Synthesis of phosphaguanidines by hydrophosphination of carbodiimides with phosphine boranes.
Busacca, Carl A.; Milligan, John A.; Rattanangkool, Eakkaphon; Ramavarapu, Cyrus; Chen, Anji; Saha, Anjan K.; Li, Zhibin; Lee, Heewon; Geib, Steven J.; Wang, Guijun; Senanayake, Chris H.; Wipf, Peter; The Journal of organic chemistry 79 (2014) 9878–9887; doi:10.1021/jo501841s

data_4029984
_publ_section_title
;
 Synthesis of phosphaguanidines by hydrophosphination of carbodiimides
 with phosphine boranes.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9878
_journal_page_last               9887
_journal_paper_doi               10.1021/jo501841s
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C21 H34 B3 N4 P'
_chemical_formula_weight         405.92
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.043(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0389(7)
_cell_length_b                   22.5581(18)
_cell_length_c                   12.9197(11)
_cell_measurement_temperature    100(2)
_cell_volume                     2342.5(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.676
_diffrn_measured_fraction_theta_max 0.738
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.676
_diffrn_reflns_Laue_measured_fraction_max 0.738
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11192
_diffrn_reflns_point_group_measured_fraction_full 0.676
_diffrn_reflns_point_group_measured_fraction_max 0.738
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.966
_diffrn_reflns_theta_min         5.206
_exptl_absorpt_coefficient_mu    1.128
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         2872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2004
_reflns_number_total             2872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo501841s_si_001.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 4029984--4029987.cif.'
_cod_database_code               4029984
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2013-2
_shelx_res_checksum              69638
_shelx_hkl_checksum              1280