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#$Date: 2016-03-21 16:56:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178761 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/15/4101551.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_4101551
loop_
_publ_author_name
'Loiseau, Thierry'
'Lecroq, Ludovic'
'Volkringer, Christophe'
'Marrot, Jérôme'
'Férey, Gérard'
'Haouas, Mohamed'
'Taulelle, Francis'
'Bourrelly, Sandrine'
'Llewellyn, Philip L'
'Latroche, Michel'
_publ_section_title
;
 MIL-96, a porous aluminum trimesate 3D structure constructed from a
 hexagonal network of 18-membered rings and mu3-oxo-centered trinuclear
 units.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10223
_journal_page_last               10230
_journal_paper_doi               10.1021/ja0621086
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C6 H2 Al1.56 O7.33'
_chemical_formula_weight         233.38
_chemical_name_common            'MIL-96 (Al)'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   14.2074(2)
_cell_length_b                   14.2074(2)
_cell_length_c                   31.2302(9)
_cell_measurement_temperature    293(2)
_cell_volume                     5459.27(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            65893
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.219
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0509
_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)+(0.1187P)²+3.5760P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1807
_reflns_number_gt                1473
_reflns_number_total             1858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0621086si20060407_050628.cif
_cod_data_source_block           MIL96
_cod_original_sg_symbol_H-M      P63/mmc
_cod_database_code               4101551
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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 0.07451(7) 0.14903(13) 0.2500 0.0118(4) Uani 1 4 d S
Al2 Al 0.16926(9) 0.58463(5) 0.41657(4) 0.0140(4) Uani 1 2 d S
Al3 Al 0.0000 0.5000 0.5000 0.0121(4) Uani 1 4 d S
Al4 Al 0.26760(13) 0.73240(13) 0.33447(10) 0.0076(7) Uiso 0.33 2 d SP
O1 O 0.0000 0.0000 0.2500 0.0116(13) Uani 1 12 d S
O2 O 0.1342(2) 0.56708(11) 0.47425(8) 0.0127(6) Uani 1 2 d S
O3 O 0.27169(11) 0.72831(11) 0.42465(10) 0.0201(7) Uani 1 2 d S
O4 O 0.15356(17) 0.3071(3) 0.2500 0.0266(10) Uani 1 4 d S
O5 O 0.1973(3) 0.59864(16) 0.35686(11) 0.0616(14) Uani 1 2 d S
O6 O -0.0489(2) 0.3831(2) 0.46235(10) 0.0604(11) Uani 1 1 d .
O7 O -0.00872(18) 0.16451(17) 0.29369(7) 0.0270(6) Uani 1 1 d .
O8 O 0.06292(17) 0.43666(17) 0.40605(7) 0.0271(6) Uani 1 1 d .
C1 C -0.0628(3) 0.2315(3) 0.36778(11) 0.0330(9) Uani 1 1 d .
H1 H 0.0033 0.2785 0.3548 0.040 Uiso 1 1 calc R
C2 C -0.1324(2) 0.1324(2) 0.34903(15) 0.0302(11) Uani 1 2 d S
C3 C -0.0908(3) 0.2611(3) 0.40566(12) 0.0379(10) Uani 1 1 d .
C4 C -0.1900(2) 0.1900(2) 0.42472(18) 0.0426(15) Uani 1 2 d S
H4 H -0.2090 0.2090 0.4505 0.051 Uiso 1 2 calc SR
C5 C -0.09957(17) 0.09957(17) 0.30903(14) 0.0203(10) Uani 1 2 d S
C6 C -0.0189(3) 0.3678(3) 0.42625(11) 0.0347(9) Uani 1 1 d .
OW O 0.3333 0.6667 0.5252(3) 0.076(3) Uiso 1 6 d S
O11 O 0.2116(4) 0.7884(4) 0.3306(3) 0.031(2) Uiso 0.33 2 d SP
O12 O 0.2925(4) 0.7075(4) 0.2935(3) 0.036(3) Uiso 0.33 2 d SP
O13 O 0.2412(5) 0.7588(5) 0.3007(4) 0.053(3) Uiso 0.33 2 d SP
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'
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'
H H 0.0000 0.0000 '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
O1 Al1 O7 95.79(8) . 16_556
O1 Al1 O7 95.79(8) . .
O7 Al1 O7 92.49(15) 16_556 .
O1 Al1 O7 95.79(8) . 20
O7 Al1 O7 168.43(16) 16_556 20
O7 Al1 O7 86.34(15) . 20
O1 Al1 O7 95.79(8) . 11
O7 Al1 O7 86.34(15) 16_556 11
O7 Al1 O7 168.43(16) . 11
O7 Al1 O7 92.49(15) 20 11
O1 Al1 O4 180.0 . .
O7 Al1 O4 84.21(8) 16_556 .
O7 Al1 O4 84.21(8) . .
O7 Al1 O4 84.21(8) 20 .
O7 Al1 O4 84.21(8) 11 .
O3 Al2 O3 91.25(18) 2_665 .
O3 Al2 O2 91.52(12) 2_665 .
O3 Al2 O2 91.52(12) . .
O3 Al2 O5 90.59(13) 2_665 .
O3 Al2 O5 90.59(14) . .
O2 Al2 O5 176.99(16) . .
O3 Al2 O8 89.39(11) 2_665 .
O3 Al2 O8 177.93(14) . .
O2 Al2 O8 90.43(10) . .
O5 Al2 O8 87.44(12) . .
O3 Al2 O8 177.93(14) 2_665 21_565
O3 Al2 O8 89.39(11) . 21_565
O2 Al2 O8 90.43(10) . 21_565
O5 Al2 O8 87.44(12) . 21_565
O8 Al2 O8 89.90(16) . 21_565
O2 Al3 O2 180.00(18) 13_566 .
O2 Al3 O6 89.19(9) 13_566 21_565
O2 Al3 O6 90.81(9) . 21_565
O2 Al3 O6 90.81(9) 13_566 13_566
O2 Al3 O6 89.19(9) . 13_566
O6 Al3 O6 90.3(2) 21_565 13_566
O2 Al3 O6 89.19(9) 13_566 .
O2 Al3 O6 90.81(9) . .
O6 Al3 O6 89.7(2) 21_565 .
O6 Al3 O6 180.00(13) 13_566 .
O2 Al3 O6 90.81(9) 13_566 9_556
O2 Al3 O6 89.19(9) . 9_556
O6 Al3 O6 180.00(14) 21_565 9_556
O6 Al3 O6 89.7(2) 13_566 9_556
O6 Al3 O6 90.3(2) . 9_556
O13 Al4 O11 53.4(7) . .
O13 Al4 O12 57.2(7) . .
O11 Al4 O12 110.6(6) . .
O13 Al4 O5 124.17(19) . .
O11 Al4 O5 117.9(2) . .
O12 Al4 O5 99.5(3) . .
O13 Al4 O5 124.17(19) . 3_565
O11 Al4 O5 117.9(2) . 3_565
O12 Al4 O5 99.5(3) . 3_565
O5 Al4 O5 108.3(3) . 3_565
O13 Al4 Al4 117.0(5) . 3_565
O11 Al4 Al4 149.63(7) . 3_565
O12 Al4 Al4 68.1(4) . 3_565
O5 Al4 Al4 91.56(14) . 3_565
O5 Al4 Al4 38.46(13) 3_565 3_565
O13 Al4 Al4 117.0(5) . 2_665
O11 Al4 Al4 149.63(6) . 2_665
O12 Al4 Al4 68.1(4) . 2_665
O5 Al4 Al4 38.46(13) . 2_665
O5 Al4 Al4 91.56(14) 3_565 2_665
Al4 Al4 Al4 60.000(1) 3_565 2_665
Al1 O1 Al1 120.0 2 .
Al1 O1 Al1 120.0 2 3
Al1 O1 Al1 120.0 . 3
Al3 O2 Al2 129.46(15) . .
Al2 O3 Al2 144.08(18) 3_565 .
Al4 O5 Al4 103.1(3) . 2_665
Al4 O5 Al2 118.19(16) . .
Al4 O5 Al2 118.19(16) 2_665 .
C6 O6 Al3 135.2(2) . .
C5 O7 Al1 131.9(2) . .
C6 O8 Al2 133.5(2) . .
C3 C1 C2 120.4(3) . .
C1 C2 C1 120.2(4) . 19
C1 C2 C5 119.9(2) . .
C1 C2 C5 119.9(2) 19 .
C1 C3 C4 119.2(3) . .
C1 C3 C6 121.8(3) . .
C4 C3 C6 119.0(3) . .
C3 C4 C3 120.7(4) 19 .
O7 C5 O7 125.1(4) 19 .
O7 C5 C2 117.47(19) 19 .
O7 C5 C2 117.47(19) . .
O8 C6 O6 125.3(3) . .
O8 C6 C3 118.4(3) . .
O6 C6 C3 116.3(3) . .
O13 O11 Al4 57.0(8) . .
O13 O12 Al4 54.3(7) . .
O13 O12 O12 148.5(2) . 2_665
Al4 O12 O12 111.9(4) . 2_665
O13 O12 O12 148.5(2) . 3_565
Al4 O12 O12 111.9(4) . 3_565
O12 O12 O12 60.000(3) 2_665 3_565
O11 O13 Al4 69.5(9) . .
O11 O13 O12 138.1(13) . .
Al4 O13 O12 68.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.8336(16) .
Al1 O7 1.889(2) 16_556
Al1 O7 1.889(2) .
Al1 O7 1.889(2) 20
Al1 O7 1.889(2) 11
Al1 O4 1.945(5) .
Al2 O3 1.8378(12) 2_665
Al2 O3 1.8378(12) .
Al2 O2 1.852(3) .
Al2 O5 1.896(3) .
Al2 O8 1.906(2) .
Al2 O8 1.906(2) 21_565
Al3 O2 1.836(3) 13_566
Al3 O2 1.836(3) .
Al3 O6 1.863(2) 21_565
Al3 O6 1.863(2) 13_566
Al3 O6 1.863(2) .
Al3 O6 1.863(2) 9_556
Al4 O13 1.239(13) .
Al4 O11 1.384(10) .
Al4 O12 1.420(11) .
Al4 O5 1.789(3) .
Al4 O5 1.789(3) 3_565
Al4 Al4 2.802(6) 3_565
Al4 Al4 2.802(6) 2_665
O1 Al1 1.8336(17) 2
O1 Al1 1.8336(16) 3
O3 Al2 1.8378(12) 3_565
O5 Al4 1.789(3) 2_665
O6 C6 1.262(4) .
O7 C5 1.247(3) .
O8 C6 1.253(4) .
C1 C3 1.380(5) .
C1 C2 1.382(4) .
C2 C1 1.382(4) 19
C2 C5 1.487(6) .
C3 C4 1.392(4) .
C3 C6 1.486(5) .
C4 C3 1.392(4) 19
C5 O7 1.247(3) 19
O11 O13 1.187(15) .
O12 O13 1.282(16) .
O12 O12 1.740(18) 2_665
O12 O12 1.740(18) 3_565
