Synthesis of an Aluminum Spirocyclic Hybrid with an Inorganic B2O3 and an Organic C3N2 Core
Zhi Yang; Xiaoli Ma; Rainer B. Oswald; Herbert W. Roesky; Mathias Noltemeyer; Journal of the American Chemical Society 128 (2006) 12406–12407; doi:10.1021/ja064035w

data_4110913
_publ_section_title
;
 Synthesis of an Aluminum Spirocyclic Hybrid with an Inorganic B2O3 and an
 Organic C3N2 Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12406
_journal_page_last               12407
_journal_paper_doi               10.1021/ja064035w
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C41 H51 Al B2 N2 O3'
_chemical_formula_weight         668.44
_chemical_name_systematic
; 
 ? 
;
_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                74.936(13)
_cell_angle_beta                 76.052(13)
_cell_angle_gamma                74.564(13)
_cell_formula_units_Z            2
_cell_length_a                   11.436(2)
_cell_length_b                   12.091(2)
_cell_length_c                   15.359(3)
_cell_measurement_temperature    133(2)
_cell_volume                     1942.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  IPDS2
_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  0.3176
_diffrn_reflns_av_sigmaI/netI    0.4025
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20290
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9955
_exptl_absorpt_correction_T_min  0.9910
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.815
_refine_ls_R_factor_all          0.2753
_refine_ls_R_factor_gt           0.0912
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                1955
_reflns_number_total             6644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064035wsi20060608_085133.cif
_cod_data_source_block           r1198
_cod_database_code               4110913