Carbon-Carbon Double Bond Formation Reactions of the Unique Spirocyclic Aluminum Bis(iminophosphorano) Methandiide Complex: Insertion of Heteroallenes into Aluminum-Carbon Bonds
Kasani Aparna; Robert McDonald; Ronald G. Cavell; Journal of the American Chemical Society 122 (2000) 9314–9315; doi:10.1021/ja001445q

data_4116157
_publ_section_title
;
 Carbon-Carbon Double Bond Formation Reactions of the Unique Spirocyclic
 Aluminum Bis(iminophosphorano) Methandiide Complex: Insertion of
 Heteroallenes into Aluminum-Carbon Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9314
_journal_page_last               9315
_journal_paper_doi               10.1021/ja001445q
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C46 H65 Al2 N3 O P2 Si2'
_chemical_formula_weight         848.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.6006(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6208(6)
_cell_length_b                   18.2546(11)
_cell_length_c                   24.4927(14)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    193(2)
_cell_volume                     4667.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28813
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7113
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.8952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                6721
_reflns_number_total             8849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja001445q_1.cif
_cod_data_source_block           rgc9924
_cod_database_code               4116157