#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:40:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178719 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/30/4083016.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_4083016
loop_
_publ_author_name
'Bayram, Melike'
'Bläser, Dieter'
'Wölper, Christoph'
'Schulz, Stephan'
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universität Duisburg-Essen
         Campus Essen, Universitätsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 Syntheses and Structures of Bis-Amidinate--Alane Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2080
_journal_paper_doi               10.1021/om5002217
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C26 H62 Al4 N4'
_chemical_formula_sum            'C26 H62 Al4 N4'
_chemical_formula_weight         538.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.365(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5420(4)
_cell_length_b                   14.8430(6)
_cell_length_c                   13.2769(5)
_cell_measurement_reflns_used    16599
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.58
_cell_volume                     1836.81(13)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      180(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34486
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         4543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0387
_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)+(0.0683P)²+0.3993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1166
_reflns_number_gt                3780
_reflns_number_total             4543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5002217_si_001.cif
_cod_data_source_block           mb_015m
_cod_depositor_comments
'Adding full bibliography for 4083015--4083021.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4083016
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Al1 Al 0.22340(4) 0.03259(2) 0.80239(3) 0.02857(12) Uani 1 1 d .
Al2 Al -0.09684(4) 0.14102(3) 0.74042(3) 0.02792(11) Uani 1 1 d .
N1 N 0.29094(11) 0.15688(7) 0.81709(8) 0.0284(2) Uani 1 1 d .
N2 N 0.09764(11) 0.11410(6) 0.70238(7) 0.0235(2) Uani 1 1 d .
C1 C 0.00088(15) 0.01037(9) 0.55648(9) 0.0314(3) Uani 1 1 d .
H1A H -0.0988 0.0163 0.5660 0.038 Uiso 1 1 d R
H1B H 0.0471 -0.0399 0.6003 0.038 Uiso 1 1 d R
C2 C 0.08211(14) 0.09692(8) 0.58922(9) 0.0295(3) Uani 1 1 d .
H2A H 0.1785 0.0931 0.5730 0.035 Uiso 1 1 d R
H2B H 0.0305 0.1480 0.5498 0.035 Uiso 1 1 d R
C3 C 0.19819(13) 0.18391(8) 0.73802(9) 0.0262(2) Uani 1 1 d .
C4 C 0.41264(15) 0.20611(10) 0.88321(13) 0.0425(3) Uani 1 1 d .
C5 C 0.5283(2) 0.22071(16) 0.8217(2) 0.0810(7) Uani 1 1 d .
H5A H 0.5535 0.1628 0.7948 0.121 Uiso 1 1 d R
H5B H 0.6135 0.2470 0.8665 0.121 Uiso 1 1 d R
H5C H 0.4922 0.2617 0.7641 0.121 Uiso 1 1 d R
C6 C 0.4663(3) 0.14357(14) 0.97384(19) 0.0791(7) Uani 1 1 d .
H6A H 0.3885 0.1315 1.0096 0.119 Uiso 1 1 d R
H6B H 0.5466 0.1721 1.0217 0.119 Uiso 1 1 d R
H6C H 0.4986 0.0868 0.9487 0.119 Uiso 1 1 d R
C7 C 0.3662(2) 0.29454(12) 0.92351(15) 0.0595(5) Uani 1 1 d .
H7A H 0.3477 0.3389 0.8676 0.089 Uiso 1 1 d R
H7B H 0.4425 0.3168 0.9796 0.089 Uiso 1 1 d R
H7C H 0.2786 0.2850 0.9494 0.089 Uiso 1 1 d R
C8 C -0.04182(16) 0.21554(12) 0.86665(12) 0.0455(4) Uani 1 1 d .
H8A H -0.1238 0.2209 0.8999 0.068 Uiso 1 1 d R
H8B H -0.0130 0.2756 0.8481 0.068 Uiso 1 1 d R
H8C H 0.0385 0.1870 0.9143 0.068 Uiso 1 1 d R
C9 C -0.21081(18) 0.20720(12) 0.62130(13) 0.0501(4) Uani 1 1 d .
H9A H -0.2296 0.1678 0.5606 0.075 Uiso 1 1 d R
H9B H -0.1573 0.2604 0.6071 0.075 Uiso 1 1 d R
H9C H -0.3021 0.2262 0.6371 0.075 Uiso 1 1 d R
C10 C -0.18490(17) 0.02356(11) 0.76007(12) 0.0433(3) Uani 1 1 d .
H10A H -0.1999 0.0195 0.8307 0.065 Uiso 1 1 d R
H10B H -0.1211 -0.0252 0.7481 0.065 Uiso 1 1 d R
H10C H -0.2773 0.0181 0.7112 0.065 Uiso 1 1 d R
C11 C 0.3471(2) -0.04075(12) 0.73617(15) 0.0553(4) Uani 1 1 d .
H11A H 0.4377 -0.0525 0.7852 0.083 Uiso 1 1 d R
H11B H 0.3666 -0.0086 0.6762 0.083 Uiso 1 1 d R
H11C H 0.2993 -0.0980 0.7138 0.083 Uiso 1 1 d R
C12 C 0.15512(18) -0.01558(12) 0.91947(13) 0.0508(4) Uani 1 1 d .
H12A H 0.1045 -0.0725 0.8997 0.076 Uiso 1 1 d R
H12B H 0.0895 0.0277 0.9408 0.076 Uiso 1 1 d R
H12C H 0.2369 -0.0263 0.9769 0.076 Uiso 1 1 d R
C13 C 0.18663(19) 0.27256(9) 0.68402(12) 0.0440(4) Uani 1 1 d .
H13A H 0.2717 0.3090 0.7121 0.066 Uiso 1 1 d R
H13B H 0.1006 0.3042 0.6943 0.066 Uiso 1 1 d R
H13C H 0.1800 0.2628 0.6101 0.066 Uiso 1 1 d 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_3
C12 Al1 C11 119.61(8) .
C12 Al1 N1 115.32(7) .
C11 Al1 N1 110.76(7) .
C12 Al1 N2 119.85(6) .
C11 Al1 N2 111.99(7) .
N1 Al1 N2 68.40(4) .
C12 Al1 C3 127.16(6) .
C11 Al1 C3 112.76(7) .
N1 Al1 C3 32.33(4) .
N2 Al1 C3 36.36(4) .
C10 Al2 C9 111.53(8) .
C10 Al2 C8 115.06(7) .
C9 Al2 C8 113.55(8) .
C10 Al2 N2 106.94(6) .
C9 Al2 N2 105.65(6) .
C8 Al2 N2 103.04(5) .
C3 N1 C4 130.00(12) .
C3 N1 Al1 93.36(8) .
C4 N1 Al1 136.27(9) .
C3 N2 C2 111.84(9) .
C3 N2 Al1 87.34(7) .
C2 N2 Al1 118.67(8) .
C3 N2 Al2 110.82(7) .
C2 N2 Al2 112.14(8) .
Al1 N2 Al2 113.49(5) .
C2 C1 C1 110.48(13) 3_556
N2 C2 C1 111.49(10) .
N1 C3 N2 110.00(11) .
N1 C3 C13 129.49(12) .
N2 C3 C13 120.51(11) .
N1 C3 Al1 54.31(7) .
N2 C3 Al1 56.30(6) .
C13 C3 Al1 171.79(9) .
N1 C4 C7 112.49(12) .
N1 C4 C6 104.79(12) .
C7 C4 C6 108.86(16) .
N1 C4 C5 108.48(14) .
C7 C4 C5 111.44(16) .
C6 C4 C5 110.59(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 C12 1.9457(16) .
Al1 C11 1.9486(16) .
Al1 N1 1.9501(11) .
Al1 N2 1.9961(10) .
Al1 C3 2.3968(13) .
Al2 C10 1.9768(16) .
Al2 C9 1.9779(15) .
Al2 C8 1.9828(15) .
Al2 N2 2.0639(11) .
N1 C3 1.2839(16) .
N1 C4 1.4888(16) .
N2 C3 1.4225(15) .
N2 C2 1.4996(14) .
C1 C2 1.5152(17) .
C1 C1 1.528(2) 3_556
C3 C13 1.4913(18) .
C4 C7 1.519(2) .
C4 C6 1.519(3) .
C4 C5 1.522(3) .
