#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:13:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179367 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/64/4326422.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_4326422
loop_
_publ_author_name
'Christopher J. Snyder'
'Mary Jane Heeg'
'Charles H. Winter'
_publ_contact_author             'Prof. Charles H. Winter'
_publ_contact_author_address
; Department of Chemistry
     Wayne State University
 Detroit, Michigan 48202
 USA
;
_publ_contact_author_email       chw@chem.wayne.edu
_publ_section_title
;
 Poly(pyrazolyl)aluminate Complexes Containing Aluminum-Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9210
_journal_page_last               9212
_journal_paper_doi               10.1021/ic201541c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C80 H84 Al Li N8 O5'
_chemical_formula_weight         1271.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5326(7)
_cell_length_b                   15.5326(7)
_cell_length_c                   13.9967(10)
_cell_measurement_reflns_used    7817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.6
_cell_volume                     3376.9(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_method       'Bruker APEX2'
_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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29852
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       rod
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0465
_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)+(0.0539P)²+1.3911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                3414
_reflns_number_total             4139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201541c_si_002_4.cif
_cod_data_source_block           adyn
_cod_database_code               4326422
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-y, x, -z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-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
O1 O 0.46434(12) 0.09380(10) 0.82593(11) 0.0460(4) Uani 1 1 d . . .
C16 C 0.43591(16) 0.09670(16) 0.92331(14) 0.0396(5) Uani 1 1 d . B .
H16A H 0.4856 0.0986 0.9675 0.047 Uiso 1 1 calc R . .
H16B H 0.4004 0.0457 0.9388 0.047 Uiso 1 1 calc R . .
C17 C 0.38305(17) 0.17857(18) 0.93061(18) 0.0493(6) Uani 1 1 d . . .
H17A H 0.3211 0.1667 0.9202 0.059 Uiso 1 1 calc R B .
H17B H 0.3906 0.2062 0.9938 0.059 Uiso 1 1 calc R . .
C18 C 0.4191(2) 0.23424(18) 0.8518(2) 0.0657(8) Uani 1 1 d . B .
H18A H 0.3720 0.2598 0.8136 0.079 Uiso 1 1 calc R A 1
H18B H 0.4545 0.2814 0.8788 0.079 Uiso 1 1 calc R A 1
C19 C 0.4700(5) 0.1798(5) 0.7949(6) 0.081(2) Uiso 0.50 1 d P B 1
H19A H 0.5307 0.1990 0.7977 0.097 Uiso 0.50 1 calc PR B 1
H19B H 0.4506 0.1837 0.7276 0.097 Uiso 0.50 1 calc PR B 1
C19' C 0.4304(3) 0.1704(2) 0.7725(2) 0.0207(7) Uiso 0.50 1 d P B 2
H19C H 0.4722 0.1911 0.7243 0.025 Uiso 0.50 1 calc PR B 2
H19D H 0.3749 0.1574 0.7407 0.025 Uiso 0.50 1 calc PR B 2
Li1 Li 0.5000 0.0000 0.7500 0.0314(14) Uani 1 4 d S . .
Al1 Al 0.5000 0.0000 0.2500 0.0189(2) Uani 1 4 d S . .
N1 N 0.58562(10) -0.04084(10) 0.33224(11) 0.0217(3) Uani 1 1 d . . .
N2 N 0.54951(10) -0.10800(10) 0.38229(10) 0.0222(3) Uani 1 1 d . . .
C1 C 0.67199(12) -0.03673(12) 0.35088(13) 0.0232(4) Uani 1 1 d . . .
C2 C 0.69141(12) -0.10231(12) 0.41376(12) 0.0237(4) Uani 1 1 d . . .
H2 H 0.7463 -0.1158 0.4397 0.028 Uiso 1 1 calc R . .
C3 C 0.61339(12) -0.14503(12) 0.43146(13) 0.0219(4) Uani 1 1 d . . .
C4 C 0.72971(12) 0.02862(12) 0.31179(12) 0.0230(4) Uani 1 1 d . . .
C5 C 0.81394(13) 0.00640(13) 0.28922(14) 0.0299(4) Uani 1 1 d . . .
H5 H 0.8322 -0.0515 0.2969 0.036 Uiso 1 1 calc R . .
C6 C 0.87147(14) 0.06698(14) 0.25578(18) 0.0393(5) Uani 1 1 d . . .
H6 H 0.9288 0.0505 0.2408 0.047 Uiso 1 1 calc R . .
C7 C 0.84610(14) 0.15098(14) 0.24416(16) 0.0361(5) Uani 1 1 d . . .
H7 H 0.8859 0.1928 0.2216 0.043 Uiso 1 1 calc R . .
C8 C 0.76272(14) 0.17444(13) 0.26532(15) 0.0316(4) Uani 1 1 d . . .
H8 H 0.7446 0.2322 0.2556 0.038 Uiso 1 1 calc R . .
C9 C 0.70505(13) 0.11389(12) 0.30083(13) 0.0263(4) Uani 1 1 d . . .
H9 H 0.6483 0.1311 0.3177 0.032 Uiso 1 1 calc R . .
C10 C 0.59705(12) -0.22017(12) 0.49285(12) 0.0230(4) Uani 1 1 d . . .
C11 C 0.66190(13) -0.25437(13) 0.54989(14) 0.0267(4) Uani 1 1 d . . .
H11 H 0.7174 -0.2286 0.5495 0.032 Uiso 1 1 calc R . .
C12 C 0.64679(13) -0.32564(13) 0.60741(14) 0.0288(4) Uani 1 1 d . . .
H12 H 0.6918 -0.3487 0.6456 0.035 Uiso 1 1 calc R . .
C13 C 0.56563(14) -0.36294(13) 0.60872(15) 0.0309(4) Uani 1 1 d . . .
H13 H 0.5548 -0.4115 0.6483 0.037 Uiso 1 1 calc R . .
C14 C 0.50083(13) -0.32968(13) 0.55281(14) 0.0298(4) Uani 1 1 d . . .
H14 H 0.4453 -0.3552 0.5538 0.036 Uiso 1 1 calc R . .
C15 C 0.51652(13) -0.25888(13) 0.49497(14) 0.0280(4) Uani 1 1 d . . .
H15 H 0.4715 -0.2366 0.4563 0.034 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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
C19 O1 C16 106.4(4) . .
C19 O1 C19' 27.8(3) . .
C16 O1 C19' 109.92(19) . .
C19 O1 Li1 122.7(3) . .
C16 O1 Li1 130.57(14) . .
C19' O1 Li1 115.76(16) . .
O1 C16 C17 104.89(18) . .
C18 C17 C16 103.3(2) . .
C19 C18 C19' 27.9(3) . .
C19 C18 C17 106.2(4) . .
C19' C18 C17 101.9(2) . .
C18 C19 O1 111.2(6) . .
C18 C19' O1 101.3(2) . .
O1 Li1 O1 108.50(5) 6_556 .
O1 Li1 O1 111.43(9) 6_556 7_546
O1 Li1 O1 108.50(5) . 7_546
O1 Li1 O1 108.50(5) 6_556 4_655
O1 Li1 O1 111.43(9) . 4_655
O1 Li1 O1 108.50(5) 7_546 4_655
N1 Al1 N1 112.27(5) 7_545 .
N1 Al1 N1 104.01(9) 7_545 6
N1 Al1 N1 112.27(5) . 6
N1 Al1 N1 112.27(5) 7_545 4_655
N1 Al1 N1 104.01(9) . 4_655
N1 Al1 N1 112.27(5) 6 4_655
C1 N1 N2 109.75(14) . .
C1 N1 Al1 143.03(13) . .
N2 N1 Al1 106.30(11) . .
C3 N2 N1 106.60(14) . .
N1 C1 C2 107.55(16) . .
N1 C1 C4 124.25(16) . .
C2 C1 C4 128.17(17) . .
C1 C2 C3 105.84(16) . .
N2 C3 C2 110.26(16) . .
N2 C3 C10 120.91(16) . .
C2 C3 C10 128.82(17) . .
C9 C4 C5 118.16(17) . .
C9 C4 C1 122.38(17) . .
C5 C4 C1 119.37(17) . .
C6 C5 C4 121.18(19) . .
C7 C6 C5 120.17(19) . .
C6 C7 C8 119.7(2) . .
C7 C8 C9 120.24(19) . .
C4 C9 C8 120.49(18) . .
C15 C10 C11 118.35(17) . .
C15 C10 C3 120.76(17) . .
C11 C10 C3 120.88(17) . .
C12 C11 C10 120.99(18) . .
C13 C12 C11 119.61(19) . .
C14 C13 C12 120.03(18) . .
C13 C14 C15 120.08(19) . .
C14 C15 C10 120.95(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C19 1.408(8) .
O1 C16 1.434(2) .
O1 C19' 1.501(4) .
O1 Li1 1.8866(15) .
C16 C17 1.517(4) .
C17 C18 1.509(4) .
C18 C19 1.405(8) .
C18 C19' 1.499(5) .
Li1 O1 1.8866(15) 6_556
Li1 O1 1.8866(15) 7_546
Li1 O1 1.8866(15) 4_655
Al1 N1 1.8697(15) 7_545
Al1 N1 1.8697(15) .
Al1 N1 1.8697(15) 6
Al1 N1 1.8697(15) 4_655
N1 C1 1.368(2) .
N1 N2 1.376(2) .
N2 C3 1.338(2) .
C1 C2 1.380(3) .
C1 C4 1.461(3) .
C2 C3 1.404(3) .
C3 C10 1.471(3) .
C4 C9 1.387(3) .
C4 C5 1.389(3) .
C5 C6 1.380(3) .
C6 C7 1.373(3) .
C7 C8 1.378(3) .
C8 C9 1.391(3) .
C10 C15 1.388(3) .
C10 C11 1.391(3) .
C11 C12 1.389(3) .
C12 C13 1.388(3) .
C13 C14 1.376(3) .
C14 C15 1.387(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C19 O1 C16 C17 28.6(4) . .
C19' O1 C16 C17 -0.5(3) . .
Li1 O1 C16 C17 -157.25(18) . .
O1 C16 C17 C18 -25.3(3) . .
C16 C17 C18 C19 13.0(5) . .
C16 C17 C18 C19' 41.4(3) . .
C19' C18 C19 O1 -80.4(8) . .
C17 C18 C19 O1 4.4(7) . .
C16 O1 C19 C18 -21.2(7) . .
C19' O1 C19 C18 80.4(8) . .
Li1 O1 C19 C18 164.0(4) . .
C19 C18 C19' O1 61.5(8) . .
C17 C18 C19' O1 -40.7(3) . .
C19 O1 C19' C18 -61.5(8) . .
C16 O1 C19' C18 26.1(3) . .
Li1 O1 C19' C18 -173.4(2) . .
C19 O1 Li1 O1 32.6(4) . 6_556
C16 O1 Li1 O1 -140.76(19) . 6_556
C19' O1 Li1 O1 63.6(2) . 6_556
C19 O1 Li1 O1 -88.6(4) . 7_546
C16 O1 Li1 O1 98.02(16) . 7_546
C19' O1 Li1 O1 -57.6(2) . 7_546
C19 O1 Li1 O1 152.0(4) . 4_655
C16 O1 Li1 O1 -21.37(17) . 4_655
C19' O1 Li1 O1 -177.0(2) . 4_655
N1 Al1 N1 C1 -7.8(2) 7_545 .
N1 Al1 N1 C1 108.9(2) 6 .
N1 Al1 N1 C1 -129.5(2) 4_655 .
N1 Al1 N1 N2 -174.78(11) 7_545 .
N1 Al1 N1 N2 -58.02(8) 6 .
N1 Al1 N1 N2 63.60(9) 4_655 .
C1 N1 N2 C3 -0.02(18) . .
Al1 N1 N2 C3 171.68(11) . .
N2 N1 C1 C2 0.04(19) . .
Al1 N1 C1 C2 -166.63(16) . .
N2 N1 C1 C4 -178.06(16) . .
Al1 N1 C1 C4 15.3(3) . .
N1 C1 C2 C3 -0.1(2) . .
C4 C1 C2 C3 177.95(17) . .
N1 N2 C3 C2 -0.02(19) . .
N1 N2 C3 C10 -179.60(16) . .
C1 C2 C3 N2 0.0(2) . .
C1 C2 C3 C10 179.59(17) . .
N1 C1 C4 C9 38.2(3) . .
C2 C1 C4 C9 -139.5(2) . .
N1 C1 C4 C5 -145.30(18) . .
C2 C1 C4 C5 37.0(3) . .
C9 C4 C5 C6 -0.7(3) . .
C1 C4 C5 C6 -177.4(2) . .
C4 C5 C6 C7 0.0(4) . .
C5 C6 C7 C8 -0.5(3) . .
C6 C7 C8 C9 1.8(3) . .
C5 C4 C9 C8 2.0(3) . .
C1 C4 C9 C8 178.53(18) . .
C7 C8 C9 C4 -2.6(3) . .
N2 C3 C10 C15 5.5(3) . .
C2 C3 C10 C15 -174.03(18) . .
N2 C3 C10 C11 -174.76(17) . .
C2 C3 C10 C11 5.7(3) . .
C15 C10 C11 C12 0.2(3) . .
C3 C10 C11 C12 -179.56(18) . .
C10 C11 C12 C13 -0.6(3) . .
C11 C12 C13 C14 0.4(3) . .
C12 C13 C14 C15 0.0(3) . .
C13 C14 C15 C10 -0.4(3) . .
C11 C10 C15 C14 0.3(3) . .
C3 C10 C15 C14 -179.94(18) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.500 0.000 127.1 41.0
2 0.000 0.000 0.500 127.1 40.9
