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_4121219
_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         'C34 H55 N8 P2, C2 F6 N O4 S2'
_chemical_formula_sum            'C36 H55 F6 N9 O4 P2 S2'
_chemical_formula_weight         917.97
_chemical_name_common            'TPPN x HN(SO2CF3)2'
_chemical_name_systematic
;
1,8-Bis(trispyrrolidinophosphazenyl)naphthalene x HN(SO2CF3)2
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.6867(8)
_cell_length_b                   17.8745(6)
_cell_length_c                   26.9816(8)
_cell_measurement_reflns_used    13987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      1.62
_cell_volume                     8530.0(5)
_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
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1764
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42020
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.92
_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    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.687
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         17843
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.690
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                7383
_reflns_number_total             17843
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja409760z_si_002_3.cif
_cod_data_source_block           jfk61
_cod_original_formula_sum        'C36 H55 F6 N9 O4 P2 S2 '
_cod_database_code               4121219