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_7112247
_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         'C40 H72 N14 P4'
_chemical_formula_sum            'C40 H72 N14 P4'
_chemical_formula_weight         873.00
_chemical_name_common            'Binaph-P2-NMe2 (3)'
_chemical_name_systematic
;

(1S)-[1,1'-Binaphthalene]-2,2'-diamine,N2,N2'-bis([tris-(dimethylamino)phosphazenyl]bis(dimethylamino)phosphoranylidene)
;
_space_group_IT_number           1
_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                87.901(4)
_cell_angle_beta                 89.867(4)
_cell_angle_gamma                82.976(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5097(10)
_cell_length_b                   13.3588(14)
_cell_length_c                   16.9068(17)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0861
_cell_measurement_theta_min      2.6019
_cell_volume                     2354.3(4)
_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 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15745
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.13(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         11795
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+7.9934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                10327
_reflns_number_total             11795
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc00773e2.cif
_cod_data_source_block           nkjk19
_cod_database_code               7112247