Aspects of phosphaallene chemistry - heat induced formation of 1,2-dihydrophosphetes by intramolecular nucleophilic aromatic substitution and photochemical generation of tricyclic phosphiranes.
Tendyck, Jonas C.; Klöcker, Hans; Schürmann, Lina; Würthwein, Ernst-Ulrich; Hepp, Alexander; Layh, Marcus; Uhl, Werner; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b03056

data_4037970
_publ_section_title
;
 Aspects of phosphaallene chemistry - heat induced formation of
 1,2-dihydrophosphetes by intramolecular nucleophilic aromatic
 substitution and photochemical generation of tricyclic phosphiranes.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b03056
_journal_year                    2020
_chemical_formula_sum            'C38 H51 Cl3 Ir P'
_chemical_formula_weight         837.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.2300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.065(2)
_cell_length_b                   9.2931(4)
_cell_length_c                   21.2408(8)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.897
_cell_measurement_theta_min      2.252
_cell_volume                     7782.8(6)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.814
_diffrn_reflns_theta_min         2.066
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_T_max  0.7787
_exptl_absorpt_correction_T_min  0.6108
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'TWINABS 2012/1'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
The unit cell contains 6 molecules of benzene which have
been treated as a diffuse contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON
;
_refine_diff_density_max         2.514
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10042
_refine_ls_number_restraints     467
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+6.0266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
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_reflns_number_gt                7887
_reflns_number_total             10042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03056_si_001.cif
_cod_data_source_block           platon_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4037970
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.837
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              83357
_shelx_hkl_checksum              46762
_shelx_fab_checksum              34627