#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/81/1508107.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_1508107
loop_
_publ_author_name
'Bonyhady, Simon J.'
'Collis, David'
'Frenking, Gernot'
'Holzmann, Nicole'
'Jones, Cameron'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis of a stable adduct of dialane(4) (Al2H4) via hydrogenation of a
 magnesium(I) dimer.
;
_journal_issue                   10
_journal_name_full               'Nature chemistry'
_journal_page_first              865
_journal_page_last               869
_journal_paper_doi               10.1038/nchem.762
_journal_volume                  2
_journal_year                    2010
_chemical_formula_sum            'C86 H120 Al2 I2 N6'
_chemical_formula_weight         1545.64
_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                111.76(3)
_cell_angle_beta                 93.91(3)
_cell_angle_gamma                114.89(3)
_cell_formula_units_Z            1
_cell_length_a                   11.992(2)
_cell_length_b                   13.192(3)
_cell_length_c                   15.969(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2051.6(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18459
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0410P)²+2.5176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                8170
_reflns_number_total             9810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.762-s12.cif
_cod_data_source_block           compound17a
_cod_original_cell_volume        2051.5(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1508107
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
I1 I 0.571447(18) 0.746938(16) 0.697741(13) 0.03078(7) Uani 1 1 d .
Al1 Al 0.51201(6) 0.52020(6) 0.58746(5) 0.01550(14) Uani 1 1 d .
N1 N 0.39688(17) 0.39007(17) 0.61394(13) 0.0154(4) Uani 1 1 d .
C1 C 0.4948(2) 0.3764(2) 0.64921(15) 0.0150(4) Uani 1 1 d .
N2 N 0.60510(17) 0.47004(17) 0.65180(13) 0.0154(4) Uani 1 1 d .
C2 C 0.2707(2) 0.3450(2) 0.62678(16) 0.0149(4) Uani 1 1 d .
N3 N 0.47866(18) 0.28258(18) 0.67223(14) 0.0192(4) Uani 1 1 d .
C3 C 0.2515(2) 0.3912(2) 0.71658(17) 0.0205(5) Uani 1 1 d .
C4 C 0.1259(2) 0.3515(2) 0.72407(19) 0.0254(5) Uani 1 1 d .
H4 H 0.1117 0.3815 0.7841 0.030 Uiso 1 1 calc R
C5 C 0.0227(2) 0.2704(2) 0.6472(2) 0.0274(6) Uani 1 1 d .
H5 H -0.0614 0.2451 0.6542 0.033 Uiso 1 1 calc R
C6 C 0.0423(2) 0.2261(2) 0.55991(19) 0.0229(5) Uani 1 1 d .
H6 H -0.0291 0.1705 0.5068 0.028 Uiso 1 1 calc R
C7 C 0.1655(2) 0.2614(2) 0.54797(16) 0.0173(4) Uani 1 1 d .
C8 C 0.3582(3) 0.4857(3) 0.80486(18) 0.0299(6) Uani 1 1 d .
H8 H 0.4413 0.4975 0.7902 0.036 Uiso 1 1 calc R
C9 C 0.3583(3) 0.6112(3) 0.8397(2) 0.0464(8) Uani 1 1 d .
H9A H 0.3667 0.6390 0.7904 0.070 Uiso 1 1 calc R
H9B H 0.4302 0.6732 0.8952 0.070 Uiso 1 1 calc R
H9C H 0.2782 0.6014 0.8559 0.070 Uiso 1 1 calc R
C10 C 0.3456(3) 0.4437(4) 0.8826(2) 0.0514(9) Uani 1 1 d .
H10A H 0.2711 0.4440 0.9042 0.077 Uiso 1 1 calc R
H10B H 0.4226 0.5008 0.9350 0.077 Uiso 1 1 calc R
H10C H 0.3351 0.3593 0.8586 0.077 Uiso 1 1 calc R
C11 C 0.1790(2) 0.2040(2) 0.45007(17) 0.0226(5) Uani 1 1 d .
H11 H 0.2716 0.2318 0.4544 0.027 Uiso 1 1 calc R
C12 C 0.1306(3) 0.2462(3) 0.3856(2) 0.0406(7) Uani 1 1 d .
H12A H 0.0438 0.2311 0.3878 0.061 Uiso 1 1 calc R
H12B H 0.1303 0.1993 0.3214 0.061 Uiso 1 1 calc R
H12C H 0.1866 0.3354 0.4061 0.061 Uiso 1 1 calc R
C13 C 0.1074(3) 0.0608(2) 0.4065(2) 0.0336(6) Uani 1 1 d .
H13A H 0.1300 0.0332 0.4511 0.050 Uiso 1 1 calc R
H13B H 0.1312 0.0270 0.3491 0.050 Uiso 1 1 calc R
H13C H 0.0152 0.0310 0.3917 0.050 Uiso 1 1 calc R
C14 C 0.7338(2) 0.4921(2) 0.67352(17) 0.0173(4) Uani 1 1 d .
C15 C 0.8138(2) 0.5801(2) 0.76432(17) 0.0211(5) Uani 1 1 d .
C16 C 0.9396(2) 0.6041(3) 0.7852(2) 0.0287(6) Uani 1 1 d .
H16 H 0.9936 0.6619 0.8465 0.034 Uiso 1 1 calc R
C17 C 0.9873(2) 0.5453(3) 0.7183(2) 0.0309(6) Uani 1 1 d .
H17 H 1.0728 0.5612 0.7340 0.037 Uiso 1 1 calc R
C18 C 0.9101(2) 0.4635(2) 0.6288(2) 0.0258(5) Uani 1 1 d .
H18 H 0.9441 0.4249 0.5829 0.031 Uiso 1 1 calc R
C19 C 0.7833(2) 0.4358(2) 0.60369(17) 0.0195(5) Uani 1 1 d .
C20 C 0.7695(2) 0.6512(2) 0.84136(17) 0.0248(5) Uani 1 1 d .
H20 H 0.6779 0.6241 0.8159 0.030 Uiso 1 1 calc R
C21 C 0.7814(4) 0.6267(3) 0.9272(2) 0.0434(8) Uani 1 1 d .
H21A H 0.7337 0.5370 0.9083 0.065 Uiso 1 1 calc R
H21B H 0.7466 0.6696 0.9729 0.065 Uiso 1 1 calc R
H21C H 0.8714 0.6579 0.9555 0.065 Uiso 1 1 calc R
C22 C 0.8477(3) 0.7921(3) 0.8732(2) 0.0353(6) Uani 1 1 d .
H22A H 0.9368 0.8210 0.9020 0.053 Uiso 1 1 calc R
H22B H 0.8132 0.8355 0.9188 0.053 Uiso 1 1 calc R
H22C H 0.8428 0.8097 0.8189 0.053 Uiso 1 1 calc R
C23 C 0.7090(2) 0.3538(2) 0.50152(17) 0.0215(5) Uani 1 1 d .
H23 H 0.6196 0.3397 0.4960 0.026 Uiso 1 1 calc R
C24 C 0.7039(3) 0.2264(3) 0.4620(2) 0.0348(6) Uani 1 1 d .
H24A H 0.7900 0.2376 0.4617 0.052 Uiso 1 1 calc R
H24B H 0.6485 0.1755 0.3979 0.052 Uiso 1 1 calc R
H24C H 0.6698 0.1845 0.5010 0.052 Uiso 1 1 calc R
C25 C 0.7669(3) 0.4205(3) 0.4425(2) 0.0356(7) Uani 1 1 d .
H25A H 0.7618 0.4979 0.4632 0.053 Uiso 1 1 calc R
H25B H 0.7197 0.3666 0.3766 0.053 Uiso 1 1 calc R
H25C H 0.8564 0.4398 0.4500 0.053 Uiso 1 1 calc R
C26 C 0.3641(2) 0.1588(2) 0.61286(19) 0.0230(5) Uani 1 1 d .
H26 H 0.2978 0.1773 0.5911 0.028 Uiso 1 1 calc R
C27 C 0.3900(3) 0.0850(3) 0.5243(2) 0.0328(6) Uani 1 1 d .
H27A H 0.4243 0.1366 0.4917 0.049 Uiso 1 1 calc R
H27B H 0.3104 0.0100 0.4832 0.049 Uiso 1 1 calc R
H27C H 0.4521 0.0611 0.5414 0.049 Uiso 1 1 calc R
C28 C 0.3051(3) 0.0820(3) 0.6650(2) 0.0360(7) Uani 1 1 d .
H28A H 0.3646 0.0573 0.6851 0.054 Uiso 1 1 calc R
H28B H 0.2254 0.0074 0.6234 0.054 Uiso 1 1 calc R
H28C H 0.2875 0.1319 0.7198 0.054 Uiso 1 1 calc R
C29 C 0.5832(2) 0.2967(2) 0.73863(19) 0.0239(5) Uani 1 1 d .
H29 H 0.6555 0.3821 0.7577 0.029 Uiso 1 1 calc R
C30 C 0.5495(3) 0.2945(3) 0.8288(2) 0.0386(7) Uani 1 1 d .
H30A H 0.5162 0.3526 0.8544 0.058 Uiso 1 1 calc R
H30B H 0.6260 0.3194 0.8745 0.058 Uiso 1 1 calc R
H30C H 0.4846 0.2102 0.8153 0.058 Uiso 1 1 calc R
C31 C 0.6359(3) 0.2073(3) 0.6976(2) 0.0398(7) Uani 1 1 d .
H31A H 0.5706 0.1221 0.6816 0.060 Uiso 1 1 calc R
H31B H 0.7112 0.2305 0.7437 0.060 Uiso 1 1 calc R
H31C H 0.6598 0.2118 0.6411 0.060 Uiso 1 1 calc R
C32 C 0.2167(3) 0.0283(4) 0.8795(3) 0.0520(9) Uani 1 1 d .
H32 H 0.1544 0.0552 0.8861 0.062 Uiso 1 1 calc R
C33 C 0.1856(4) -0.0889(4) 0.8126(3) 0.0660(13) Uani 1 1 d .
H33 H 0.1014 -0.1434 0.7729 0.079 Uiso 1 1 calc R
C34 C 0.2770(5) -0.1268(4) 0.8035(3) 0.0672(13) Uani 1 1 d .
H34 H 0.2558 -0.2073 0.7572 0.081 Uiso 1 1 calc R
C35 C 0.3970(4) -0.0495(4) 0.8605(3) 0.0550(10) Uani 1 1 d .
H35 H 0.4600 -0.0756 0.8543 0.066 Uiso 1 1 calc R
C36 C 0.4268(3) 0.0656(3) 0.9266(3) 0.0466(8) Uani 1 1 d .
H36 H 0.5109 0.1193 0.9667 0.056 Uiso 1 1 calc R
C37 C 0.3385(3) 0.1053(3) 0.9363(2) 0.0424(7) Uani 1 1 d .
H37 H 0.3613 0.1863 0.9824 0.051 Uiso 1 1 calc R
C38 C 1.0783(3) 0.7987(3) 1.1491(2) 0.0408(7) Uani 1 1 d .
H38 H 1.0355 0.8051 1.1972 0.049 Uiso 1 1 calc R
C39 C 1.0844(3) 0.6918(3) 1.1014(2) 0.0388(7) Uani 1 1 d .
H39 H 1.0462 0.6240 1.1168 0.047 Uiso 1 1 calc R
C40 C 1.1457(3) 0.6818(3) 1.0309(2) 0.0418(7) Uani 1 1 d .
H40 H 1.1495 0.6074 0.9977 0.050 Uiso 1 1 calc R
C41 C 1.2014(3) 0.7809(4) 1.0089(2) 0.0439(8) Uani 1 1 d .
H41 H 1.2436 0.7746 0.9604 0.053 Uiso 1 1 calc R
C42 C 1.1958(3) 0.8880(4) 1.0569(3) 0.0494(9) Uani 1 1 d .
H42 H 1.2340 0.9559 1.0417 0.059 Uiso 1 1 calc R
C43 C 1.1349(3) 0.8975(3) 1.1270(2) 0.0452(8) Uani 1 1 d .
H43 H 1.1317 0.9722 1.1605 0.054 Uiso 1 1 calc R
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'
I I -0.4742 1.8119 '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_3
N1 Al1 N2 69.77(8) .
N1 Al1 I1 118.04(7) .
N2 Al1 I1 107.20(7) .
N1 Al1 Al1 117.87(8) 2_666
N2 Al1 Al1 125.45(8) 2_666
I1 Al1 Al1 112.45(5) 2_666
C1 N1 C2 127.28(19) .
C1 N1 Al1 91.65(14) .
C2 N1 Al1 138.15(15) .
N3 C1 N2 128.8(2) .
N3 C1 N1 124.5(2) .
N2 C1 N1 106.59(18) .
C1 N2 C14 129.82(19) .
C1 N2 Al1 91.44(13) .
C14 N2 Al1 136.91(15) .
C7 C2 C3 120.1(2) .
C7 C2 N1 119.2(2) .
C3 C2 N1 120.6(2) .
C1 N3 C29 120.59(19) .
C1 N3 C26 116.20(19) .
C29 N3 C26 121.94(19) .
C4 C3 C2 118.2(2) .
C4 C3 C8 117.8(2) .
C2 C3 C8 124.0(2) .
C5 C4 C3 122.0(2) .
C4 C5 C6 119.5(2) .
C5 C6 C7 121.3(2) .
C6 C7 C2 119.0(2) .
C6 C7 C11 118.1(2) .
C2 C7 C11 122.9(2) .
C3 C8 C10 112.0(3) .
C3 C8 C9 109.8(2) .
C10 C8 C9 108.9(3) .
C7 C11 C12 111.7(2) .
C7 C11 C13 111.6(2) .
C12 C11 C13 109.0(2) .
C19 C14 C15 120.3(2) .
C19 C14 N2 120.9(2) .
C15 C14 N2 118.5(2) .
C16 C15 C14 118.8(2) .
C16 C15 C20 117.9(2) .
C14 C15 C20 123.3(2) .
C17 C16 C15 121.1(3) .
C18 C17 C16 119.6(2) .
C17 C18 C19 121.9(3) .
C18 C19 C14 118.1(2) .
C18 C19 C23 118.1(2) .
C14 C19 C23 123.6(2) .
C15 C20 C21 112.4(2) .
C15 C20 C22 110.8(2) .
C21 C20 C22 108.1(2) .
C19 C23 C25 109.8(2) .
C19 C23 C24 113.5(2) .
C25 C23 C24 109.2(2) .
N3 C26 C28 114.5(2) .
N3 C26 C27 111.6(2) .
C28 C26 C27 112.3(2) .
N3 C29 C31 115.3(2) .
N3 C29 C30 112.8(2) .
C31 C29 C30 110.4(2) .
C37 C32 C33 119.2(4) .
C34 C33 C32 119.9(4) .
C35 C34 C33 120.1(4) .
C34 C35 C36 119.7(4) .
C37 C36 C35 121.2(4) .
C36 C37 C32 119.9(3) .
C39 C38 C43 119.7(3) .
C38 C39 C40 120.3(3) .
C39 C40 C41 119.6(3) .
C42 C41 C40 120.0(3) .
C41 C42 C43 120.1(3) .
C42 C43 C38 120.2(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Al1 2.5854(14) .
Al1 N1 1.912(2) .
Al1 N2 1.926(2) .
Al1 Al1 2.6128(15) 2_666
N1 C1 1.375(3) .
N1 C2 1.435(3) .
C1 N3 1.360(3) .
C1 N2 1.362(3) .
N2 C14 1.436(3) .
C2 C7 1.405(3) .
C2 C3 1.413(3) .
N3 C29 1.486(3) .
N3 C26 1.496(3) .
C3 C4 1.401(3) .
C3 C8 1.513(4) .
C4 C5 1.374(4) .
C5 C6 1.376(4) .
C6 C7 1.400(3) .
C7 C11 1.518(3) .
C8 C10 1.530(4) .
C8 C9 1.537(4) .
C11 C12 1.524(4) .
C11 C13 1.539(4) .
C14 C19 1.412(3) .
C14 C15 1.413(3) .
C15 C16 1.392(3) .
C15 C20 1.525(4) .
C16 C17 1.383(4) .
C17 C18 1.378(4) .
C18 C19 1.395(3) .
C19 C23 1.519(4) .
C20 C21 1.531(4) .
C20 C22 1.537(4) .
C23 C25 1.527(4) .
C23 C24 1.532(4) .
C26 C28 1.524(4) .
C26 C27 1.529(4) .
C29 C31 1.527(4) .
C29 C30 1.529(4) .
C32 C37 1.370(5) .
C32 C33 1.381(6) .
C33 C34 1.379(7) .
C34 C35 1.356(6) .
C35 C36 1.361(5) .
C36 C37 1.359(5) .
C38 C39 1.368(5) .
C38 C43 1.382(5) .
C39 C40 1.382(5) .
C40 C41 1.384(5) .
C41 C42 1.368(5) .
C42 C43 1.374(5) .
