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_4121220
_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         'C52 H87 F6 N15 O4 P4 S2'
_chemical_formula_sum            'C52 H87 F6 N15 O4 P4 S2'
_chemical_formula_weight         1288.37
_chemical_name_common            'P2-TPPN (2) x HN(SO2CF3)2'
_chemical_name_systematic
;
1,8-Bis-[tris(pyrrolidino)phosphazenylbis(pyrrolidino)phosphazenyl]naphthalene 
x HN(SO2CF3)2
;
_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_author_name               'Julius K\"ogel'
_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                 95.424(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.826(3)
_cell_length_b                   32.917(8)
_cell_length_c                   14.386(3)
_cell_measurement_reflns_used    13230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.02
_cell_volume                     6046(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1074
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58477
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         10589
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+6.9754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                7210
_reflns_number_total             10589
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja409760z_si_002_4.cif
_cod_data_source_block           jfk178_0m
_cod_original_cell_volume        6046(3)
_cod_database_code               4121220