#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:54:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179942 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/37/7023790.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_7023790
loop_
_publ_author_name
'Nako, Adi E.'
'Gates, Sarah J.'
'White, Andrew J. P.'
'Crimmin, Mark R.'
_publ_section_title
;
 Preparation and properties of a series of structurally diverse aluminium
 hydrides supported by β-diketiminate and bis(amide) ligands.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15199
_journal_page_last               15206
_journal_paper_doi               10.1039/c3dt52148f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C27 H31 Al N2'
_chemical_formula_sum            'C27 H31 Al N2'
_chemical_formula_weight         410.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   14.3480(3)
_cell_length_b                   18.1039(4)
_cell_length_c                   9.2139(2)
_cell_measurement_reflns_used    6709
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.6037
_cell_measurement_theta_min      3.0482
_cell_volume                     2393.35(9)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            26614
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         32.68
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablets
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         4247
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0525
_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)+(0.0848P)²+0.4672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                3172
_reflns_number_total             4247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52148f.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7023790
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Al Al 0.60492(3) 0.2500 0.63878(5) 0.02969(14) Uani 1 2 d S . .
H H 0.5435(13) 0.2500 0.775(2) 0.030(5) Uiso 1 2 d S . .
C1 C 0.78568(8) 0.18096(7) 0.65116(12) 0.0328(2) Uani 1 1 d D A .
N1 N 0.69315(7) 0.17191(5) 0.65245(11) 0.0329(2) Uani 1 1 d D . .
C2 C 0.82802(11) 0.2500 0.64252(17) 0.0328(3) Uani 1 2 d S . .
H2A H 0.8937 0.2500 0.6291 0.039 Uiso 1 2 calc SR A .
C3 C 0.84878(10) 0.11496(8) 0.66455(18) 0.0510(4) Uani 1 1 d . . .
H3A H 0.8415 0.0929 0.7611 0.076 Uiso 1 1 calc R A .
H3B H 0.9136 0.1305 0.6510 0.076 Uiso 1 1 calc R . .
H3C H 0.8323 0.0785 0.5903 0.076 Uiso 1 1 calc R . .
C4 C 0.65553(10) 0.09797(6) 0.6701(2) 0.0363(4) Uani 0.784(6) 1 d PGDU A 1
C5 C 0.64101(10) 0.05194(7) 0.5514(2) 0.0432(5) Uani 0.784(6) 1 d PGDU A 1
C6 C 0.60268(11) -0.01783(6) 0.5714(3) 0.0604(8) Uani 0.784(6) 1 d PGDU A 1
H6A H 0.5928 -0.0493 0.4904 0.073 Uiso 0.784(6) 1 calc PR A 1
C7 C 0.57886(11) -0.04158(8) 0.7100(4) 0.0670(10) Uani 0.784(6) 1 d PGU A 1
H7A H 0.5527 -0.0893 0.7237 0.080 Uiso 0.784(6) 1 calc PR A 1
C8 C 0.59338(11) 0.00444(11) 0.8286(3) 0.0637(9) Uani 0.784(6) 1 d PGDU A 1
H8A H 0.5771 -0.0118 0.9233 0.076 Uiso 0.784(6) 1 calc PR A 1
C9 C 0.63172(11) 0.07422(10) 0.8086(2) 0.0475(5) Uani 0.784(6) 1 d PGDU A 1
C10 C 0.66697(18) 0.07610(13) 0.3981(3) 0.0492(5) Uani 0.784(6) 1 d PDU A 1
H10A H 0.6323 0.1210 0.3729 0.074 Uiso 0.784(6) 1 calc PR A 1
H10B H 0.6512 0.0367 0.3294 0.074 Uiso 0.784(6) 1 calc PR A 1
H10C H 0.7340 0.0862 0.3934 0.074 Uiso 0.784(6) 1 calc PR A 1
C11 C 0.6530(2) 0.1206(2) 0.9412(3) 0.0631(8) Uani 0.784(6) 1 d PDU A 1
H11A H 0.6327 0.0943 1.0286 0.095 Uiso 0.784(6) 1 calc PR A 1
H11B H 0.6199 0.1678 0.9342 0.095 Uiso 0.784(6) 1 calc PR A 1
H11C H 0.7202 0.1297 0.9466 0.095 Uiso 0.784(6) 1 calc PR A 1
C4' C 0.6591(5) 0.1024(3) 0.7054(6) 0.046(2) Uiso 0.216(6) 1 d PGDU A 2
C5' C 0.6349(6) 0.0505(4) 0.6009(6) 0.066(3) Uiso 0.216(6) 1 d PGDU A 2
C6' C 0.5916(5) -0.0150(3) 0.6419(8) 0.0505(19) Uiso 0.216(6) 1 d PGDU A 2
H6'A H 0.5751 -0.0505 0.5704 0.061 Uiso 0.216(6) 1 calc PR A 2
C7' C 0.5726(5) -0.0286(3) 0.7874(9) 0.059(2) Uiso 0.216(6) 1 d PGU A 2
H7'A H 0.5431 -0.0733 0.8154 0.070 Uiso 0.216(6) 1 calc PR A 2
C8' C 0.5969(4) 0.0233(3) 0.8919(7) 0.056(2) Uiso 0.216(6) 1 d PGDU A 2
H8'A H 0.5839 0.0141 0.9914 0.067 Uiso 0.216(6) 1 calc PR A 2
C9' C 0.6401(4) 0.0888(3) 0.8510(6) 0.0289(13) Uiso 0.216(6) 1 d PGDU A 2
C10' C 0.6546(7) 0.0654(6) 0.4440(10) 0.052(3) Uiso 0.216(6) 1 d PDU A 2
H10D H 0.7002 0.0295 0.4080 0.077 Uiso 0.216(6) 1 calc PR A 2
H10E H 0.6797 0.1154 0.4334 0.077 Uiso 0.216(6) 1 calc PR A 2
H10F H 0.5968 0.0610 0.3881 0.077 Uiso 0.216(6) 1 calc PR A 2
C11' C 0.6731(7) 0.1434(5) 0.9630(10) 0.049(2) Uiso 0.216(6) 1 d PDU A 2
H11D H 0.6283 0.1452 1.0432 0.074 Uiso 0.216(6) 1 calc PR A 2
H11E H 0.6784 0.1924 0.9187 0.074 Uiso 0.216(6) 1 calc PR A 2
H11F H 0.7341 0.1280 1.0001 0.074 Uiso 0.216(6) 1 calc PR A 2
C12 C 0.52611(11) 0.2500 0.46195(18) 0.0328(3) Uani 1 2 d S . .
C13 C 0.55446(15) 0.2500 0.3159(2) 0.0436(4) Uani 1 2 d S A .
H13A H 0.6192 0.2500 0.2946 0.052 Uiso 1 2 calc SR . .
C14 C 0.49136(18) 0.2500 0.2016(2) 0.0506(5) Uani 1 2 d S . .
H14A H 0.5135 0.2500 0.1044 0.061 Uiso 1 2 calc SR A .
C15 C 0.39748(17) 0.2500 0.2282(2) 0.0533(5) Uani 1 2 d S A .
H15A H 0.3546 0.2500 0.1497 0.064 Uiso 1 2 calc SR . .
C16 C 0.36549(16) 0.2500 0.3689(2) 0.0521(5) Uani 1 2 d S . .
H16A H 0.3004 0.2500 0.3882 0.063 Uiso 1 2 calc SR A .
C17 C 0.42948(12) 0.2500 0.48360(19) 0.0406(4) Uani 1 2 d S A .
H17A H 0.4064 0.2500 0.5802 0.049 Uiso 1 2 calc SR . .
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
N1 Al N1 96.03(6) 7_565
N1 Al C12 115.72(4) 7_565
N1 Al C12 115.72(4) .
N1 C1 C2 122.93(11) .
N1 C1 C3 119.95(11) .
C2 C1 C3 117.08(11) .
C1 N1 C4' 116.6(3) .
C1 N1 C4 118.86(11) .
C1 N1 Al 124.68(8) .
C4' N1 Al 116.6(3) .
C4 N1 Al 116.43(8) .
C1 C2 C1 127.77(14) 7_565
C5 C4 C9 120.0 .
C5 C4 N1 121.36(10) .
C9 C4 N1 118.62(10) .
C6 C5 C4 120.0 .
C6 C5 C10 118.67(11) .
C4 C5 C10 121.33(11) .
C7 C6 C5 120.0 .
C8 C7 C6 120.0 .
C7 C8 C9 120.0 .
C8 C9 C4 120.0 .
C8 C9 C11 118.51(13) .
C4 C9 C11 121.34(13) .
C5' C4' C9' 120.0 .
C5' C4' N1 116.2(3) .
C9' C4' N1 123.3(3) .
C4' C5' C6' 120.0 .
C4' C5' C10' 120.0(5) .
C6' C5' C10' 120.0(5) .
C7' C6' C5' 120.0 .
C8' C7' C6' 120.0 .
C7' C8' C9' 120.0 .
C8' C9' C4' 120.0 .
C8' C9' C11' 120.9(4) .
C4' C9' C11' 118.9(4) .
C17 C12 C13 115.01(16) .
C17 C12 Al 116.58(12) .
C13 C12 Al 128.42(13) .
C14 C13 C12 122.49(18) .
C15 C14 C13 120.39(18) .
C14 C15 C16 119.79(19) .
C15 C16 C17 119.5(2) .
C16 C17 C12 122.80(17) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al N1 1.9018(10) 7_565
Al N1 1.9018(10) .
Al C12 1.9833(17) .
C1 N1 1.3377(14) .
C1 C2 1.3919(14) .
C1 C3 1.5043(17) .
N1 C4' 1.436(4) .
N1 C4 1.4525(13) .
C2 C1 1.3919(14) 7_565
C4 C5 1.3900 .
C4 C9 1.3900 .
C5 C6 1.3900 .
C5 C10 1.525(3) .
C6 C7 1.3900 .
C7 C8 1.3900 .
C8 C9 1.3900 .
C9 C11 1.513(3) .
C4' C5' 1.3900 .
C4' C9' 1.3900 .
C5' C6' 1.3900 .
C5' C10' 1.497(8) .
C6' C7' 1.3900 .
C7' C8' 1.3900 .
C8' C9' 1.3900 .
C9' C11' 1.505(7) .
C12 C17 1.401(2) .
C12 C13 1.406(2) .
C13 C14 1.389(3) .
C14 C15 1.369(3) .
C15 C16 1.376(3) .
C16 C17 1.400(3) .
