Potassium-Mediated Hydrophosphorylation of Heterocumulenes with Diarylphosphane Oxide and Sulfide.
Härling, Stephan M; Görls, Helmar; Krieck, Sven; Westerhausen, Matthias; Inorganic chemistry 55 (2016) 10741–10750; doi:10.1021/acs.inorgchem.6b01973

data_4349146
_publ_section_title
;
 Potassium-Mediated Hydrophosphorylation of Heterocumulenes with
 Diarylphosphane Oxide and Sulfide.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10741
_journal_page_last               10750
_journal_paper_doi               10.1021/acs.inorgchem.6b01973
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C22 H30 N O2 P'
_chemical_formula_sum            'C22 H30 N O2 P'
_chemical_formula_weight         371.44
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.199(1)
_cell_angle_beta                 92.364(1)
_cell_angle_gamma                117.618(1)
_cell_formula_units_Z            4
_cell_length_a                   12.5040(3)
_cell_length_b                   13.0411(4)
_cell_length_c                   14.4520(4)
_cell_measurement_reflns_used    11728
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.13
_cell_volume                     2070.24(10)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11728
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                6568
_reflns_number_total             8935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01973_si_001.cif
_cod_data_source_block           FO6016
_cod_database_code               4349146