#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:48:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179937 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/32/7023283.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_7023283
loop_
_publ_author_name
'Liu, Pei-Hsin'
'Chuang, Fu-Jung'
'Tu, Cheng-Yi'
'Hu, Ching-Han'
'Lin, Tzu-Wei'
'Wang, Yu-Tang'
'Lin, Chia-Her'
'Datta, Amitabha'
'Huang, Jui-Hsien'
_publ_section_title
;
 Aluminum complexes incorporating symmetrical and asymmetrical tridentate
 pincer type pyrrolyl ligands: synthesis, characterization and reactivity
 study.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13754
_journal_page_last               13764
_journal_paper_doi               10.1039/c3dt51133b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C12 H22 Al Cl2 N3'
_chemical_formula_sum            'C12 H22 Al Cl2 N3'
_chemical_formula_weight         306.21
_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                 112.575(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5365(4)
_cell_length_b                   13.4673(4)
_cell_length_c                   10.0304(3)
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.01
_cell_volume                     1563.70(9)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21774
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.054
_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     168
_refine_ls_number_reflns         3884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0330
_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)+(0.0480P)²+0.5836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                3283
_reflns_number_total             3884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51133b.txt
_cod_data_source_block           pei1081_0m
_cod_original_cell_volume        1563.70(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7023283
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
Cl1 Cl 0.05659(3) 0.89602(3) 0.80388(4) 0.03165(11) Uani 1 1 d .
Cl2 Cl 0.20143(4) 1.10378(3) 1.02636(4) 0.03397(11) Uani 1 1 d .
Al3 Al 0.21732(4) 0.96034(3) 0.94205(4) 0.02222(11) Uani 1 1 d .
N1 N 0.34264(10) 0.88042(9) 0.97511(13) 0.0248(2) Uani 1 1 d .
N2 N 0.22956(11) 0.88266(9) 1.14042(14) 0.0272(3) Uani 1 1 d .
N3 N 0.29408(10) 1.02657(9) 0.79599(13) 0.0242(2) Uani 1 1 d .
H1 H 0.3281 1.0839 0.8459 0.029 Uiso 1 1 calc R
C1 C 0.30325(17) 1.12536(14) 0.58882(19) 0.0419(4) Uani 1 1 d .
H1A H 0.3593 1.0800 0.5751 0.063 Uiso 1 1 calc R
H1B H 0.3444 1.1770 0.6584 0.063 Uiso 1 1 calc R
H1C H 0.2564 1.1562 0.4963 0.063 Uiso 1 1 calc R
C2 C 0.16627(14) 0.98255(12) 0.54380(16) 0.0326(3) Uani 1 1 d .
H2A H 0.1188 0.9440 0.5832 0.049 Uiso 1 1 calc R
H2B H 0.2253 0.9394 0.5327 0.049 Uiso 1 1 calc R
H2C H 0.1172 1.0097 0.4495 0.049 Uiso 1 1 calc R
C3 C 0.13364(17) 1.13768(13) 0.6595(2) 0.0400(4) Uani 1 1 d .
H3A H 0.1719 1.1911 0.7274 0.060 Uiso 1 1 calc R
H3B H 0.0824 1.1009 0.6950 0.060 Uiso 1 1 calc R
H3C H 0.0882 1.1662 0.5647 0.060 Uiso 1 1 calc R
C4 C 0.22458(14) 1.06728(12) 0.64619(16) 0.0297(3) Uani 1 1 d .
C5 C 0.39825(13) 0.96787(12) 0.80218(15) 0.0280(3) Uani 1 1 d .
H5A H 0.3833 0.9372 0.7070 0.034 Uiso 1 1 calc R
H5B H 0.4658 1.0125 0.8260 0.034 Uiso 1 1 calc R
C6 C 0.42310(12) 0.88866(11) 0.91523(15) 0.0255(3) Uani 1 1 d .
C7 C 0.50473(13) 0.81580(12) 0.97190(17) 0.0309(3) Uani 1 1 d .
H7 H 0.5707 0.8045 0.9494 0.037 Uiso 1 1 calc R
C8 C 0.47150(13) 0.76021(12) 1.07124(17) 0.0321(3) Uani 1 1 d .
H8 H 0.5111 0.7050 1.1275 0.039 Uiso 1 1 calc R
C9 C 0.37121(13) 0.80218(11) 1.06930(16) 0.0285(3) Uani 1 1 d .
C10 C 0.28202(14) 0.78403(12) 1.13254(18) 0.0325(3) Uani 1 1 d .
H10A H 0.2220 0.7378 1.0707 0.039 Uiso 1 1 calc R
H10B H 0.3184 0.7546 1.2301 0.039 Uiso 1 1 calc R
C11 C 0.11872(15) 0.86759(14) 1.15932(19) 0.0368(4) Uani 1 1 d .
H11A H 0.0848 0.9322 1.1649 0.055 Uiso 1 1 calc R
H11B H 0.1331 0.8304 1.2486 0.055 Uiso 1 1 calc R
H11C H 0.0652 0.8302 1.0770 0.055 Uiso 1 1 calc R
C12 C 0.30997(15) 0.93533(14) 1.26955(17) 0.0368(4) Uani 1 1 d .
H12A H 0.3242 0.8945 1.3555 0.055 Uiso 1 1 calc R
H12B H 0.2758 0.9988 1.2801 0.055 Uiso 1 1 calc R
H12C H 0.3832 0.9476 1.2584 0.055 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'
Cl Cl 0.1484 0.1585 '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
N1 Al3 Cl1 114.15(5)
N1 Al3 Cl2 131.42(5)
Cl1 Al3 Cl2 114.33(2)
N1 Al3 N2 78.42(5)
Cl1 Al3 N2 96.58(4)
Cl2 Al3 N2 93.23(4)
N1 Al3 N3 78.26(5)
Cl1 Al3 N3 105.86(4)
Cl2 Al3 N3 91.58(4)
N2 Al3 N3 152.66(5)
C6 N1 C9 108.99(12)
C6 N1 Al3 127.07(10)
C9 N1 Al3 123.93(10)
C12 N2 C11 108.03(12)
C12 N2 C10 107.80(13)
C11 N2 C10 109.67(12)
C12 N2 Al3 110.53(10)
C11 N2 Al3 115.85(10)
C10 N2 Al3 104.68(9)
C5 N3 C4 112.86(11)
C5 N3 Al3 110.46(9)
C4 N3 Al3 124.52(9)
N3 C4 C2 109.95(12)
N3 C4 C3 107.52(12)
C2 C4 C3 110.07(14)
N3 C4 C1 110.34(13)
C2 C4 C1 109.93(13)
C3 C4 C1 108.99(14)
C6 C5 N3 109.23(11)
N1 C6 C7 108.63(13)
N1 C6 C5 114.66(12)
C7 C6 C5 136.60(13)
C6 C7 C8 106.99(13)
C9 C8 C7 106.55(14)
N1 C9 C8 108.83(13)
N1 C9 C10 112.15(12)
C8 C9 C10 138.90(15)
N2 C10 C9 106.92(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 Al3 2.1418(6)
Cl2 Al3 2.1485(5)
Al3 N1 1.8266(13)
Al3 N2 2.2006(13)
Al3 N3 2.2249(12)
N1 C6 1.3623(18)
N1 C9 1.3680(19)
N2 C12 1.481(2)
N2 C11 1.4867(19)
N2 C10 1.4977(19)
N3 C5 1.5073(19)
N3 C4 1.5206(19)
C1 C4 1.533(2)
C2 C4 1.521(2)
C3 C4 1.528(2)
C5 C6 1.500(2)
C6 C7 1.374(2)
C7 C8 1.430(2)
C8 C9 1.372(2)
C9 C10 1.502(2)
