#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:55:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179218 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/44/4314438.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_4314438
loop_
_publ_author_name
'Yu-Ling Lien'
'Ya-Chi Chang'
'Nien-Tsu Chuang'
'Amitabha Datta'
'Shau-Jiun Chen'
'Ching-Han Hu'
'Wen-Yen Huang'
'Chia-Her Lin'
'Jui-Hsien Huang'
_publ_section_title
;
 A New Type of Asymmetric Tridentate Pyrrolyl-Linked Pincer Ligand and Its
 Aluminum Dihydride Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              136
_journal_page_last               143
_journal_paper_doi               10.1021/ic9016189
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C12 H24 Al N3'
_chemical_formula_weight         237.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.110(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.9553(16)
_cell_length_b                   6.5478(4)
_cell_length_c                   19.3734(12)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     2836.1(3)
_computing_cell_refinement       'APEX2 v1.0-22'
_computing_data_collection       'APEX2 v1.0-22 (Bruker, 2004)'
_computing_data_reduction        'APEX2 v1.0-22'
_computing_molecular_graphics    'SHELXTL 5.1'
_computing_publication_material  'SHELXTL 5.1'
_computing_structure_refinement  'SHELXTL 5.1'
_computing_structure_solution    'SHELXTL 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18114
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_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  0.9852
_exptl_absorpt_correction_T_min  0.9660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0327
_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)+(0.0505P)²+0.9399P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                2763
_reflns_number_total             3422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9016189_si_001_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314438
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Al1 Al 0.116363(14) 0.62809(6) 0.998298(17) 0.02327(11) Uani 1 1 d . . .
C1 C 0.11275(5) 0.88600(19) 0.85509(6) 0.0261(3) Uani 1 1 d . . .
C2 C 0.08607(6) 0.6887(2) 0.81919(6) 0.0349(3) Uani 1 1 d . . .
H2A H 0.1184 0.5971 0.8135 0.052 Uiso 1 1 calc R . .
H2B H 0.0607 0.7205 0.7726 0.052 Uiso 1 1 calc R . .
H2C H 0.0620 0.6220 0.8485 0.052 Uiso 1 1 calc R . .
C3 C 0.06288(6) 1.0249(2) 0.86789(7) 0.0353(3) Uani 1 1 d . . .
H3A H 0.0414 0.9567 0.8997 0.053 Uiso 1 1 calc R . .
H3B H 0.0350 1.0544 0.8226 0.053 Uiso 1 1 calc R . .
H3C H 0.0802 1.1529 0.8896 0.053 Uiso 1 1 calc R . .
C4 C 0.14844(6) 0.9949(2) 0.80821(7) 0.0365(3) Uani 1 1 d . . .
H4A H 0.1635 1.1252 0.8300 0.055 Uiso 1 1 calc R . .
H4B H 0.1225 1.0201 0.7614 0.055 Uiso 1 1 calc R . .
H4C H 0.1822 0.9089 0.8032 0.055 Uiso 1 1 calc R . .
C5 C 0.19000(5) 0.99087(19) 0.96464(6) 0.0249(2) Uani 1 1 d . . .
H5A H 0.2271 1.0072 0.9473 0.030 Uiso 1 1 calc R . .
H5B H 0.1676 1.1213 0.9572 0.030 Uiso 1 1 calc R . .
C6 C 0.20501(5) 0.93674(19) 1.04190(6) 0.0234(2) Uani 1 1 d . . .
C7 C 0.24051(5) 1.0185(2) 1.10283(6) 0.0295(3) Uani 1 1 d . . .
H7 H 0.2664 1.1330 1.1058 0.035 Uiso 1 1 calc R . .
C8 C 0.23081(5) 0.8978(2) 1.16039(6) 0.0318(3) Uani 1 1 d . . .
H8 H 0.2488 0.9169 1.2092 0.038 Uiso 1 1 calc R . .
C9 C 0.19046(5) 0.7484(2) 1.13173(6) 0.0269(3) Uani 1 1 d . . .
C10 C 0.16455(5) 0.5598(2) 1.15636(6) 0.0297(3) Uani 1 1 d . . .
H10A H 0.1926 0.4440 1.1584 0.036 Uiso 1 1 calc R . .
H10B H 0.1575 0.5815 1.2044 0.036 Uiso 1 1 calc R . .
C11 C 0.05859(5) 0.6350(2) 1.12465(7) 0.0329(3) Uani 1 1 d . . .
H11A H 0.0208 0.6092 1.0904 0.049 Uiso 1 1 calc R . .
H11B H 0.0684 0.7807 1.1244 0.049 Uiso 1 1 calc R . .
H11C H 0.0546 0.5951 1.1721 0.049 Uiso 1 1 calc R . .
C12 C 0.09240(6) 0.2948(2) 1.10513(7) 0.0331(3) Uani 1 1 d . . .
H12A H 0.0868 0.2555 1.1520 0.050 Uiso 1 1 calc R . .
H12B H 0.1253 0.2152 1.0940 0.050 Uiso 1 1 calc R . .
H12C H 0.0555 0.2677 1.0694 0.050 Uiso 1 1 calc R . .
N1 N 0.15255(4) 0.82185(15) 0.92497(5) 0.0219(2) Uani 1 1 d . . .
N2 N 0.17496(4) 0.77405(16) 1.05987(5) 0.0237(2) Uani 1 1 d . . .
N3 N 0.10686(4) 0.51438(16) 1.10502(5) 0.0255(2) Uani 1 1 d . . .
H13 H 0.0517(6) 0.694(2) 0.9772(7) 0.038(4) Uiso 1 1 d . . .
H14 H 0.1778(6) 0.734(2) 0.9144(7) 0.027(3) Uiso 1 1 d . . .
H15 H 0.1341(7) 0.428(2) 0.9698(8) 0.045(4) Uiso 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'
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
_geom_angle_publ_flag
N2 Al1 N1 78.04(4) . . ?
N2 Al1 N3 77.68(4) . . ?
N1 Al1 N3 155.62(4) . . ?
N1 C1 C3 110.10(9) . . ?
N1 C1 C2 105.75(10) . . ?
C3 C1 C2 109.88(10) . . ?
N1 C1 C4 111.40(9) . . ?
C3 C1 C4 109.95(11) . . ?
C2 C1 C4 109.68(10) . . ?
C6 C5 N1 108.16(9) . . ?
N2 C6 C7 108.71(10) . . ?
N2 C6 C5 115.24(9) . . ?
C7 C6 C5 135.93(11) . . ?
C6 C7 C8 106.70(11) . . ?
C9 C8 C7 106.79(10) . . ?
N2 C9 C8 108.67(11) . . ?
N2 C9 C10 113.32(10) . . ?
C8 C9 C10 137.66(11) . . ?
N3 C10 C9 107.99(9) . . ?
C5 N1 C1 114.42(9) . . ?
C5 N1 Al1 110.50(7) . . ?
C1 N1 Al1 119.87(7) . . ?
C6 N2 C9 109.12(9) . . ?
C6 N2 Al1 125.33(8) . . ?
C9 N2 Al1 125.24(8) . . ?
C12 N3 C11 109.77(10) . . ?
C12 N3 C10 111.02(9) . . ?
C11 N3 C10 108.96(10) . . ?
C12 N3 Al1 113.06(7) . . ?
C11 N3 Al1 107.07(7) . . ?
C10 N3 Al1 106.79(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 N2 1.8487(10) . ?
Al1 N1 2.2030(10) . ?
Al1 N3 2.2543(10) . ?
C1 N1 1.5108(14) . ?
C1 C3 1.5257(17) . ?
C1 C2 1.5279(17) . ?
C1 C4 1.5303(17) . ?
C5 C6 1.5002(15) . ?
C5 N1 1.5017(14) . ?
C6 N2 1.3567(15) . ?
C6 C7 1.3812(16) . ?
C7 C8 1.4249(18) . ?
C8 C9 1.3747(17) . ?
C9 N2 1.3668(14) . ?
C9 C10 1.4950(18) . ?
C10 N3 1.4948(14) . ?
C11 N3 1.4788(15) . ?
C12 N3 1.4760(17) . ?
