#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:30:41 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179666 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/19/4511942.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_4511942
loop_
_publ_author_name
'Wharmby, Michael T.'
'Snoyek, Malte'
'Rhauderwiek, Timo'
'Ritter, Knut'
'Stock, Norbert'
_publ_section_title
;
 Group 13 Metal Carboxylates: Using Molecular Clusters As Hybrid Building
 Units in a MIL-53 Type Framework
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5310
_journal_paper_doi               10.1021/cg501189n
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C16 H12 Al2 N2 O16'
_chemical_formula_sum            'C16 H12 Al2 N2 O16'
_chemical_formula_weight         542.24
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.12.10 svn.r2853 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.700(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6630(8)
_cell_length_b                   11.7211(8)
_cell_length_c                   6.4221(4)
_cell_measurement_reflns_used    525
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      2.0
_cell_volume                     1013.77(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
    Reference Run
      Phi                  : 0.0
      Omega range          : 0.0 - 10.0
      Omega increment      : 10.0
      Exposure time [min]  : 2.0
      Frames               : 1
      Interval [h]         : 0.00

    Run #1
      Phi                  : 0.0
      Omega range          : 0.0 - 150.0
      Omega increment      : 1.0
      Exposure time [min]  : 30.0
      Frames               : 150

    Run #2
      Phi                  : 90.0
      Omega range          : 0.0 - 180.0
      Omega increment      : 1.0
      Exposure time [min]  : 30.0
      Frames               : 180
;
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       ψ-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6481
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.965
_diffrn_reflns_theta_min         2.303
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       Needle
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0384P)²+0.3642P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1847
_reflns_number_total             2415
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg501189n_si_003.cif
_cod_data_source_block           AlPTC2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511941--4511944.cif.
;
_cod_database_code               4511942
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5A)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Al1 Al 0.92516(6) 0.03660(6) 0.82994(12) 0.02148(18) Uani 1 1 d .
O1 O 0.86045(13) 0.15665(14) 0.9688(3) 0.0247(4) Uani 1 1 d .
O2 O 0.71681(15) 0.22687(17) 1.0347(3) 0.0305(4) Uani 1 1 d .
O3 O 0.93330(14) -0.09213(15) 0.6393(3) 0.0262(4) Uani 1 1 d .
O4 O 0.84741(17) -0.23485(18) 0.4620(3) 0.0372(5) Uani 1 1 d .
O5 O 0.47241(17) -0.21719(19) 0.5497(4) 0.0386(5) Uani 1 1 d .
H5 H 0.407(4) -0.235(4) 0.530(7) 0.062(13) Uiso 1 1 d .
O6 O 0.42438(16) -0.06732(19) 0.7248(4) 0.0407(5) Uani 1 1 d .
O7 O 1.05583(14) 0.05881(17) 0.9316(3) 0.0254(4) Uani 1 1 d .
H7 H 1.079(3) 0.113(3) 0.937(5) 0.032(10) Uiso 1 1 d .
O8 O 0.92592(16) 0.13316(18) 0.5961(3) 0.0309(4) Uani 1 1 d .
H8A H 0.899(4) 0.199(4) 0.572(7) 0.069(14) Uiso 1 1 d .
H8B H 0.967(3) 0.121(4) 0.516(7) 0.065(13) Uiso 1 1 d .
N1 N 0.78433(16) -0.00616(18) 0.7544(3) 0.0228(4) Uani 1 1 d .
C1 C 0.76508(19) 0.1544(2) 0.9578(4) 0.0232(5) Uani 1 1 d .
C2 C 0.71671(19) 0.0524(2) 0.8387(4) 0.0232(5) Uani 1 1 d .
C3 C 0.6192(2) 0.0154(2) 0.8117(4) 0.0271(5) Uani 1 1 d .
H3 H 0.5717 0.0552 0.8706 0.033 Uiso 1 1 calc R
C4 C 0.59427(19) -0.0837(2) 0.6934(4) 0.0270(5) Uani 1 1 d .
C5 C 0.6659(2) -0.1421(2) 0.6052(4) 0.0274(5) Uani 1 1 d .
H5A H 0.6497 -0.2075 0.5249 0.033 Uiso 1 1 calc R
C6 C 0.7619(2) -0.1001(2) 0.6404(4) 0.0248(5) Uani 1 1 d .
C7 C 0.8535(2) -0.1490(2) 0.5708(4) 0.0262(5) Uani 1 1 d .
C8 C 0.4877(2) -0.1214(2) 0.6601(4) 0.0290(6) Uani 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'
Al Al 0.0645 0.0514 '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'
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 Al1 100.82(7) . 3_757
O1 Al1 O3 156.56(9) . .
O1 Al1 N1 78.30(8) . .
O3 Al1 Al1 97.92(7) . 3_757
O3 Al1 N1 78.81(9) . .
O7 Al1 Al1 38.39(6) 3_757 3_757
O7 Al1 Al1 40.04(6) . 3_757
O7 Al1 O1 103.06(9) . .
O7 Al1 O1 93.88(9) 3_757 .
O7 Al1 O3 92.09(9) 3_757 .
O7 Al1 O3 100.34(9) . .
O7 Al1 O7 78.43(10) . 3_757
O7 Al1 O8 171.86(10) 3_757 .
O7 Al1 O8 93.64(10) . .
O7 Al1 N1 92.55(9) 3_757 .
O7 Al1 N1 170.92(9) . .
O8 Al1 Al1 133.66(8) . 3_757
O8 Al1 O1 89.70(9) . .
O8 Al1 O3 87.47(9) . .
O8 Al1 N1 95.34(10) . .
N1 Al1 Al1 130.93(8) . 3_757
C1 O1 Al1 119.30(15) . .
C7 O3 Al1 118.53(16) . .
Al1 O7 Al1 101.57(10) . 3_757
C2 N1 Al1 118.89(17) . .
C6 N1 Al1 118.13(17) . .
C6 N1 C2 122.5(2) . .
O1 C1 C2 113.2(2) . .
O2 C1 O1 124.6(2) . .
O2 C1 C2 122.1(2) . .
N1 C2 C1 109.8(2) . .
N1 C2 C3 120.3(2) . .
C3 C2 C1 129.9(2) . .
C2 C3 C4 118.0(2) . .
C3 C4 C8 117.6(2) . .
C5 C4 C3 120.4(2) . .
C5 C4 C8 121.9(2) . .
C6 C5 C4 118.1(2) . .
N1 C6 C5 120.6(2) . .
N1 C6 C7 110.6(2) . .
C5 C6 C7 128.8(2) . .
O3 C7 C6 113.4(2) . .
O4 C7 O3 126.4(3) . .
O4 C7 C6 120.1(2) . .
O5 C8 C4 112.7(2) . .
O6 C8 O5 125.0(3) . .
O6 C8 C4 122.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.9549(18) .
Al1 O3 1.9582(19) .
Al1 O7 1.813(2) .
Al1 O7 1.879(2) 3_757
Al1 O8 1.882(2) .
Al1 N1 1.968(2) .
O1 C1 1.293(3) .
O2 C1 1.229(3) .
O3 C7 1.290(3) .
O4 C7 1.220(3) .
O5 C8 1.326(3) .
O6 C8 1.201(4) .
O7 Al1 1.879(2) 3_757
N1 C2 1.337(3) .
N1 C6 1.329(3) .
C1 C2 1.510(3) .
C2 C3 1.384(4) .
C3 C4 1.397(4) .
C4 C5 1.391(4) .
C4 C8 1.503(4) .
C5 C6 1.384(4) .
C6 C7 1.511(4) .
