Synthesis, Reactivity, and Computational Analysis of Halophosphines Supported by Dianionic Guanidinate Ligands
Allison L. Brazeau; Mikko M. Hänninen; Heikki M. Tuononen; Nathan D. Jones; Paul J. Ragogna; Journal of the American Chemical Society 134 (2012) 5398–5414; doi:10.1021/ja300587z

data_4117720
_publ_contact_author_address
;
Department of Chemistry, The University of Western Ontario, 
1151 Richmond St., London, Ontario, N6A 5B7, Canada
;
_publ_contact_author_email       pragogna@uwo.ca
_publ_contact_author_fax         519-661-3022
_publ_contact_author_name        'Paul J. Ragogna'
_publ_contact_author_phone       '519-661-2111 x 87048'
_publ_section_title
;
 Synthesis, Reactivity, and Computational Analysis of Halophosphines
 Supported by Dianionic Guanidinate Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5398
_journal_page_last               5414
_journal_paper_doi               10.1021/ja300587z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C37 H51 Cl N3 P'
_chemical_formula_sum            'C37 H51 Cl N3 P'
_chemical_formula_weight         604.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.42(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.829(3)
_cell_length_b                   11.199(2)
_cell_length_c                   24.175(8)
_cell_measurement_reflns_used    37104
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     3492.3(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL/PC (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans'
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21313
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.9351
_exptl_absorpt_correction_T_min  0.9252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       0.033(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0550
_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^)+(0.1051P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                4298
_reflns_number_total             6230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300587z_si_001_03.cif
_cod_data_source_block           2PCl
_cod_original_cell_volume        3492.3(15)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4117720