A New Synthetic Pathway to the Second and Third Generation of Superbasic Bisphosphazene Proton Sponges: The Run for the Best Chelating Ligand for a Proton
Julius F. Kögel; Benjamin Oelkers; Borislav Kovačević; Jörg Sundermeyer; Journal of the American Chemical Society 135 (2013) 17768–17774; doi:10.1021/ja409760z

data_4121217
_publ_contact_author_address
;
   Philipps-Universitaet Marburg, FB Chemie    
   Hans-Meerwein-Strasse
   35032 Marburg
   Germany
;
_publ_contact_author_email       jsu@staff.uni-marburg.de
_publ_contact_author_name        'Joerg Sundermeyer'
_publ_section_title
;
 A New Synthetic Pathway to the Second and Third Generation of Superbasic
 Bisphosphazene Proton Sponges: The Run for the Best Chelating Ligand for
 a Proton
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17768
_journal_page_last               17774
_journal_paper_doi               10.1021/ja409760z
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C34 H54 N8 P2, C2 H3 N'
_chemical_formula_sum            'C36 H57 N9 P2'
_chemical_formula_weight         677.85
_chemical_name_common            'TPPN (1)'
_chemical_name_systematic
;
1,8-Bis(trispyrrolidinophosphazenyl)naphthalene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.427(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2714(17)
_cell_length_b                   13.8754(12)
_cell_length_c                   16.5807(15)
_cell_measurement_reflns_used    8033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      1.96
_cell_volume                     3625.4(6)
_computing_cell_refinement       'APEX2 v2012.10-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics
;
K. Brandenburg, H. Putz: 
Diamond - Crystal and Molecular Structure Visualization v3.2i, 
Crystal Impact GbR, Bonn, Germany, 2012
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
SIR97 (A. Altomare, M. C. Burla, M. Camalli, G. Cascarano, C. Giacovazzo, 
A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna, 
J. Appl. Crystallogr. 1999, 32, 115-119.)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_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  0.1010
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38686
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+1.3463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                4561
_reflns_number_total             6379
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja409760z_si_002_1.cif
_cod_data_source_block           jfk501a_0m
_cod_database_code               4121217