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_4116158
_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            'C55 H80 Al2 N4 P2 Si2'
_chemical_formula_weight         969.31
_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                91.0447(13)
_cell_angle_beta                 101.9669(13)
_cell_angle_gamma                109.6232(12)
_cell_formula_units_Z            2
_cell_length_a                   12.4477(9)
_cell_length_b                   13.2048(9)
_cell_length_c                   18.2357(13)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    193(2)
_cell_volume                     2749.4(3)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17573
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.9440
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         10340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0885P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                7937
_reflns_number_total             10340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja001445q_2.cif
_cod_data_source_block           rgc9926
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