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_4029986
_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_moiety         'C25 H49 B N2 P, B F4'
_chemical_formula_sum            'C25 H49 B2 F4 N2 P'
_chemical_formula_weight         506.25
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.0953(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0541(3)
_cell_length_b                   16.1202(4)
_cell_length_c                   15.0576(3)
_cell_measurement_temperature    180(2)
_cell_volume                     2923.95(12)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.422
_diffrn_reflns_theta_min         4.019
_diffrn_source                   'IMuS micro-focus source'
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Twinabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0680P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8008
_reflns_number_total             9574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo501841s_si_001.cif
_cod_data_source_block           compound_21
_cod_depositor_comments
'Adding full bibliography for 4029984--4029987.cif.'
_cod_database_code               4029986
_shelx_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.872
_shelxl_version_number           2013-4
_shelx_res_checksum              49230
_shelx_hkl_checksum              69299