#------------------------------------------------------------------------------
#$Date: 2016-01-27 09:37:59 +0200 (Wed, 27 Jan 2016) $
#$Revision: 175148 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/40/7224032.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_7224032
loop_
_publ_author_name
'Huang, Jui-Hsien'
'Hu, Ting-Jia'
'Wu, Ming-Chun'
'Wu, Shih-Sheng'
'Hu, Ching-Han'
'Lin, Chia-Her'
'Datta, Amitabha'
'Lin, Tzung-Han'
_publ_section_title
;
 Synthesis, Characterization and Reactivity Study of Aluminum Compounds
 Incorporating Bi- and Tri-dentate Pyrrole-piperazine Ligands
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA01694D
_journal_year                    2016
_chemical_formula_sum            'C30.5 H38.5 Al N3 O1.5'
_chemical_formula_weight         498.12
_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
_audit_update_record
;
2015-07-18 deposited with the CCDC.
2016-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.230(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.8669(10)
_cell_length_b                   12.1406(5)
_cell_length_c                   18.5317(6)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.73
_cell_volume                     5468.0(4)
_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      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39369
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.9762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0869P)²+6.7312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                3905
_reflns_number_total             7081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra01694d2.cif
_cod_data_source_block           lobo3530201
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C30.50 H38.50 Al N3 O1.50'
_cod_database_code               7224032
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
Al1 Al 0.74530(3) 0.77383(7) 0.58618(4) 0.0345(2) Uani 1 1 d .
C1 C 0.67790(13) 0.9861(3) 0.55425(19) 0.0535(8) Uani 1 1 d .
H1 H 0.6521 0.9782 0.5016 0.064 Uiso 1 1 calc R
C2 C 0.68265(15) 1.0757(3) 0.6010(2) 0.0628(9) Uani 1 1 d .
H2 H 0.6608 1.1385 0.5864 0.075 Uiso 1 1 calc R
C3 C 0.72677(15) 1.0555(3) 0.6754(2) 0.0598(9) Uani 1 1 d .
H3 H 0.7400 1.1025 0.7192 0.072 Uiso 1 1 calc R
C4 C 0.74647(12) 0.9535(3) 0.67093(17) 0.0455(7) Uani 1 1 d .
C5 C 0.79192(12) 0.8830(3) 0.72783(16) 0.0512(8) Uani 1 1 d .
H5A H 0.7779 0.8337 0.7560 0.061 Uiso 1 1 calc R
H5B H 0.8204 0.9286 0.7667 0.061 Uiso 1 1 calc R
C6 C 0.85074(12) 0.8920(3) 0.65783(18) 0.0502(7) Uani 1 1 d .
H6A H 0.8782 0.9256 0.7058 0.060 Uiso 1 1 calc R
H6B H 0.8283 0.9505 0.6239 0.060 Uiso 1 1 calc R
C7 C 0.87939(12) 0.8315(3) 0.61469(18) 0.0489(7) Uani 1 1 d .
H7A H 0.8521 0.8037 0.5642 0.059 Uiso 1 1 calc R
H7B H 0.9031 0.8822 0.6035 0.059 Uiso 1 1 calc R
C8 C 0.87832(13) 0.6661(3) 0.6856(2) 0.0570(9) Uani 1 1 d .
H8A H 0.9013 0.6079 0.7193 0.068 Uiso 1 1 calc R
H8B H 0.8504 0.6323 0.6382 0.068 Uiso 1 1 calc R
C9 C 0.85100(12) 0.7275(3) 0.72974(17) 0.0539(8) Uani 1 1 d .
H9A H 0.8291 0.6766 0.7445 0.065 Uiso 1 1 calc R
H9B H 0.8790 0.7585 0.7783 0.065 Uiso 1 1 calc R
C10 C 0.94850(9) 0.6884(2) 0.63393(14) 0.0522(8) Uani 1 1 d G
C11 C 0.97459(13) 0.75319(16) 0.5985(2) 0.111(2) Uani 1 1 d G
H11 H 0.9669 0.8281 0.5910 0.133 Uiso 1 1 calc R
C12 C 1.01213(12) 0.7060(2) 0.5743(2) 0.1080(19) Uani 1 1 d G
H12 H 1.0296 0.7493 0.5507 0.130 Uiso 1 1 calc R
C13 C 1.02357(10) 0.5940(2) 0.58554(16) 0.0730(11) Uani 1 1 d G
H13 H 1.0487 0.5624 0.5694 0.088 Uiso 1 1 calc R
C14 C 0.99749(13) 0.5292(2) 0.6209(2) 0.145(3) Uani 1 1 d G
H14 H 1.0051 0.4543 0.6284 0.174 Uiso 1 1 calc R
C15 C 0.95995(12) 0.5764(2) 0.6451(2) 0.141(3) Uani 1 1 d G
H15 H 0.9425 0.5331 0.6688 0.170 Uiso 1 1 calc R
C16 C 0.67925(11) 0.6023(2) 0.60891(16) 0.0415(6) Uani 1 1 d .
C17 C 0.67456(13) 0.5027(2) 0.56753(17) 0.0462(7) Uani 1 1 d .
C18 C 0.62746(15) 0.4406(3) 0.5484(2) 0.0608(9) Uani 1 1 d .
H18 H 0.6235 0.3746 0.5210 0.073 Uiso 1 1 calc R
C19 C 0.58608(15) 0.4742(3) 0.5690(2) 0.0671(10) Uani 1 1 d .
H19 H 0.5544 0.4319 0.5546 0.080 Uiso 1 1 calc R
C20 C 0.59194(13) 0.5698(3) 0.6107(2) 0.0608(9) Uani 1 1 d .
H20 H 0.5640 0.5918 0.6245 0.073 Uiso 1 1 calc R
C21 C 0.63871(12) 0.6351(3) 0.63312(18) 0.0470(7) Uani 1 1 d .
C22 C 0.72006(14) 0.4656(3) 0.54594(19) 0.0541(8) Uani 1 1 d .
H22 H 0.7318 0.5299 0.5252 0.065 Uiso 1 1 calc R
C23 C 0.77000(15) 0.4260(3) 0.6205(2) 0.0730(11) Uani 1 1 d .
H23A H 0.7809 0.4824 0.6605 0.110 Uiso 1 1 calc R
H23B H 0.7999 0.4103 0.6067 0.110 Uiso 1 1 calc R
H23C H 0.7604 0.3605 0.6407 0.110 Uiso 1 1 calc R
C24 C 0.70319(19) 0.3759(3) 0.4816(2) 0.0784(12) Uani 1 1 d .
H24A H 0.6959 0.3087 0.5025 0.118 Uiso 1 1 calc R
H24B H 0.7325 0.3642 0.4658 0.118 Uiso 1 1 calc R
H24C H 0.6707 0.3988 0.4362 0.118 Uiso 1 1 calc R
C25 C 0.64393(14) 0.7380(3) 0.6816(2) 0.0585(9) Uani 1 1 d .
H25 H 0.6807 0.7684 0.6958 0.070 Uiso 1 1 calc R
C26 C 0.60247(17) 0.8258(3) 0.6349(3) 0.0929(15) Uani 1 1 d .
H26A H 0.6065 0.8427 0.5870 0.139 Uiso 1 1 calc R
H26B H 0.6088 0.8910 0.6668 0.139 Uiso 1 1 calc R
H26C H 0.5659 0.7991 0.6212 0.139 Uiso 1 1 calc R
C27 C 0.63991(17) 0.7097(4) 0.7594(3) 0.0834(13) Uani 1 1 d .
H27A H 0.6059 0.6719 0.7475 0.125 Uiso 1 1 calc R
H27B H 0.6411 0.7762 0.7881 0.125 Uiso 1 1 calc R
H27C H 0.6702 0.6631 0.7914 0.125 Uiso 1 1 calc R
C29 C 1.0000 0.2659(5) 0.7500 0.0709(14) Uani 1 2 d S
H29 H 1.0000 0.3425 0.7500 0.085 Uiso 1 2 calc SR
C30 C 0.97302(15) 0.2110(3) 0.6790(2) 0.0685(10) Uani 1 1 d .
C31 C 0.97404(15) 0.0966(4) 0.6797(2) 0.0712(10) Uani 1 1 d .
H31 H 0.9569 0.0582 0.6319 0.085 Uiso 1 1 calc R
C32 C 1.0000 0.0390(5) 0.7500 0.0752(15) Uani 1 2 d S
H32 H 1.0000 -0.0377 0.7500 0.090 Uiso 1 2 calc SR
C33 C 0.9408(3) 0.2811(7) 0.6103(4) 0.080(2) Uani 0.50 1 d P
H33A H 0.9486 0.3571 0.6251 0.120 Uiso 0.50 1 calc PR
H33B H 0.9023 0.2674 0.5939 0.120 Uiso 0.50 1 calc PR
H33C H 0.9503 0.2645 0.5671 0.120 Uiso 0.50 1 calc PR
N2 N 0.81517(9) 0.8174(2) 0.67998(12) 0.0406(5) Uani 1 1 d .
N3 N 0.91209(10) 0.7401(2) 0.66251(14) 0.0512(7) Uani 1 1 d .
N1 N 0.71705(9) 0.90905(19) 0.59656(13) 0.0423(5) Uani 1 1 d .
O1 O 0.72493(7) 0.66616(16) 0.62762(11) 0.0417(5) Uani 1 1 d .
O2 O 0.7500 0.7500 0.5000 0.0415(6) Uani 1 2 d S
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'
O O 0.0106 0.0060 '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
O2 Al1 O1 117.44(8) .
O2 Al1 N1 116.83(8) .
O1 Al1 N1 113.88(10) .
O2 Al1 N2 116.52(7) .
O1 Al1 N2 99.87(10) .
N1 Al1 N2 87.13(10) .
C2 C1 N1 109.8(3) .
C1 C2 C3 107.2(3) .
C4 C3 C2 106.6(3) .
C3 C4 N1 110.3(3) .
C3 C4 C5 134.3(3) .
N1 C4 C5 115.5(2) .
C4 C5 N2 107.8(2) .
N2 C6 C7 112.3(3) .
N3 C7 C6 111.0(2) .
N3 C8 C9 111.1(3) .
N2 C9 C8 111.2(2) .
C11 C10 C15 120.0 .
C11 C10 N3 119.03(19) .
C15 C10 N3 120.88(19) .
C12 C11 C10 120.0 .
C13 C12 C11 120.0 .
C12 C13 C14 120.0 .
C13 C14 C15 120.0 .
C14 C15 C10 120.0 .
O1 C16 C21 119.7(3) .
O1 C16 C17 119.2(2) .
C21 C16 C17 121.1(3) .
C18 C17 C16 117.9(3) .
C18 C17 C22 121.7(3) .
C16 C17 C22 120.4(3) .
C19 C18 C17 121.6(3) .
C20 C19 C18 119.7(3) .
C19 C20 C21 121.6(3) .
C20 C21 C16 118.0(3) .
C20 C21 C25 119.4(3) .
C16 C21 C25 122.5(3) .
C17 C22 C24 114.5(3) .
C17 C22 C23 110.6(2) .
C24 C22 C23 109.4(3) .
C21 C25 C26 112.5(3) .
C21 C25 C27 110.4(3) .
C26 C25 C27 111.5(3) .
C30 C29 C30 122.0(6) 2_756
C29 C30 C31 118.4(4) .
C29 C30 C33 115.2(5) .
C31 C30 C33 126.1(5) .
C32 C31 C30 121.1(4) .
C31 C32 C31 119.0(6) 2_756
C9 N2 C6 107.1(2) .
C9 N2 C5 110.1(2) .
C6 N2 C5 108.3(2) .
C9 N2 Al1 117.5(2) .
C6 N2 Al1 113.10(17) .
C5 N2 Al1 100.30(16) .
C10 N3 C7 115.9(2) .
C10 N3 C8 116.3(2) .
C7 N3 C8 110.9(2) .
C4 N1 C1 106.1(2) .
C4 N1 Al1 111.49(19) .
C1 N1 Al1 142.3(2) .
C16 O1 Al1 137.80(17) .
Al1 O2 Al1 179.998(2) 7_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O2 1.6799(7) .
Al1 O1 1.7193(19) .
Al1 N1 1.853(2) .
Al1 N2 2.011(2) .
C1 C2 1.362(5) .
C1 N1 1.376(4) .
C2 C3 1.405(5) .
C3 C4 1.363(4) .
C4 N1 1.374(4) .
C4 C5 1.496(4) .
C5 N2 1.511(3) .
C6 N2 1.496(4) .
C6 C7 1.515(4) .
C7 N3 1.458(4) .
C8 N3 1.464(4) .
C8 C9 1.509(4) .
C9 N2 1.487(4) .
C10 C11 1.3900 .
C10 C15 1.3900 .
C10 N3 1.440(3) .
C11 C12 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C14 C15 1.3900 .
C16 O1 1.365(3) .
C16 C21 1.401(4) .
C16 C17 1.409(4) .
C17 C18 1.384(5) .
C17 C22 1.508(4) .
C18 C19 1.383(5) .
C19 C20 1.366(5) .
C20 C21 1.391(4) .
C21 C25 1.510(4) .
C22 C24 1.533(5) .
C22 C23 1.536(5) .
C25 C26 1.518(5) .
C25 C27 1.531(5) .
C29 C30 1.374(5) 2_756
C29 C30 1.374(5) .
C30 C31 1.390(6) .
C30 C33 1.467(9) .
C31 C32 1.378(5) .
C32 C31 1.378(5) 2_756
O2 Al1 1.6799(7) 7_666
