Carbene-Stabilized Parent Phosphinidene†
Wang, Yuzhong; Xie, Yaoming; Abraham, Mariham Y.; Gilliard, Robert J.; Wei, Pingrong; Schaefer, Henry F.; Schleyer, Paul v. R.; Robinson, Gregory H.; Organometallics 29 (2010) 4778–; doi:10.1021/om100335j

data_4066175
_publ_section_title
;
 Carbene-Stabilized Parent Phosphinidene&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4778
_journal_paper_doi               10.1021/om100335j
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C39 H60 Li N2 O3 P'
_chemical_formula_weight         642.80
_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                74.0970(10)
_cell_angle_beta                 89.7740(10)
_cell_angle_gamma                67.7320(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4993(9)
_cell_length_b                   11.3546(10)
_cell_length_c                   19.1402(16)
_cell_measurement_reflns_used    4425
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      21.830
_cell_measurement_theta_min      2.494
_cell_volume                     2018.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21699
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9898
_exptl_absorpt_correction_T_min  0.9679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7110
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0855P)^2^+0.4988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                4247
_reflns_number_total             7110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100335j_si_002.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066175