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_4087197
_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_sum            'C27 H25 Cl P S Te'
_chemical_formula_weight         575.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.4650(10)
_cell_angle_beta                 85.8230(10)
_cell_angle_gamma                80.7810(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2470(2)
_cell_length_b                   11.2205(3)
_cell_length_c                   13.1314(3)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.51
_cell_volume                     1187.40(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Venture D8'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38000
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.9876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                5540
_reflns_number_total             5912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00133_si_002.cif
_cod_data_source_block           2S
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4087197