#------------------------------------------------------------------------------ #$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120081 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/80/4308067.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308067 loop_ _publ_author_name 'Silke Courtenay' 'Denise Walsh' 'Sarah Hawkeswood' 'Pingrong Wei' 'Anjan Kumar Das' 'Douglas W. Stephan' _publ_section_title ; Boron and Aluminum Complexes of Sterically Demanding Phosphinimines and Phosphinimides ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3623 _journal_page_last 3631 _journal_volume 46 _journal_year 2007 _chemical_formula_sum 'C24 H58 Al2 N2 P2' _chemical_formula_weight 490.62 _space_group_IT_number 205 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.486(4) _cell_length_b 14.486(4) _cell_length_c 14.486(4) _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 2.0 _cell_volume 3039.8(15) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 12178 _diffrn_reflns_theta_full 23.25 _diffrn_reflns_theta_max 23.25 _diffrn_reflns_theta_min 2.44 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_T_max 0.256608 _exptl_absorpt_correction_T_min 0.150057 _exptl_absorpt_correction_type empirical _exptl_crystal_density_diffrn 1.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.215 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 56 _refine_ls_number_reflns 732 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0482 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+1.2622P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1423 _refine_ls_wR_factor_ref 0.1527 _reflns_number_gt 559 _reflns_number_total 732 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic0700351si20070111_011533_4.cif _[local]_cod_data_source_block '[(?-t-Bu3PN)AlH2]2' _cod_original_cell_volume 3039.5(14) _cod_database_code 4308067 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al -0.07466(16) 0.5308(2) 0.95458(19) 0.0506(7) Uani 0.33 1 d P . . P1 P 0.11704(4) 0.61704(4) 0.88296(4) 0.0373(5) Uani 1 3 d S . . N1 N 0.05336(14) 0.55336(14) 0.94664(14) 0.0467(11) Uani 1 3 d S . . C1 C 0.1314(2) 0.5625(2) 0.76451(19) 0.0620(10) Uani 1 1 d . . . C2 C 0.1549(4) 0.4601(3) 0.7746(3) 0.127(2) Uani 1 1 d . . . H2A H 0.1617 0.4330 0.7145 0.191 Uiso 1 1 calc R . . H2B H 0.1061 0.4294 0.8073 0.191 Uiso 1 1 calc R . . H2C H 0.2116 0.4537 0.8083 0.191 Uiso 1 1 calc R . . C3 C 0.0403(3) 0.5646(4) 0.7110(3) 0.129(2) Uani 1 1 d . . . H3A H 0.0490 0.5368 0.6515 0.194 Uiso 1 1 calc R . . H3B H 0.0206 0.6274 0.7034 0.194 Uiso 1 1 calc R . . H3C H -0.0058 0.5309 0.7446 0.194 Uiso 1 1 calc R . . C4 C 0.2052(3) 0.6073(3) 0.7025(3) 0.1089(16) Uani 1 1 d . . . H4A H 0.2074 0.5756 0.6443 0.163 Uiso 1 1 calc R . . H4B H 0.2644 0.6032 0.7321 0.163 Uiso 1 1 calc R . . H4C H 0.1900 0.6710 0.6924 0.163 Uiso 1 1 calc R . . H1 H -0.149(4) 0.604(4) 1.001(4) 0.099(17) Uiso 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0326(13) 0.0593(15) 0.0597(17) 0.0260(11) -0.0023(12) -0.0025(13) P1 0.0373(5) 0.0373(5) 0.0373(5) 0.0030(3) 0.0030(3) -0.0030(3) N1 0.0467(11) 0.0467(11) 0.0467(11) 0.0059(10) 0.0059(10) -0.0059(10) C1 0.077(2) 0.065(2) 0.0435(17) -0.0073(14) 0.0152(15) -0.0150(16) C2 0.208(6) 0.073(3) 0.101(3) -0.031(3) 0.037(4) 0.007(3) C3 0.113(4) 0.217(6) 0.058(2) -0.031(3) -0.011(2) -0.049(4) C4 0.134(4) 0.121(3) 0.072(2) -0.021(2) 0.057(3) -0.041(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Al1 Al1 Al1 119.962(13) 20_466 23_656 ? Al1 Al1 N1 70.01(13) 20_466 . ? Al1 Al1 N1 70.01(13) 23_656 . ? Al1 Al1 N1 68.52(13) 20_466 13_567 ? Al1 Al1 N1 68.52(13) 23_656 13_567 ? N1 Al1 N1 89.86(19) . 13_567 ? Al1 Al1 Al1 90.000(1) 20_466 8_656 ? Al1 Al1 Al1 30.019(7) 23_656 8_656 ? N1 Al1 Al1 51.96(8) . 8_656 ? N1 Al1 Al1 52.40(8) 13_567 8_656 ? Al1 Al1 Al1 30.019(6) 20_466 11_466 ? Al1 Al1 Al1 90.000(1) 23_656 11_466 ? N1 Al1 Al1 51.96(8) . 11_466 ? N1 Al1 Al1 52.40(8) 13_567 11_466 ? Al1 Al1 Al1 60.0 8_656 11_466 ? Al1 Al1 Al1 59.995(2) 20_466 13_567 ? Al1 Al1 Al1 59.995(1) 23_656 13_567 ? N1 Al1 Al1 45.21(11) . 13_567 ? N1 Al1 Al1 44.65(11) 13_567 13_567 ? Al1 Al1 Al1 30.005(2) 8_656 13_567 ? Al1 Al1 Al1 30.005(2) 11_466 13_567 ? N1 P1 C1 110.14(10) . . ? N1 P1 C1 110.14(10) . 8_656 ? C1 P1 C1 108.79(10) . 8_656 ? N1 P1 C1 110.14(10) . 11_466 ? C1 P1 C1 108.79(10) . 11_466 ? C1 P1 C1 108.79(10) 8_656 11_466 ? P1 N1 Al1 134.65(11) . . ? P1 N1 Al1 134.65(11) . 8_656 ? Al1 N1 Al1 76.07(17) . 8_656 ? P1 N1 Al1 134.65(11) . 11_466 ? Al1 N1 Al1 76.07(17) . 11_466 ? Al1 N1 Al1 76.07(17) 8_656 11_466 ? P1 N1 Al1 135.21(10) . 23_656 ? Al1 N1 Al1 41.47(7) . 23_656 ? Al1 N1 Al1 41.47(7) 8_656 23_656 ? Al1 N1 Al1 90.14(19) 11_466 23_656 ? P1 N1 Al1 135.21(10) . 13_567 ? Al1 N1 Al1 90.14(19) . 13_567 ? Al1 N1 Al1 41.47(7) 8_656 13_567 ? Al1 N1 Al1 41.47(7) 11_466 13_567 ? Al1 N1 Al1 75.20(16) 23_656 13_567 ? P1 N1 Al1 135.21(10) . 20_466 ? Al1 N1 Al1 41.47(7) . 20_466 ? Al1 N1 Al1 90.14(19) 8_656 20_466 ? Al1 N1 Al1 41.47(7) 11_466 20_466 ? Al1 N1 Al1 75.20(16) 23_656 20_466 ? Al1 N1 Al1 75.20(16) 13_567 20_466 ? C2 C1 C3 105.0(4) . . ? C2 C1 C4 108.0(3) . . ? C3 C1 C4 107.2(3) . . ? C2 C1 P1 110.0(2) . . ? C3 C1 P1 110.8(3) . . ? C4 C1 P1 115.3(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 Al1 1.342(2) 20_466 ? Al1 Al1 1.342(2) 23_656 ? Al1 N1 1.887(3) . ? Al1 N1 1.905(3) 13_567 ? Al1 Al1 2.325(4) 8_656 ? Al1 Al1 2.325(4) 11_466 ? Al1 Al1 2.685(5) 13_567 ? P1 N1 1.598(4) . ? P1 C1 1.900(3) . ? P1 C1 1.900(3) 8_656 ? P1 C1 1.900(3) 11_466 ? N1 Al1 1.887(3) 8_656 ? N1 Al1 1.887(3) 11_466 ? N1 Al1 1.905(3) 23_656 ? N1 Al1 1.905(3) 13_567 ? N1 Al1 1.905(3) 20_466 ? C1 C2 1.529(5) . ? C1 C3 1.531(5) . ? C1 C4 1.541(5) . ? _journal_paper_doi 10.1021/ic0700351