Selective Oxidation and Functionalization of 6-Diphenylphosphinoacenaphthyl-5-tellurenyl Species 6-Ph2P-Ace-5-TeX (X = Mes, Cl, O3SCF3). Various Types of P‒E···Te(II,IV) Bonding Situations (E = O, S, Se)
Hupf, Emanuel; Do, Truong Giang; Nordheider, Andreas; Wehrhahn, Maren; Sanz Camacho, Paula; Ashbrook, Sharon E.; Lork, Enno; Slawin, Alexandra M. Z.; Mebs, Stefan; Woollins, J. Derek; Beckmann, Jens; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00133

data_4087206
_publ_section_title
;
 Selective Oxidation and Functionalization of
 6-Diphenylphosphinoacenaphthyl-5-tellurenyl Species 6-Ph2P-Ace-5-TeX (X =
 Mes, Cl, O3SCF3). Various Types of P--E&#x00B7;&#x00B7;&#x00B7;Te(II,IV)
 Bonding Situations (E = O, S, Se)
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00133
_journal_year                    2017
_chemical_formula_moiety         'C18 H22 Cl3 O P Te'
_chemical_formula_sum            'C18 H22 Cl3 O P Te'
_chemical_formula_weight         519.30
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.2187(12)
_cell_length_b                   11.8772(13)
_cell_length_c                   18.454(2)
_cell_measurement_reflns_used    6220
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.00
_cell_volume                     2020.6(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 11.628
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24935
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_min         2.039
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.36
_refine_diff_density_min         -0.89
_refine_ls_abs_structure_details
;
 Flack x determined using 1435 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.500(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                3480
_reflns_number_total             3714
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om7b00133_si_002.cif
_cod_data_source_block           4OPr
_cod_database_code               4087206