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_4121218
_publ_contact_author             '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         'C50 H86 N14 P4'
_chemical_formula_sum            'C50 H86 N14 P4'
_chemical_formula_weight         1007.21
_chemical_name_common            'P2-TPPN (2)'
_chemical_name_systematic
;
1,8-Bis-[tris(pyrrolidino)phosphazenylbis(pyrrolidino)phosphazenyl]naphthalene
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Benjamin Oelkers'
_audit_contact_author_address
;
   Philipps-Universitaet Marburg, FB Chemie    
   Hans-Meerwein-Strasse
   35032 Marburg
   Germany
;
_audit_contact_author_email      jsu@staff.uni-marburg.de
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.583(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5184(6)
_cell_length_b                   14.6995(5)
_cell_length_c                   28.0986(12)
_cell_measurement_reflns_used    11105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      1.47
_cell_volume                     5112.6(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS 2'
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            21216
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  1.1487
_exptl_absorpt_correction_T_min  0.8774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.760
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.760
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                3430
_reflns_number_total             5410
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja409760z_si_002_2.cif
_cod_data_source_block           p2-tppn
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4121218