A base-free copper-assisted synthesis of C2-symmetric spirotelluranes and biaryls based on divergent stoichiometry of Na2Te
Batabyal, Monojit; Jain, Saket; Upadhyay, Aditya; Raju, Saravanan; Kumar, Sangit; Chemical Communications  (2022) –; doi:10.1039/D2CC02181A

data_7130176
_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         '4(C16 O6 Te)'
_chemical_formula_sum            'C16 H12 O6 Te'
_chemical_formula_weight         427.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2430(14)
_cell_length_b                   4.7234(3)
_cell_length_c                   15.8545(12)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.48
_cell_volume                     1441.05(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14409
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         2.476
_exptl_absorpt_coefficient_mu    2.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.207
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Flack x determined using 977 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3399
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0515
_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/[\s^2^(Fo^2^)+(0.0356P)^2^+8.8172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                2634
_reflns_number_total             3399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02181a2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7130176
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              69020
_shelx_hkl_checksum              31309