Trispirocyclic Bis(dimethylaluminum)bis(amido)cyclodiphosph(V)azanes
Lief, Graham R.; Carrow, Christopher J.; Stahl, Lothar; Staples, Richard J.; Organometallics 20 (2001) 1629–; doi:10.1021/om000916e

data_4077248
_publ_section_title
;
 Trispirocyclic Bis(dimethylaluminum)bis(amido)cyclodiphosph(V)azanes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1629
_journal_paper_doi               10.1021/om000916e
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C20 H48 Al2 N4 O2 P2'
_chemical_formula_weight         492.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.573(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.560(2)
_cell_length_b                   7.9179(7)
_cell_length_c                   20.518(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2973.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3330
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.226
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0072(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.208
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+1.4562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                2283
_reflns_number_total             2609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000916e.cif
_cod_data_source_block           11
_cod_original_cell_volume        2973.2(6)
_cod_database_code               4077248