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#$Date: 2022-06-02 01:00:08 +0300 (Thu, 02 Jun 2022) $
#$Revision: 275722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/01/7130174.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_7130174
loop_
_publ_author_name
'Batabyal, Monojit'
'Jain, Saket'
'Upadhyay, Aditya'
'Raju, Saravanan'
'Kumar, Sangit'
_publ_section_title
;
 A base-free copper-assisted synthesis of C2-symmetric spirotelluranes and
 biaryls based on divergent stoichiometry of Na2Te
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02181A
_journal_year                    2022
_chemical_formula_moiety         'C7 H5 O Te0.50'
_chemical_formula_sum            'C7 H5 O Te0.5'
_chemical_formula_weight         168.91
_chemical_name_common            'C7 H5 O Te0.50'
_chemical_name_systematic        'C7 H5 O Te0.50'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-08 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.957(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.507(4)
_cell_length_b                   4.8515(8)
_cell_length_c                   14.046(2)
_cell_measurement_reflns_used    1772
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      4.13
_cell_volume                     1222.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4171
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.668
_diffrn_reflns_theta_min         4.129
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.036
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0371P)²+0.7485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1390
_reflns_number_total             1563
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc02181a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1222.8(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C7 H5 O Te0.50'
_cod_database_code               7130174
_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.
;
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 0.500000 0.32832(6) 0.250000 0.04734(13) Uani 1 2 d S T P . .
O1 O 0.55779(15) 0.3858(6) 0.41519(18) 0.0577(6) Uani 1 1 d . . . . .
C2B C 0.5865(9) 0.705(2) 0.1720(8) 0.0536(11) Uani 0.54(5) 1 d . . P A 2
H2B H 0.556722 0.632339 0.102814 0.064 Uiso 0.54(5) 1 calc R U P A 2
C3B C 0.6375(14) 0.904(3) 0.1899(12) 0.062(2) Uani 0.54(5) 1 d . . P A 2
H3B H 0.644172 0.966448 0.132621 0.075 Uiso 0.54(5) 1 calc R U P A 2
C4B C 0.6795(12) 1.016(3) 0.2921(13) 0.064(2) Uani 0.54(5) 1 d . . P A 2
H4B H 0.713509 1.154835 0.302397 0.077 Uiso 0.54(5) 1 calc R U P A 2
C5B C 0.6721(6) 0.925(2) 0.3795(9) 0.0613(11) Uani 0.54(5) 1 d . . P A 2
H5B H 0.701183 1.001775 0.448045 0.074 Uiso 0.54(5) 1 calc R U P A 2
C6 C 0.62177(17) 0.7224(7) 0.36465(19) 0.0474(7) Uani 1 1 d G . . . .
C5A C 0.6787(5) 0.909(2) 0.3865(5) 0.0613(11) Uani 0.46(5) 1 d G . P A 1
H5A H 0.706314 0.982425 0.456050 0.074 Uiso 0.46(5) 1 calc R U P A 1
C4A C 0.6945(9) 0.986(4) 0.3045(8) 0.064(2) Uani 0.46(5) 1 d G . P A 1
H4A H 0.732587 1.111386 0.319155 0.077 Uiso 0.46(5) 1 calc R U P A 1
C3A C 0.6533(9) 0.877(4) 0.2006(7) 0.062(2) Uani 0.46(5) 1 d G . P A 1
H3A H 0.663790 0.928656 0.145733 0.075 Uiso 0.46(5) 1 calc R U P A 1
C2A C 0.5963(5) 0.690(2) 0.1787(4) 0.0536(11) Uani 0.46(5) 1 d G . P A 1
H2A H 0.568719 0.616964 0.109205 0.064 Uiso 0.46(5) 1 calc R U P A 1
C1 C 0.58056(15) 0.6129(6) 0.26074(19) 0.0431(7) Uani 1 1 d G . . A .
C7 C 0.6029(2) 0.6226(9) 0.4501(3) 0.0589(9) Uani 1 1 d . . . . .
H7 H 0.618994 0.706863 0.517276 0.071 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'
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
_geom_angle_publ_flag
O1 Te1 O1 164.35(15) 2_655 . ?
O1 Te1 C1 80.0(4) 2_655 2_655 ?
O1 Te1 C1 89.7(5) . 2_655 ?
O1 Te1 C1 89.74(10) 2_655 . ?
O1 Te1 C1 79.96(10) . . ?
C1 Te1 C1 97.9(6) 2_655 . ?
C7 O1 Te1 115.36(19) . . ?
C3B C2B C1 117.3(7) . . ?
C3B C2B H2B 121.4 . . ?
C1 C2B H2B 121.4 . . ?
C2B C3B C4B 120.7(7) . . ?
C2B C3B H3B 119.6 . . ?
C4B C3B H3B 119.6 . . ?
C3B C4B C5B 121.3(7) . . ?
C3B C4B H4B 119.4 . . ?
C5B C4B H4B 119.4 . . ?
C6 C5B C4B 119.6(7) . . ?
C6 C5B H5B 120.2 . . ?
C4B C5B H5B 120.2 . . ?
C5B C6 C1 117.7(6) . . ?
C5A C6 C1 120.0 . . ?
C5B C6 C7 125.2(5) . . ?
C5A C6 C7 123.1(3) . . ?
C1 C6 C7 116.9(3) . . ?
C6 C5A C4A 120.0 . . ?
C6 C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C2A C3A C4A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C1 C2A C3A 120.0 . . ?
C1 C2A H2A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C2B C1 C6 123.3(7) . . ?
C2A C1 C6 120.0 . . ?
C2B C1 Te1 123.7(6) . . ?
C2A C1 Te1 127.4(2) . . ?
C6 C1 Te1 112.6(2) . . ?
O1 C7 C6 111.3(3) . . ?
O1 C7 H7 124.3 . . ?
C6 C7 H7 124.3 . . ?
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 O1 2.050(2) 2_655 ?
Te1 O1 2.050(2) . ?
Te1 C1 2.102(19) 2_655 ?
Te1 C1 2.102(3) . ?
O1 C7 1.405(5) . ?
C2B C3B 1.356(12) . ?
C2B C1 1.384(9) . ?
C2B H2B 0.9300 . ?
C3B C4B 1.378(13) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.379(11) . ?
C4B H4B 0.9300 . ?
C5B C6 1.367(10) . ?
C5B H5B 0.9300 . ?
C6 C5A 1.3900 . ?
C6 C1 1.3900 . ?
C6 C7 1.509(5) . ?
C5A C4A 1.3900 . ?
C5A H5A 0.9300 . ?
C4A C3A 1.3900 . ?
C4A H4A 0.9300 . ?
C3A C2A 1.3900 . ?
C3A H3A 0.9300 . ?
C2A C1 1.3900 . ?
C2A H2A 0.9300 . ?
C7 H7 0.9300 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2B C3B C4B -2.1(10) . . . . ?
C2B C3B C4B C5B 1.2(11) . . . . ?
C3B C4B C5B C6 -0.5(11) . . . . ?
C4B C5B C6 C1 0.9(10) . . . . ?
C4B C5B C6 C7 -174.1(8) . . . . ?
C1 C6 C5A C4A 0.0 . . . . ?
C7 C6 C5A C4A 178.2(7) . . . . ?
C6 C5A C4A C3A 0.0 . . . . ?
C5A C4A C3A C2A 0.0 . . . . ?
C4A C3A C2A C1 0.0 . . . . ?
C3B C2B C1 C6 2.6(9) . . . . ?
C3B C2B C1 Te1 175.1(7) . . . . ?
C3A C2A C1 C6 0.0 . . . . ?
C3A C2A C1 Te1 -178.2(7) . . . . ?
C5B C6 C1 C2B -2.0(9) . . . . ?
C7 C6 C1 C2B 173.4(8) . . . . ?
C5A C6 C1 C2A 0.0 . . . . ?
C7 C6 C1 C2A -178.3(6) . . . . ?
C5B C6 C1 Te1 -175.2(7) . . . . ?
C5A C6 C1 Te1 178.4(6) . . . . ?
C7 C6 C1 Te1 0.1(4) . . . . ?
Te1 O1 C7 C6 -21.7(4) . . . . ?
C5B C6 C7 O1 -171.1(8) . . . . ?
C5A C6 C7 O1 -164.4(6) . . . . ?
C1 C6 C7 O1 13.9(4) . . . . ?
