C15 1.346(8) . ?
C11 C12 1.359(7) . ?
C11 Cl1 1.693(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.369(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.375(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.343(10) . ?
C15 H15 0.9500 . ?
