Two C2-symmetric chelating P2-bisphosphazene superbases connected via a binaphthyl backbone - synthesis, structural features and preparation of a cationic alkyl aluminum complex
Julius F. Kogel; Nis-Julian Kneusels; Jorg Sundermeyer; Chem.Commun. 50 (2014) 4319–; doi:10.1039/C4CC00773E

data_7112249
_publ_section_title
;
 Two C2-symmetric chelating P2-bisphosphazene superbases connected via a
 binaphthyl backbone - synthesis, structural features and preparation of a
 cationic alkyl aluminum complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              4319
_journal_paper_doi               10.1039/C4CC00773E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C10 H30 Br N6 P2, Br'
_chemical_formula_sum            'C10 H30 Br2 N6 P2'
_chemical_formula_weight         456.16
_chemical_name_common            '(Pyr)3P=N-P(Pyr)2Br2 (1)'
_chemical_name_systematic
;

[tris(pyrrolidinyl)phosphazenyl]bis(pyrrolidinyl)bromophosphonium bromide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.141(5)
_cell_angle_beta                 92.459(5)
_cell_angle_gamma                94.663(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1153(5)
_cell_length_b                   9.5111(6)
_cell_length_c                   13.1754(9)
_cell_measurement_reflns_used    12209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      1.63
_cell_volume                     960.70(11)
_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 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11610
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.65
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    4.387
_exptl_absorpt_correction_T_max  0.5252
_exptl_absorpt_correction_T_min  0.2588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0599
_reflns_number_gt                3582
_reflns_number_total             4040
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc00773e2.cif
_cod_data_source_block           p2nme2br2
_cod_original_cell_volume        960.71(11)
_cod_database_code               7112249
_audit_contact_author            'Joerg Sundermeyer'