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_7112248
_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_absolute_configuration syn
_chemical_formula_moiety         'C62 H98 Al N14 P4, C4 H12 Al'
_chemical_formula_sum            'C66 H110 Al2 N14 P4'
_chemical_formula_weight         1277.53
_chemical_name_common            'Binaph-P2-Pyrx2AlMe3 ([4-AlMe2]+[AlMe4]-)'
_chemical_name_systematic
;

(1S)-[1,1'-Binaphthalene]-2,2'-diamine,N2,N2'-bis([tris-(pyrrolidinyl)phosphazenyl]bis(pyrrolidinyl)phosphoranylidene) x 2AlMe3
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 116.309(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.751(3)
_cell_length_b                   33.100(7)
_cell_length_c                   10.900(3)
_cell_measurement_reflns_used    12204
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.17
_cell_volume                     3477.1(16)
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_sigmaI/netI    0.1588
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25958
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         12333
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0613P)^2^+0.2610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                8399
_reflns_number_total             12333
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4cc00773e2.cif
_cod_data_source_block           jfk548_0m
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_database_code               7112248
_audit_contact_author            'Joerg Sundermeyer'