#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:40:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178719 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/30/4083018.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_4083018
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_sum            'C16 H36 Al2 N4'
_chemical_formula_weight         338.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.725(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1060(4)
_cell_length_b                   12.7670(5)
_cell_length_c                   18.6329(7)
_cell_measurement_reflns_used    21532
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      26.90
_cell_measurement_theta_min      2.25
_cell_volume                     2104.34(15)
_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 Vers. 2008/4'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43558
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.915
_diffrn_reflns_theta_min         1.595
_diffrn_source                   'sealed X-RAY tube'
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.58
_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    1.068
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0581P)²+1.5948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4004
_reflns_number_total             4595
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5002217_si_001.cif
_cod_data_source_block           mb_032m
_cod_depositor_comments
'Adding full bibliography for 4083015--4083021.cif.'
_cod_database_code               4083018
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Al1 Al 0.68281(7) 0.94929(5) 0.37441(3) 0.02203(16) Uani 1 1 d . .
Al2 Al 0.94538(7) 0.95600(5) 0.15749(3) 0.02321(16) Uani 1 1 d . .
N1 N 0.7475(2) 0.81433(14) 0.41847(9) 0.0241(4) Uani 1 1 d . .
N2 N 0.9357(2) 0.80967(13) 0.35318(9) 0.0219(4) Uani 1 1 d . .
N3 N 0.91894(19) 0.84597(13) 0.22740(9) 0.0205(4) Uani 1 1 d . .
N4 N 0.73539(19) 0.91125(13) 0.28597(9) 0.0203(3) Uani 1 1 d . .
C1 C 0.8668(2) 0.77070(16) 0.40692(11) 0.0236(4) Uani 1 1 d . .
C2 C 0.8594(2) 0.85790(15) 0.28551(11) 0.0192(4) Uani 1 1 d . .
C3 C 1.1040(2) 0.81080(18) 0.37070(12) 0.0265(4) Uani 1 1 d . .
H3A H 1.1422 0.8096 0.4251 0.032 Uiso 1 1 d R U
H3B H 1.1373 0.8775 0.3526 0.032 Uiso 1 1 d R U
C4 C 1.1778(3) 0.72087(18) 0.33830(13) 0.0293(5) Uani 1 1 d . .
H4A H 1.2876 0.7196 0.3614 0.035 Uiso 1 1 d R U
H4B H 1.1341 0.6539 0.3501 0.035 Uiso 1 1 d R U
C5 C 1.1539(3) 0.73033(18) 0.25512(13) 0.0291(5) Uani 1 1 d . .
H5A H 1.1937 0.6666 0.2360 0.035 Uiso 1 1 d R U
H5B H 1.2118 0.7912 0.2436 0.035 Uiso 1 1 d R U
C6 C 0.9877(2) 0.74358(16) 0.21687(12) 0.0241(4) Uani 1 1 d . .
H6A H 0.9766 0.7330 0.1632 0.029 Uiso 1 1 d R U
H6B H 0.9293 0.6877 0.2343 0.029 Uiso 1 1 d R U
C7 C 0.4629(3) 0.9574(2) 0.36194(14) 0.0331(5) Uani 1 1 d . .
H7A H 0.4242 1.0212 0.3348 0.050 Uiso 1 1 d R U
H7B H 0.4397 0.9588 0.4107 0.050 Uiso 1 1 d R U
H7C H 0.4150 0.8960 0.3344 0.050 Uiso 1 1 d R U
C8 C 0.8108(3) 1.06009(19) 0.42875(14) 0.0400(6) Uani 1 1 d . .
H8A H 0.9148 1.0494 0.4244 0.060 Uiso 1 1 d R U
H8B H 0.8078 1.0576 0.4810 0.060 Uiso 1 1 d R U
H8C H 0.7745 1.1285 0.4081 0.060 Uiso 1 1 d R U
C9 C 0.6658(3) 0.7679(2) 0.47066(14) 0.0367(6) Uani 1 1 d . .
H9A H 0.6920 0.6928 0.4781 0.044 Uiso 1 1 d R U
H9B H 0.5555 0.7734 0.4497 0.044 Uiso 1 1 d R U
C10 C 0.7067(5) 0.8248(2) 0.54406(16) 0.0602(10) Uani 1 1 d . .
H10A H 0.8124 0.8100 0.5684 0.090 Uiso 1 1 d R U
H10B H 0.6411 0.8005 0.5754 0.090 Uiso 1 1 d R U
H10C H 0.6934 0.9004 0.5359 0.090 Uiso 1 1 d R U
C11 C 0.9379(3) 0.67586(19) 0.44912(13) 0.0346(5) Uani 1 1 d . .
H11A H 0.9393 0.6847 0.5015 0.052 Uiso 1 1 d R U
H11B H 1.0417 0.6677 0.4435 0.052 Uiso 1 1 d R U
H11C H 0.8790 0.6134 0.4299 0.052 Uiso 1 1 d R U
C12 C 0.8044(3) 0.9219(2) 0.06106(12) 0.0343(5) Uani 1 1 d . .
H12A H 0.8227 0.8501 0.0469 0.051 Uiso 1 1 d R U
H12B H 0.8210 0.9706 0.0231 0.051 Uiso 1 1 d R U
H12C H 0.6999 0.9283 0.0659 0.051 Uiso 1 1 d R U
C13 C 0.9219(3) 1.09294(17) 0.20504(13) 0.0315(5) Uani 1 1 d . .
H13A H 0.8145 1.1051 0.2026 0.047 Uiso 1 1 d R U
H13B H 0.9605 1.1492 0.1788 0.047 Uiso 1 1 d R U
H13C H 0.9785 1.0919 0.2568 0.047 Uiso 1 1 d R U
C14 C 1.1561(3) 0.94719(19) 0.14515(13) 0.0323(5) Uani 1 1 d . .
H14A H 1.2272 0.9632 0.1922 0.048 Uiso 1 1 d R U
H14B H 1.1696 0.9977 0.1077 0.048 Uiso 1 1 d R U
H14C H 1.1753 0.8763 0.1294 0.048 Uiso 1 1 d R U
C15 C 0.6266(2) 0.93234(16) 0.21467(11) 0.0231(4) Uani 1 1 d . .
H15A H 0.6810 0.9658 0.1806 0.028 Uiso 1 1 d R U
H15B H 0.5490 0.9822 0.2229 0.028 Uiso 1 1 d R U
C16 C 0.5495(3) 0.83368(18) 0.17915(13) 0.0302(5) Uani 1 1 d . .
H16A H 0.6241 0.7882 0.1645 0.045 Uiso 1 1 d R U
H16B H 0.4707 0.8525 0.1354 0.045 Uiso 1 1 d R U
H16C H 0.5039 0.7966 0.2145 0.045 Uiso 1 1 d R U
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
N4 Al1 N1 91.51(8)
N4 Al1 C8 113.28(11)
N1 Al1 C8 109.86(10)
N4 Al1 C7 111.93(10)
N1 Al1 C7 107.21(10)
C8 Al1 C7 119.27(12)
N3 Al2 C14 107.99(9)
N3 Al2 C12 106.69(9)
C14 Al2 C12 108.43(11)
N3 Al2 C13 106.78(9)
C14 Al2 C13 108.01(11)
C12 Al2 C13 118.53(11)
C1 N1 C9 120.90(19)
C1 N1 Al1 119.94(15)
C9 N1 Al1 118.92(15)
C1 N2 C2 125.49(17)
C1 N2 C3 117.48(17)
C2 N2 C3 116.75(17)
C2 N3 C6 118.39(17)
C2 N3 Al2 126.47(14)
C6 N3 Al2 114.82(13)
C2 N4 C15 118.60(17)
C2 N4 Al1 122.24(14)
C15 N4 Al1 118.86(13)
N1 C1 N2 120.58(18)
N1 C1 C11 122.6(2)
N2 C1 C11 116.83(19)
N4 C2 N3 125.39(18)
N4 C2 N2 117.06(17)
N3 C2 N2 117.55(18)
N2 C3 C4 115.67(18)
C5 C4 C3 111.99(18)
C4 C5 C6 111.87(19)
N3 C6 C5 116.13(17)
N1 C9 C10 110.3(2)
N4 C15 C16 112.49(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Al1 N4 1.8854(18)
Al1 N1 1.9391(18)
Al1 C8 1.956(3)
Al1 C7 1.964(2)
Al2 N3 1.9690(18)
Al2 C14 1.989(2)
Al2 C12 1.993(2)
Al2 C13 1.994(2)
N1 C1 1.283(3)
N1 C9 1.481(3)
N2 C1 1.394(3)
N2 C2 1.427(3)
N2 C3 1.489(3)
N3 C2 1.330(3)
N3 C6 1.482(3)
N4 C2 1.320(3)
N4 C15 1.481(3)
C1 C11 1.504(3)
C3 C4 1.526(3)
C4 C5 1.518(3)
C5 C6 1.522(3)
C9 C10 1.514(4)
C15 C16 1.515(3)
