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_4037965
_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            'C31 H37 O5 P W'
_chemical_formula_weight         704.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.1910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2859(5)
_cell_length_b                   14.0636(6)
_cell_length_c                   17.5304(7)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.945
_cell_measurement_theta_min      2.362
_cell_volume                     2971.4(2)
_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 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_limit_k_max       18
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_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
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_diffrn_reflns_theta_max         27.952
_diffrn_reflns_theta_min         2.244
_diffrn_source                   microsource
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_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     353
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     0
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_refine_ls_R_factor_gt           0.0279
_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^)+(0.0284P)^2^+2.5198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5953
_reflns_number_total             7122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03056_si_001.cif
_cod_data_source_block           sad_a
_cod_original_sg_symbol_H-M      'P 21/n'
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_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.489
_shelx_estimated_absorpt_t_max   0.587
_shelx_res_checksum              69365
_shelx_hkl_checksum              63918