#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:50:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179131 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/93/4309310.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_4309310
loop_
_publ_author_name
'Andreas Stasch'
'Herbert W. Roesky'
'Mathias Noltemeyer'
'Hans-Georg Schmidt'
_publ_section_title
;
Aluminum Hydride Cations Stabilized by Weakly Coordinating Carbaalanates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5854
_journal_page_last               5857
_journal_paper_doi               10.1021/ic048594k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C48 H114 Al10 N4'
_chemical_formula_weight         1017.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.375(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.013(3)
_cell_length_b                   15.676(4)
_cell_length_c                   16.321(3)
_cell_measurement_temperature    133(2)
_cell_volume                     3319.6(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE 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  0.1384
_diffrn_reflns_av_sigmaI/netI    0.1140
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26812
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_correction_T_min  0.9314
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5663
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.0846
_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/[σ²(Fo²)+(0.0353P)²+20.4000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2182
_reflns_number_gt                3287
_reflns_number_total             5663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048594ksi20041008_051025.cif
_cod_data_source_block           r1131a
_cod_original_cell_volume        3319.9(13)
_cod_database_code               4309310
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-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 0.84838(14) 0.97298(13) -0.06420(12) 0.0219(4) Uani 1 1 d D . .
Al2 Al 1.05084(14) 0.88698(13) 0.07564(12) 0.0222(4) Uani 1 1 d D . .
Al3 Al 0.98738(14) 1.11549(13) 0.08419(11) 0.0214(4) Uani 1 1 d D . .
Al4 Al 0.88213(14) 0.97330(13) 0.09501(12) 0.0234(5) Uani 1 1 d D . .
C1 C 0.9093(4) 0.8781(4) 0.0081(4) 0.0203(13) Uani 1 1 d . . .
C10 C 0.8665(5) 0.7874(4) 0.0229(4) 0.0285(15) Uani 1 1 d . . .
H10A H 0.9155 0.7464 0.0011 0.034 Uiso 1 1 calc R . .
H10B H 0.8699 0.7788 0.0831 0.034 Uiso 1 1 calc R . .
C11 C 0.7582(5) 0.7604(4) -0.0110(4) 0.0299(16) Uani 1 1 d . . .
C12 C 0.6772(5) 0.8216(5) 0.0176(5) 0.046(2) Uani 1 1 d . . .
H12A H 0.6891 0.8307 0.0769 0.068 Uiso 1 1 calc R . .
H12B H 0.6084 0.7972 0.0052 0.068 Uiso 1 1 calc R . .
H12C H 0.6819 0.8762 -0.0111 0.068 Uiso 1 1 calc R . .
C13 C 0.7501(6) 0.7569(5) -0.1059(4) 0.0398(19) Uani 1 1 d . . .
H13A H 0.6799 0.7406 -0.1259 0.060 Uiso 1 1 calc R . .
H13B H 0.7990 0.7147 -0.1243 0.060 Uiso 1 1 calc R . .
H13C H 0.7663 0.8131 -0.1278 0.060 Uiso 1 1 calc R . .
C14 C 0.7365(6) 0.6710(5) 0.0214(6) 0.053(2) Uani 1 1 d . . .
H14A H 0.7384 0.6725 0.0815 0.079 Uiso 1 1 calc R . .
H14B H 0.7890 0.6313 0.0045 0.079 Uiso 1 1 calc R . .
H14C H 0.6683 0.6521 -0.0010 0.079 Uiso 1 1 calc R . .
C2 C 1.0328(5) 0.9994(4) 0.1384(4) 0.0205(14) Uani 1 1 d . . .
C20 C 1.0793(5) 1.0049(5) 0.2294(4) 0.0297(16) Uani 1 1 d . . .
H20A H 1.1366 0.9632 0.2352 0.036 Uiso 1 1 calc R . .
H20B H 1.1108 1.0622 0.2365 0.036 Uiso 1 1 calc R . .
C21 C 1.0142(6) 0.9909(5) 0.3022(4) 0.0339(17) Uani 1 1 d . . .
C22 C 0.9691(6) 0.8994(5) 0.3004(5) 0.047(2) Uani 1 1 d . . .
H22A H 0.9165 0.8942 0.2545 0.070 Uiso 1 1 calc R . .
H22B H 0.9379 0.8881 0.3521 0.070 Uiso 1 1 calc R . .
H22C H 1.0243 0.8581 0.2937 0.070 Uiso 1 1 calc R . .
C23 C 1.0830(7) 1.0014(6) 0.3824(4) 0.055(3) Uani 1 1 d . . .
H23A H 1.1115 1.0593 0.3853 0.082 Uiso 1 1 calc R . .
H23B H 1.1395 0.9599 0.3836 0.082 Uiso 1 1 calc R . .
H23C H 1.0419 0.9916 0.4294 0.082 Uiso 1 1 calc R . .
C24 C 0.9257(6) 1.0551(5) 0.3018(4) 0.043(2) Uani 1 1 d . . .
H24A H 0.9534 1.1132 0.2999 0.064 Uiso 1 1 calc R . .
H24B H 0.8893 1.0480 0.3517 0.064 Uiso 1 1 calc R . .
H24C H 0.8778 1.0453 0.2534 0.064 Uiso 1 1 calc R . .
C3 C 0.8565(5) 1.0773(4) 0.0157(4) 0.0233(14) Uani 1 1 d . . .
C30 C 0.7445(5) 1.1153(5) 0.0125(4) 0.0285(16) Uani 1 1 d . . .
H30A H 0.7242 1.1290 -0.0457 0.034 Uiso 1 1 calc R . .
H30B H 0.6983 1.0688 0.0284 0.034 Uiso 1 1 calc R . .
C31 C 0.7195(5) 1.1943(5) 0.0637(4) 0.0282(16) Uani 1 1 d . . .
C32 C 0.6042(5) 1.2113(5) 0.0470(5) 0.043(2) Uani 1 1 d . . .
H32A H 0.5840 1.2589 0.0812 0.065 Uiso 1 1 calc R . .
H32B H 0.5654 1.1601 0.0601 0.065 Uiso 1 1 calc R . .
H32C H 0.5892 1.2257 -0.0111 0.065 Uiso 1 1 calc R . .
C33 C 0.7791(6) 1.2721(5) 0.0381(5) 0.0401(19) Uani 1 1 d . . .
H33A H 0.7576 1.3222 0.0684 0.060 Uiso 1 1 calc R . .
H33B H 0.7649 1.2818 -0.0210 0.060 Uiso 1 1 calc R . .
H33C H 0.8530 1.2625 0.0504 0.060 Uiso 1 1 calc R . .
C34 C 0.7419(5) 1.1782(5) 0.1561(4) 0.0344(18) Uani 1 1 d . . .
H34A H 0.7176 1.2268 0.1870 0.052 Uiso 1 1 calc R . .
H34B H 0.8162 1.1710 0.1686 0.052 Uiso 1 1 calc R . .
H34C H 0.7060 1.1263 0.1717 0.052 Uiso 1 1 calc R . .
Al5 Al 0.47568(18) 1.03463(15) -0.32727(14) 0.0375(6) Uani 1 1 d D . .
N51 N 0.5498(5) 0.9242(4) -0.3253(3) 0.0339(14) Uani 1 1 d . . .
N52 N 0.5002(4) 1.0982(4) -0.2230(3) 0.0292(13) Uani 1 1 d . . .
C51 C 0.5361(6) 0.8959(5) -0.4124(5) 0.045(2) Uani 1 1 d . . .
H51A H 0.5626 0.8377 -0.4170 0.068 Uiso 1 1 calc R . .
H51B H 0.5740 0.9343 -0.4466 0.068 Uiso 1 1 calc R . .
H51C H 0.4627 0.8970 -0.4310 0.068 Uiso 1 1 calc R . .
C52 C 0.5008(9) 0.8597(6) -0.2734(6) 0.079(3) Uani 1 1 d . . .
H52A H 0.5347 0.8044 -0.2788 0.118 Uiso 1 1 calc R . .
H52B H 0.4275 0.8545 -0.2914 0.118 Uiso 1 1 calc R . .
H52C H 0.5081 0.8779 -0.2158 0.118 Uiso 1 1 calc R . .
C53 C 0.6607(6) 0.9304(7) -0.3032(6) 0.060(3) Uani 1 1 d . . .
H53A H 0.6936 0.8757 -0.3138 0.090 Uiso 1 1 calc R . .
H53B H 0.6725 0.9446 -0.2447 0.090 Uiso 1 1 calc R . .
H53C H 0.6903 0.9751 -0.3361 0.090 Uiso 1 1 calc R . .
C54 C 0.4883(6) 1.0485(5) -0.1474(5) 0.042(2) Uani 1 1 d . . .
H54A H 0.4870 1.0874 -0.1005 0.063 Uiso 1 1 calc R . .
H54B H 0.5463 1.0089 -0.1383 0.063 Uiso 1 1 calc R . .
H54C H 0.4237 1.0162 -0.1534 0.063 Uiso 1 1 calc R . .
C55 C 0.6033(6) 1.1411(6) -0.2171(5) 0.046(2) Uani 1 1 d . . .
H55A H 0.6110 1.1752 -0.1667 0.069 Uiso 1 1 calc R . .
H55B H 0.6086 1.1783 -0.2649 0.069 Uiso 1 1 calc R . .
H55C H 0.6577 1.0978 -0.2160 0.069 Uiso 1 1 calc R . .
C56 C 0.4191(6) 1.1653(5) -0.2304(5) 0.044(2) Uani 1 1 d . . .
H56A H 0.4349 1.2095 -0.1889 0.065 Uiso 1 1 calc R . .
H56B H 0.3520 1.1397 -0.2218 0.065 Uiso 1 1 calc R . .
H56C H 0.4168 1.1907 -0.2853 0.065 Uiso 1 1 calc R . .
H1 H 0.748(3) 0.978(4) -0.119(3) 0.027(17) Uiso 1 1 d D . .
H2 H 1.091(4) 0.814(3) 0.133(3) 0.020(16) Uiso 1 1 d D . .
H3 H 0.990(4) 1.190(3) 0.146(3) 0.018(16) Uiso 1 1 d D . .
H4 H 0.364(3) 1.003(4) -0.337(4) 0.032(18) Uiso 1 1 d D . .
H5 H 0.529(4) 1.092(3) -0.386(3) 0.020(16) Uiso 1 1 d D . .
H4A H 0.796(5) 0.957(6) 0.153(5) 0.09(3) Uiso 1 1 d D . .
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'
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
C1 Al1 C2 102.6(3) . 3_775 ?
C1 Al1 C3 102.3(3) . . ?
C2 Al1 C3 101.3(3) 3_775 . ?
C1 Al1 Al2 119.4(2) . 3_775 ?
C2 Al1 Al2 51.27(19) 3_775 3_775 ?
C3 Al1 Al2 51.33(19) . 3_775 ?
C1 Al1 Al3 52.34(18) . 3_775 ?
C2 Al1 Al3 51.77(18) 3_775 3_775 ?
C3 Al1 Al3 119.65(19) . 3_775 ?
Al2 Al1 Al3 91.01(9) 3_775 3_775 ?
C1 Al1 Al4 52.41(18) . . ?
C2 Al1 Al4 120.31(19) 3_775 . ?
C3 Al1 Al4 51.57(19) . . ?
Al2 Al1 Al4 91.30(9) 3_775 . ?
Al3 Al1 Al4 92.80(9) 3_775 . ?
C2 Al2 C3 102.8(3) . 3_775 ?
C2 Al2 C1 101.0(2) . . ?
C3 Al2 C1 100.2(3) 3_775 . ?
C2 Al2 Al1 52.00(18) . 3_775 ?
C3 Al2 Al1 52.19(19) 3_775 3_775 ?
C1 Al2 Al1 117.1(2) . 3_775 ?
C2 Al2 Al3 119.2(2) . 3_775 ?
C3 Al2 Al3 50.32(19) 3_775 3_775 ?
C1 Al2 Al3 51.47(17) . 3_775 ?
Al1 Al2 Al3 89.97(9) 3_775 3_775 ?
C2 Al2 Al4 50.93(18) . . ?
C3 Al2 Al4 119.2(2) 3_775 . ?
C1 Al2 Al4 51.78(17) . . ?
Al1 Al2 Al4 90.26(9) 3_775 . ?
Al3 Al2 Al4 91.75(9) 3_775 . ?
C3 Al3 C2 99.9(3) . . ?
C3 Al3 C1 100.0(3) . 3_775 ?
C2 Al3 C1 99.8(2) . 3_775 ?
C3 Al3 Al1 115.7(2) . 3_775 ?
C2 Al3 Al1 51.49(17) . 3_775 ?
C1 Al3 Al1 49.79(17) 3_775 3_775 ?
C3 Al3 Al2 50.71(19) . 3_775 ?
C2 Al3 Al2 115.81(19) . 3_775 ?
C1 Al3 Al2 50.84(17) 3_775 3_775 ?
Al1 Al3 Al2 87.85(9) 3_775 3_775 ?
C3 Al3 Al4 51.30(19) . . ?
C2 Al3 Al4 50.58(18) . . ?
C1 Al3 Al4 117.06(19) 3_775 . ?
Al1 Al3 Al4 89.63(9) 3_775 . ?
Al2 Al3 Al4 89.66(9) 3_775 . ?
C2 Al4 C3 99.2(3) . . ?
C2 Al4 C1 99.6(2) . . ?
C3 Al4 C1 99.3(3) . . ?
C2 Al4 Al1 115.14(19) . . ?
C3 Al4 Al1 51.47(19) . . ?
C1 Al4 Al1 49.51(18) . . ?
C2 Al4 Al2 50.48(18) . . ?
C3 Al4 Al2 115.04(19) . . ?
C1 Al4 Al2 50.77(17) . . ?
Al1 Al4 Al2 87.57(9) . . ?
C2 Al4 Al3 51.11(18) . . ?
C3 Al4 Al3 49.98(18) . . ?
C1 Al4 Al3 116.12(19) . . ?
Al1 Al4 Al3 89.06(9) . . ?
Al2 Al4 Al3 89.09(8) . . ?
C10 C1 Al1 129.4(4) . . ?
C10 C1 Al2 107.0(4) . . ?
Al1 C1 Al2 123.5(3) . . ?
C10 C1 Al3 114.4(4) . 3_775 ?
Al1 C1 Al3 77.9(2) . 3_775 ?
Al2 C1 Al3 77.7(2) . 3_775 ?
C10 C1 Al4 117.6(4) . . ?
Al1 C1 Al4 78.1(2) . . ?
Al2 C1 Al4 77.5(2) . . ?
Al3 C1 Al4 126.8(3) 3_775 . ?
C11 C10 C1 121.8(6) . . ?
C12 C11 C14 108.7(6) . . ?
C12 C11 C10 110.7(6) . . ?
C14 C11 C10 108.5(6) . . ?
C12 C11 C13 109.4(6) . . ?
C14 C11 C13 108.3(6) . . ?
C10 C11 C13 111.2(6) . . ?
C20 C2 Al2 118.0(4) . . ?
C20 C2 Al4 128.6(4) . . ?
Al2 C2 Al4 78.6(2) . . ?
C20 C2 Al1 106.9(4) . 3_775 ?
Al2 C2 Al1 76.7(2) . 3_775 ?
Al4 C2 Al1 124.5(3) . 3_775 ?
C20 C2 Al3 115.5(4) . . ?
Al2 C2 Al3 125.0(3) . . ?
Al4 C2 Al3 78.3(2) . . ?
Al1 C2 Al3 76.7(2) 3_775 . ?
C21 C20 C2 122.2(6) . . ?
C20 C21 C24 111.4(6) . . ?
C20 C21 C23 109.0(6) . . ?
C24 C21 C23 108.8(6) . . ?
C20 C21 C22 110.6(6) . . ?
C24 C21 C22 108.9(6) . . ?
C23 C21 C22 108.0(6) . . ?
C30 C3 Al3 129.5(4) . . ?
C30 C3 Al2 117.7(5) . 3_775 ?
Al3 C3 Al2 79.0(2) . 3_775 ?
C30 C3 Al1 105.8(4) . . ?
Al3 C3 Al1 124.7(3) . . ?
Al2 C3 Al1 76.5(2) 3_775 . ?
C30 C3 Al4 114.7(4) . . ?
Al3 C3 Al4 78.7(2) . . ?
Al2 C3 Al4 125.7(3) 3_775 . ?
Al1 C3 Al4 77.0(2) . . ?
C31 C30 C3 121.3(5) . . ?
C33 C31 C32 109.0(6) . . ?
C33 C31 C34 109.8(6) . . ?
C32 C31 C34 108.3(6) . . ?
C33 C31 C30 111.3(6) . . ?
C32 C31 C30 106.7(5) . . ?
C34 C31 C30 111.6(6) . . ?
N52 Al5 N51 112.4(3) . . ?
C53 N51 C51 107.4(6) . . ?
C53 N51 C52 111.1(7) . . ?
C51 N51 C52 108.4(7) . . ?
C53 N51 Al5 114.5(5) . . ?
C51 N51 Al5 102.9(5) . . ?
C52 N51 Al5 111.9(5) . . ?
C54 N52 C56 108.7(5) . . ?
C54 N52 C55 109.5(6) . . ?
C56 N52 C55 108.4(6) . . ?
C54 N52 Al5 115.6(5) . . ?
C56 N52 Al5 102.7(4) . . ?
C55 N52 Al5 111.5(4) . . ?
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 C1 2.023(6) . ?
Al1 C2 2.082(6) 3_775 ?
Al1 C3 2.089(7) . ?
Al1 Al2 2.571(3) 3_775 ?
Al1 Al3 2.589(3) 3_775 ?
Al1 Al4 2.602(3) . ?
Al2 C2 2.061(7) . ?
Al2 C3 2.065(7) 3_775 ?
Al2 C1 2.078(6) . ?
Al2 Al1 2.571(3) 3_775 ?
Al2 Al3 2.619(3) 3_775 ?
Al2 Al4 2.619(3) . ?
Al3 C3 2.053(7) . ?
Al3 C2 2.090(7) . ?
Al3 C1 2.097(6) 3_775 ?
Al3 Al1 2.589(3) 3_775 ?
Al3 Al2 2.618(3) 3_775 ?
Al3 Al4 2.629(3) . ?
Al4 C2 2.074(6) . ?
Al4 C3 2.092(7) . ?
Al4 C1 2.107(6) . ?
C1 C10 1.552(9) . ?
C1 Al3 2.097(6) 3_775 ?
C10 C11 1.534(9) . ?
C11 C12 1.526(10) . ?
C11 C14 1.531(10) . ?
C11 C13 1.546(10) . ?
C2 C20 1.562(9) . ?
C2 Al1 2.082(6) 3_775 ?
C20 C21 1.527(9) . ?
C21 C24 1.530(10) . ?
C21 C23 1.537(10) . ?
C21 C22 1.549(11) . ?
C3 C30 1.572(8) . ?
C3 Al2 2.065(7) 3_775 ?
C30 C31 1.542(9) . ?
C31 C33 1.520(10) . ?
C31 C32 1.529(9) . ?
C31 C34 1.536(10) . ?
Al5 N52 1.977(6) . ?
Al5 N51 1.981(6) . ?
N51 C53 1.465(9) . ?
N51 C51 1.486(9) . ?
N51 C52 1.493(10) . ?
N52 C54 1.477(9) . ?
N52 C56 1.488(9) . ?
N52 C55 1.496(9) . ?
