1,8-Bis(hexamethyltriaminophosphazenyl)naphthalene, HMPN: A Superbasic Bisphosphazene "Proton Sponge"
Volker Raab; Ekaterina Gauchenova; Alexei Merkoulov; Klaus Harms; Jörg Sundermeyer; Borislav Kovačević; Zvonimir B. Maksić; Journal of the American Chemical Society 127 (2005) 15738–15743; doi:10.1021/ja052647v

data_4112048
_publ_contact_author             'Harms, Klaus.'
_publ_contact_author_email       harms@chemie.uni-marburg.de
_publ_section_title
;
 1,8-Bis(hexamethyltriaminophosphazenyl)naphthalene, HMPN: A Superbasic
 Bisphosphazene "Proton Sponge"
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15738
_journal_page_last               15743
_journal_paper_doi               10.1021/ja052647v
_journal_volume                  127
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H43 N8 P2, F6 P'
_chemical_formula_sum            'C22 H43 F6 N8 P3'
_chemical_formula_weight         626.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_creation_date             2005-03-07T15:46:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.096(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.5851(17)
_cell_length_b                   8.2464(3)
_cell_length_c                   25.6284(13)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     6064.3(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'area detector, omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30825
_diffrn_reflns_theta_full        24.89
_diffrn_reflns_theta_max         24.89
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9257
_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    1.373
_exptl_crystal_description       needle
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3534
_reflns_number_total             5262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja052647vrom20050517_091437.cif
_cod_data_source_block           cmpd4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4112048