Synthesis, Structure, and Bonding of 1-Oxa-6,6aλ(4)- chalcogenopentalenes and Related Derivatives; The Role of Intramolecular Coordination.
Prasad, Poonam Rajesh; Selvakumar, Karuthapandi; Singh, Harkesh B.; Butcher, Ray J.; The Journal of organic chemistry 81 (2016) 3214–3226; doi:10.1021/acs.joc.6b00173

data_4036640
_publ_section_title
;
 Synthesis, Structure, and Bonding of 1-Oxa-6,6a\l(4)-
 chalcogenopentalenes and Related Derivatives; The Role of Intramolecular
 Coordination.
;
_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3214
_journal_page_last               3226
_journal_paper_doi               10.1021/acs.joc.6b00173
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C8 H7 O Te2'
_chemical_formula_sum            'C8 H7 O Te2'
_chemical_formula_weight         374.34
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4121(3)
_cell_length_b                   16.6843(5)
_cell_length_c                   4.8996(2)
_cell_measurement_reflns_used    1361
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.7024
_cell_measurement_theta_min      4.6907
_cell_volume                     932.90(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'SHELXLTL (Sheldrick, 2008)'
_computing_publication_material  SHELXLTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1868
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         72.62
_diffrn_reflns_theta_min         6.57
_exptl_absorpt_coefficient_mu    48.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.671
_refine_diff_density_min         -3.631
_refine_diff_density_rms         0.432
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1139
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1445P)^2^+25.7318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2531
_reflns_number_gt                1006
_reflns_number_total             1139
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo6b00173_si_005.cif
_cod_data_source_block           36
_cod_database_code               4036640