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_7130177
_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         'C34 H26 N4 O4'
_chemical_formula_sum            'C34 H26 N4 O4'
_chemical_formula_weight         554.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-03-08 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                79.2160(10)
_cell_angle_beta                 83.650(2)
_cell_angle_gamma                85.0130(10)
_cell_formula_units_Z            2
_cell_length_a                   7.2109(3)
_cell_length_b                   13.1523(5)
_cell_length_c                   14.1608(6)
_cell_measurement_reflns_used    8800
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.85
_cell_volume                     1308.18(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      139.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20958
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.849
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7075
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1052 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.9483.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0403P)^2^+0.7304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4906
_reflns_number_total             6689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02181a2.cif
_cod_data_source_block           f1_a
_cod_database_code               7130177
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N005(H005), N007(H007), C00A(H00A), C00C(H00C), C00F(H00F), C00G(H00G),
 C00I(H00I), C00L(H00L), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C013(H013), C014(H014),
 C015(H015), C016(H016)
2.b Idealised Me refined as rotating group:
 C00Q(H00B,H00D,H00E), C00R(H00H,H00J,H00K)
;
_shelx_res_checksum              13670
_shelx_hkl_checksum              50693
_olex2_submission_special_instructions 'No special instructions were received'