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_4112047
_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 H42 N8 P2'
_chemical_formula_sum            'C22 H42 N8 P2'
_chemical_formula_weight         480.58
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-03-07T14:24:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.179(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5264(8)
_cell_length_b                   13.6093(9)
_cell_length_c                   14.2408(8)
_cell_measurement_reflns_used    17592
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     2587.9(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18501
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.17
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  1.0659
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0007(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.9024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                2187
_reflns_number_total             2584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja052647vrom20050517_091416.cif
_cod_data_source_block           cmpd_3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4112047