#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:24:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179968 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/62/7026207.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_7026207
loop_
_publ_author_name
'Wasslen, Yamile A.'
'Kurek, Agnieszka'
'Johnson, Paul A.'
'Pigeon, Taylor C.'
'Monillas, Wesley H.'
'Yap, Glenn P. A.'
'Barry, Seán T'
_publ_section_title
;
 Heteroleptic iminopyrrolidinates of aluminium.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9046
_journal_page_last               9054
_journal_paper_doi               10.1039/c0dt00267d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C24 H50 Al2 N4'
_chemical_formula_weight         448.64
_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                 101.582(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1090(14)
_cell_length_b                   19.526(4)
_cell_length_c                   8.7766(16)
_cell_measurement_reflns_used    960
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.59
_cell_volume                     1361.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       ω
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16418
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0496
_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)+(0.0621P)²+0.4659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                2780
_reflns_number_total             3371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00267d.txt
_cod_data_source_block           seab040
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               7026207
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
Al Al 0.04038(6) 0.06371(2) 0.14686(6) 0.02582(14) Uani 1 1 d .
N1 N 0.01243(16) 0.10244(6) -0.06101(15) 0.0256(3) Uani 1 1 d .
N2 N -0.17689(16) 0.01790(7) -0.17234(16) 0.0282(3) Uani 1 1 d .
C1 C 0.1576(2) 0.12804(9) 0.3092(2) 0.0374(4) Uani 1 1 d .
H1A H 0.2771 0.1321 0.3007 0.045 Uiso 1 1 calc R
H1B H 0.1055 0.1740 0.2911 0.045 Uiso 1 1 calc R
C2 C 0.1483(3) 0.10389(14) 0.4738(2) 0.0546(6) Uani 1 1 d .
H2A H 0.2034 0.1376 0.5499 0.082 Uiso 1 1 calc R
H2B H 0.2055 0.0596 0.4943 0.082 Uiso 1 1 calc R
H2C H 0.0302 0.0990 0.4821 0.082 Uiso 1 1 calc R
C3 C -0.1860(2) 0.04276(9) 0.1875(2) 0.0333(4) Uani 1 1 d .
H3A H -0.2420 0.0090 0.1100 0.040 Uiso 1 1 calc R
H3B H -0.1738 0.0218 0.2919 0.040 Uiso 1 1 calc R
C4 C -0.2958(3) 0.10623(11) 0.1796(3) 0.0534(6) Uani 1 1 d .
H4A H -0.4011 0.0945 0.2121 0.080 Uiso 1 1 calc R
H4B H -0.3209 0.1236 0.0727 0.080 Uiso 1 1 calc R
H4C H -0.2361 0.1415 0.2490 0.080 Uiso 1 1 calc R
C5 C -0.3523(2) 0.01730(10) -0.2636(2) 0.0387(4) Uani 1 1 d .
H5A H -0.4343 0.0225 -0.1946 0.046 Uiso 1 1 calc R
H5B H -0.3764 -0.0259 -0.3231 0.046 Uiso 1 1 calc R
C6 C -0.3596(3) 0.07847(11) -0.3726(3) 0.0489(5) Uani 1 1 d .
H6A H -0.3272 0.0651 -0.4714 0.059 Uiso 1 1 calc R
H6B H -0.4738 0.0987 -0.3959 0.059 Uiso 1 1 calc R
C7 C -0.2333(2) 0.12790(9) -0.2816(2) 0.0372(4) Uani 1 1 d .
H7A H -0.2899 0.1627 -0.2282 0.045 Uiso 1 1 calc R
H7B H -0.1682 0.1513 -0.3504 0.045 Uiso 1 1 calc R
C8 C -0.12041(19) 0.08205(8) -0.16495(18) 0.0265(3) Uani 1 1 d .
C9 C 0.0257(2) 0.23105(9) -0.0333(2) 0.0415(4) Uani 1 1 d .
H9A H -0.0974 0.2311 -0.0627 0.062 Uiso 1 1 calc R
H9B H 0.0702 0.2720 -0.0754 0.062 Uiso 1 1 calc R
H9C H 0.0600 0.2310 0.0803 0.062 Uiso 1 1 calc R
C10 C 0.0952(2) 0.16685(8) -0.0993(2) 0.0325(4) Uani 1 1 d .
H10A H 0.0692 0.1715 -0.2152 0.039 Uiso 1 1 calc R
C11 C 0.2845(2) 0.15909(10) -0.0505(3) 0.0420(4) Uani 1 1 d .
H11A H 0.3188 0.1156 -0.0931 0.050 Uiso 1 1 calc R
H11B H 0.3149 0.1562 0.0643 0.050 Uiso 1 1 calc R
C12 C 0.3818(3) 0.21776(10) -0.1050(3) 0.0476(5) Uani 1 1 d .
H12A H 0.5028 0.2085 -0.0754 0.071 Uiso 1 1 calc R
H12B H 0.3557 0.2605 -0.0563 0.071 Uiso 1 1 calc R
H12C H 0.3496 0.2220 -0.2183 0.071 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'
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
N2 Al N1 112.72(6) 3 .
N2 Al C3 109.85(7) 3 .
N1 Al C3 108.14(7) . .
N2 Al C1 104.95(7) 3 .
N1 Al C1 112.01(7) . .
C3 Al C1 109.12(8) . .
C8 N1 C10 115.95(13) . .
C8 N1 Al 117.01(10) . .
C10 N1 Al 124.38(11) . .
C8 N2 C5 108.45(13) . .
C8 N2 Al 126.05(11) . 3
C5 N2 Al 121.42(11) . 3
C2 C1 Al 111.89(14) . .
C4 C3 Al 112.26(12) . .
N2 C5 C6 104.16(14) . .
C7 C6 C5 103.39(15) . .
C6 C7 C8 103.43(14) . .
N1 C8 N2 122.73(14) . .
N1 C8 C7 125.66(14) . .
N2 C8 C7 111.50(14) . .
N1 C10 C11 109.11(13) . .
N1 C10 C9 112.74(14) . .
C11 C10 C9 113.74(16) . .
C10 C11 C12 113.29(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al N2 1.9276(14) 3
Al N1 1.9457(14) .
Al C3 1.9816(17) .
Al C1 1.9920(18) .
N1 C8 1.325(2) .
N1 C10 1.4953(19) .
N2 C8 1.331(2) .
N2 C5 1.486(2) .
N2 Al 1.9277(14) 3
C1 C2 1.535(3) .
C3 C4 1.519(2) .
C5 C6 1.524(3) .
C6 C7 1.513(3) .
C7 C8 1.520(2) .
C9 C10 1.535(2) .
C10 C11 1.516(2) .
C11 C12 1.521(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N2 Al N1 C8 91.70(12) 3
C3 Al N1 C8 -29.93(13) .
C1 Al N1 C8 -150.20(12) .
N2 Al N1 C10 -107.58(12) 3
C3 Al N1 C10 130.79(12) .
C1 Al N1 C10 10.52(14) .
N2 Al C1 C2 -68.81(15) 3
N1 Al C1 C2 168.56(13) .
C3 Al C1 C2 48.86(16) .
N2 Al C3 C4 176.22(14) 3
N1 Al C3 C4 -60.40(16) .
C1 Al C3 C4 61.67(16) .
C8 N2 C5 C6 27.63(19) .
Al N2 C5 C6 -130.94(14) 3
N2 C5 C6 C7 -29.70(19) .
C5 C6 C7 C8 21.54(19) .
C10 N1 C8 N2 159.76(14) .
Al N1 C8 N2 -37.89(19) .
C10 N1 C8 C7 -24.5(2) .
Al N1 C8 C7 137.83(14) .
C5 N2 C8 N1 162.28(15) .
Al N2 C8 N1 -40.4(2) 3
C5 N2 C8 C7 -13.98(18) .
Al N2 C8 C7 143.33(12) 3
C6 C7 C8 N1 178.46(16) .
C6 C7 C8 N2 -5.41(19) .
C8 N1 C10 C11 -140.77(15) .
Al N1 C10 C11 58.33(18) .
C8 N1 C10 C9 91.86(18) .
Al N1 C10 C9 -69.05(18) .
N1 C10 C11 C12 171.80(16) .
C9 C10 C11 C12 -61.4(2) .
