#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:58:00 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178542 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/48/4064837.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_4064837
loop_
_publ_author_name
'Michel, Olaf'
'Yamamoto, Koji'
'Tsurugi, Hayato'
'Maichle-Mössmer, Cäcilia'
'Törnroos, Karl W.'
'Mashima, Kazushi'
'Anwander, Reiner'
_publ_section_title
;
 Reactivity of Permethylated Magnesium Complexes toward β-Diimines
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3818
_journal_paper_doi               10.1021/om200361m
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C22 H34 Al2 N2'
_chemical_formula_weight         380.47
_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                102.16(2)
_cell_angle_beta                 91.06(2)
_cell_angle_gamma                90.75(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8629(18)
_cell_length_b                   7.7586(19)
_cell_length_c                   11.250(3)
_cell_measurement_reflns_used    3633
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.75
_cell_measurement_theta_min      5.38
_cell_volume                     585.4(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Stoe-IPDS II'
_diffrn_measurement_method       omega-scans
_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  0.1161
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5352
_diffrn_reflns_theta_full        23.24
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             206
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         1570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0575
_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)+(0.0281P)²+0.8808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                1350
_reflns_number_total             1570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200361m_si_001.cif
_cod_data_source_block           matrix220
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064837
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
C11 C 0.0884(5) -0.0428(5) 0.0233(3) 0.0262(8) Uani 1 1 d .
C13 C 0.1337(5) 0.0048(5) 0.2338(3) 0.0276(8) Uani 1 1 d .
C14 C 0.1432(7) 0.4932(5) 0.1588(4) 0.0429(10) Uani 1 1 d .
H14A H 0.0343 0.4763 0.0996 0.064 Uiso 1 1 calc R
H14B H 0.2157 0.6014 0.1546 0.064 Uiso 1 1 calc R
H14C H 0.0927 0.5029 0.2408 0.064 Uiso 1 1 calc R
C15 C 0.3863(6) 0.2349(5) -0.0531(3) 0.0406(10) Uani 1 1 d .
H15A H 0.2678 0.2352 -0.1030 0.061 Uiso 1 1 calc R
H15B H 0.4458 0.1186 -0.0735 0.061 Uiso 1 1 calc R
H15C H 0.4786 0.3245 -0.0690 0.061 Uiso 1 1 calc R
C16 C 0.5517(7) 0.2906(6) 0.2267(4) 0.0406(10) Uani 1 1 d .
C131 C 0.1787(5) 0.0912(5) 0.3596(3) 0.0303(9) Uani 1 1 d .
C132 C 0.2298(6) -0.0136(6) 0.4415(4) 0.0371(10) Uani 1 1 d .
C133 C 0.2749(6) 0.0641(7) 0.5614(4) 0.0474(12) Uani 1 1 d .
C134 C 0.2643(7) 0.2423(7) 0.6010(4) 0.0500(12) Uani 1 1 d .
C135 C 0.2062(7) 0.3457(6) 0.5231(4) 0.0506(12) Uani 1 1 d .
C136 C 0.1647(7) 0.2714(6) 0.4024(4) 0.0420(10) Uani 1 1 d .
H11A H 0.054(5) -0.156(5) 0.036(3) 0.020(9) Uiso 1 1 d .
H11B H 0.195(5) -0.056(4) -0.034(3) 0.022(9) Uiso 1 1 d .
H13 H 0.077(5) -0.116(4) 0.224(3) 0.020(8) Uiso 1 1 d .
H13A H 0.220(6) -0.139(5) 0.416(3) 0.037(11) Uiso 1 1 d .
H13B H 0.317(7) -0.003(6) 0.609(4) 0.060(15) Uiso 1 1 d .
H13C H 0.300(7) 0.292(6) 0.681(5) 0.069(15) Uiso 1 1 d .
H13D H 0.189(6) 0.475(6) 0.553(4) 0.049(12) Uiso 1 1 d .
H13E H 0.124(5) 0.344(5) 0.354(3) 0.032(10) Uiso 1 1 d .
H16A H 0.597(8) 0.174(7) 0.228(5) 0.075(16) Uiso 1 1 d .
H16B H 0.534(7) 0.347(6) 0.310(4) 0.057(13) Uiso 1 1 d .
H16C H 0.668(8) 0.352(7) 0.201(4) 0.074(16) Uiso 1 1 d .
Al1 Al 0.31928(16) 0.28864(13) 0.12076(9) 0.0272(4) Uani 1 1 d .
N12 N 0.1592(4) 0.0693(3) 0.1391(2) 0.0235(7) Uani 1 1 d .
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'
Al Al 0.0645 0.0514 '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'
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
N12 C11 C11 109.1(3) . 2
N12 C11 H11A 109.7(19) . .
C11 C11 H11A 110(2) 2 .
N12 C11 H11B 108.2(19) . .
C11 C11 H11B 111.8(19) 2 .
H11A C11 H11B 108(3) . .
N12 C13 C131 126.7(3) . .
N12 C13 H13 119.0(18) . .
C131 C13 H13 114.2(18) . .
Al1 C14 H14A 109.5 . .
Al1 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
Al1 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
Al1 C15 H15A 109.5 . .
Al1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
Al1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
Al1 C16 H16A 113(3) . .
Al1 C16 H16B 115(3) . .
H16A C16 H16B 106(4) . .
Al1 C16 H16C 114(3) . .
H16A C16 H16C 104(4) . .
H16B C16 H16C 104(4) . .
C136 C131 C132 118.6(4) . .
C136 C131 C13 123.0(3) . .
C132 C131 C13 118.3(3) . .
C133 C132 C131 119.9(4) . .
C133 C132 H13A 121(2) . .
C131 C132 H13A 119(2) . .
C134 C133 C132 120.5(4) . .
C134 C133 H13B 121(3) . .
C132 C133 H13B 118(3) . .
C133 C134 C135 120.2(4) . .
C133 C134 H13C 119(3) . .
C135 C134 H13C 121(3) . .
C134 C135 C136 120.3(5) . .
C134 C135 H13D 121(2) . .
C136 C135 H13D 119(2) . .
C135 C136 C131 120.5(4) . .
C135 C136 H13E 118(2) . .
C131 C136 H13E 122(2) . .
C16 Al1 C15 111.7(2) . .
C16 Al1 C14 117.57(19) . .
C15 Al1 C14 111.29(18) . .
C16 Al1 N12 104.99(17) . .
C15 Al1 N12 103.04(14) . .
C14 Al1 N12 106.92(15) . .
C13 N12 C11 115.3(3) . .
C13 N12 Al1 129.4(2) . .
C11 N12 Al1 114.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C11 N12 1.475(4) .
C11 C11 1.527(7) 2
C11 H11A 0.94(3) .
C11 H11B 0.98(4) .
C13 N12 1.283(4) .
C13 C131 1.458(5) .
C13 H13 1.00(3) .
C14 Al1 1.986(4) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 Al1 1.976(4) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 Al1 1.972(4) .
C16 H16A 0.96(5) .
C16 H16B 0.95(5) .
C16 H16C 1.00(6) .
C131 C136 1.385(5) .
C131 C132 1.395(5) .
C132 C133 1.384(6) .
C132 H13A 0.96(4) .
C133 C134 1.364(7) .
C133 H13B 0.87(5) .
C134 C135 1.365(7) .
C134 H13C 0.93(5) .
C135 C136 1.381(6) .
C135 H13D 1.00(4) .
C136 H13E 0.91(4) .
Al1 N12 2.062(3) .
