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_4117727
_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         '2(C37 H44 Cl2 N4 P2), 2(C2 H3 N), C Cl2'
_chemical_formula_sum            'C79 H94 Cl6 N10 P4'
_chemical_formula_weight         1520.22
_chemical_name_systematic
; 
 ? 
;
_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                65.35(3)
_cell_angle_beta                 78.17(3)
_cell_angle_gamma                88.20(3)
_cell_formula_units_Z            1
_cell_length_a                   11.562(2)
_cell_length_b                   13.418(3)
_cell_length_c                   14.712(3)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.34
_cell_volume                     2026.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f 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  0.1067
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            122062
_diffrn_reflns_theta_full        32.01
_diffrn_reflns_theta_max         32.01
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  0.9866
_exptl_absorpt_correction_T_min  0.9572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         13992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0662P)^2^+2.3895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1846
_reflns_number_gt                8205
_reflns_number_total             13992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja300587z_si_001_10.cif
_cod_data_source_block           11
_cod_original_cell_volume        2026.6(7)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4117727