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_4037971
_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            'C42 H56 Cl2 F Ir P'
_chemical_formula_weight         873.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.020(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.082(3)
_cell_length_b                   9.348(2)
_cell_length_c                   21.825(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.260
_cell_measurement_theta_min      2.386
_cell_volume                     3938.0(12)
_computing_cell_refinement       'Bruker SAINT+'
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_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 0.999
_diffrn_measured_fraction_theta_max 0.929
_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  0.0842
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
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_diffrn_reflns_point_group_measured_fraction_max 0.929
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_diffrn_reflns_theta_min         2.385
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_exptl_absorpt_coefficient_mu    3.599
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.4626
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       stick
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.090
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_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
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_refine_ls_number_parameters     448
_refine_ls_number_reflns         15408
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_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10559
_reflns_number_total             15408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03056_si_001.cif
_cod_data_source_block           sad_a_compound_6c
_cod_original_sg_symbol_H-M      'P 21/c'
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_shelx_estimated_absorpt_t_min   0.307
_shelx_estimated_absorpt_t_max   0.762
_shelx_res_checksum              64110
_shelx_hkl_checksum              1381