Guanidinophosphazenes: Design, Synthesis, and Basicity in THF and in the Gas Phase
Alexander A. Kolomeitsev; Ilmar A. Koppel; Toomas Rodima; Jan Barten; Enno Lork; Gerd-Volker Röschenthaler; Ivari Kaljurand; Agnes Kütt; Ivar Koppel; Vahur Mäemets; Ivo Leito; Journal of the American Chemical Society 127 (2005) 17656–17666; doi:10.1021/ja053543n

data_4112115
_publ_section_title
;
 Guanidinophosphazenes: Design, Synthesis, and Basicity in THF and in the
 Gas Phase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17656
_journal_page_last               17666
_journal_paper_doi               10.1021/ja053543n
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C19 H46 N10 P, B F4'
_chemical_formula_sum            'C19 H46 B F4 N10 P'
_chemical_formula_weight         532.44
_chemical_name_systematic
; 
 ? 
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.923(2)
_cell_length_b                   28.409(3)
_cell_length_c                   16.285(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.512
_cell_measurement_theta_min      5.037
_cell_volume                     5695.4(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15389
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          1.0
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0021(4)
_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   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         12895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0981P)^2^+3.8353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1908
_reflns_number_gt                8995
_reflns_number_total             12895
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja053543nsi20050613_103444.cif
_cod_data_source_block           ak302
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4112115