#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:54:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179546 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/15/4501539.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_4501539
loop_
_publ_author_name
'Lama, Prem'
'Aijaz, Arshad'
'Neogi, Subhadip'
'Barbour, Leonard J.'
'Bharadwaj, Parimal K.'
_publ_section_title
;
 Microporous La(III) Metal−Organic Framework Using a Semirigid
 Tricarboxylic Ligand: Synthesis, Single-Crystal to Single-Crystal
 Sorption Properties, and Gas Adsorption Studies
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3410
_journal_paper_doi               10.1021/cg100078b
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C18 H19 La O12'
_chemical_formula_sum            'C18 H19 La O12'
_chemical_formula_weight         566.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.429(6)
_cell_angle_beta                 97.914(2)
_cell_angle_gamma                111.386(5)
_cell_formula_units_Z            2
_cell_length_a                   9.491(5)
_cell_length_b                   10.052(3)
_cell_length_c                   11.344(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.2
_cell_volume                     988.6(7)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_molecular_graphics    'DIAMOND 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'BRUKER SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7005
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    2.227
_exptl_absorpt_correction_T_max  0.7759
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.547
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0791
_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)+(0.0716P)²+37.5856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.1993
_reflns_number_gt                3105
_reflns_number_total             3522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100078b_si_002.cif
_cod_data_source_block           Compound1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4501539
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
La1 La 0.78599(8) 0.54591(7) 0.98706(6) 0.0099(2) Uani 1 1 d .
O1 O 0.5530(10) 0.3366(9) 0.9730(8) 0.0164(18) Uani 1 1 d .
O2 O 0.3147(10) 0.2611(9) 1.0077(8) 0.0166(18) Uiso 1 1 d .
O3 O -0.0447(10) -0.2519(9) 0.8861(8) 0.0175(19) Uani 1 1 d .
O4 O 0.0808(9) -0.3966(9) 0.9214(8) 0.0143(17) Uani 1 1 d .
O5 O 0.5621(9) -0.1077(9) 0.7384(7) 0.0141(18) Uani 1 1 d .
O6 O 0.2269(9) -0.3794(9) 0.2001(8) 0.0175(19) Uani 1 1 d .
O7 O 0.3826(10) -0.4945(9) 0.2274(7) 0.0152(18) Uani 1 1 d .
O8 O 1.1239(15) 0.3149(17) 0.5837(11) 0.060(4) Uani 1 1 d D
C1 C 0.4194(15) 0.2414(11) 0.9680(10) 0.016(3) Uani 1 1 d D
C2 C 0.3873(13) 0.0922(11) 0.9128(11) 0.013(2) Uani 1 1 d D
C3 C 0.2520(14) -0.0176(12) 0.9228(10) 0.012(2) Uani 1 1 d .
H3 H 0.1801 0.0033 0.9607 0.015 Uiso 1 1 calc R
C4 C 0.2226(13) -0.1597(13) 0.8762(10) 0.014(2) Uani 1 1 d .
C5 C 0.0770(13) -0.2758(12) 0.8940(10) 0.011(2) Uani 1 1 d .
C6 C 0.3279(14) -0.1920(13) 0.8171(11) 0.015(3) Uani 1 1 d .
H6 H 0.3112 -0.2868 0.7888 0.018 Uiso 1 1 calc R
C7 C 0.4571(13) -0.0797(14) 0.8019(12) 0.017(3) Uani 1 1 d .
C8 C 0.4927(13) 0.0630(13) 0.8507(11) 0.013(2) Uani 1 1 d .
H8 H 0.5836 0.1362 0.8423 0.016 Uiso 1 1 calc R
C9 C 0.5049(14) -0.1758(13) 0.6214(11) 0.016(3) Uani 1 1 d .
C10 C 0.3875(16) -0.1533(14) 0.5467(11) 0.021(3) Uani 1 1 d .
H10 H 0.3458 -0.0889 0.5746 0.025 Uiso 1 1 calc R
C11 C 0.3346(16) -0.2261(15) 0.4335(12) 0.022(3) Uani 1 1 d .
H11 H 0.2551 -0.2120 0.3853 0.027 Uiso 1 1 calc R
C12 C 0.3954(14) -0.3200(13) 0.3881(11) 0.015(2) Uani 1 1 d .
C13 C 0.3343(14) -0.4021(12) 0.2661(11) 0.016(3) Uani 1 1 d .
C14 C 0.5155(16) -0.3363(15) 0.4593(12) 0.022(3) Uani 1 1 d .
H14 H 0.5621 -0.3943 0.4275 0.027 Uiso 1 1 calc R
C15 C 0.5703(16) -0.2685(16) 0.5785(12) 0.026(3) Uani 1 1 d .
H15 H 0.6478 -0.2850 0.6271 0.031 Uiso 1 1 calc R
C16 C 0.979(4) 0.100(4) 0.449(3) 0.146(15) Uiso 1 1 d D
H16A H 0.9389 0.1629 0.4097 0.220 Uiso 1 1 calc R
H16B H 0.8964 0.0211 0.4694 0.220 Uiso 1 1 calc R
H16C H 1.0315 0.0631 0.3965 0.220 Uiso 1 1 calc R
C17 C 1.087(4) 0.180(2) 0.558(3) 0.120(12) Uiso 1 1 d D
C18 C 1.166(7) 0.115(5) 0.641(5) 0.27(3) Uiso 1 1 d D
H18A H 1.2337 0.1881 0.7048 0.406 Uiso 1 1 calc R
H18B H 1.2242 0.0738 0.5987 0.406 Uiso 1 1 calc R
H18C H 1.0916 0.0414 0.6739 0.406 Uiso 1 1 calc R
OW2 O 0.6925(11) 0.5452(10) 1.1922(8) 0.0196(19) Uani 1 1 d D
OW1 O 0.9971(10) 0.7216(10) 1.1517(8) 0.0184(19) Uani 1 1 d D
OW3 O 1.1106(11) 1.0179(9) 1.1929(9) 0.022(2) Uani 1 1 d D
OW4 O 0.980(8) 0.582(7) 0.592(6) 0.37(4) Uiso 1 1 d .
H1W1 H 1.04(3) 0.808(13) 1.13(2) 0.04(9) Uiso 1 1 d D
H2W1 H 0.93(2) 0.74(3) 1.19(2) 0.06(10) Uiso 1 1 d D
H1W2 H 0.766(14) 0.588(18) 1.257(9) 0.03(6) Uiso 1 1 d D
H2W2 H 0.611(13) 0.50(2) 1.226(14) 0.05(8) Uiso 1 1 d D
H2W3 H 1.089(12) 1.083(9) 1.152(8) 0.00(3) Uiso 1 1 d D
H1W3 H 1.186(16) 1.074(11) 1.253(11) 0.06(6) Uiso 1 1 d 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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 La1 O2 100.9(3) . 2_667
O1 La1 O4 85.7(3) . 2_657
O2 La1 O4 154.1(3) 2_667 2_657
O1 La1 OW1 137.7(3) . .
O2 La1 OW1 83.0(3) 2_667 .
O4 La1 OW1 75.7(3) 2_657 .
O1 La1 O3 148.7(3) . 1_665
O2 La1 O3 72.3(3) 2_667 1_665
O4 La1 O3 114.1(3) 2_657 1_665
OW1 La1 O3 72.9(3) . 1_665
O1 La1 O6 74.3(3) . 2_656
O2 La1 O6 126.1(3) 2_667 2_656
O4 La1 O6 79.7(3) 2_657 2_656
OW1 La1 O6 136.3(3) . 2_656
O3 La1 O6 85.3(3) 1_665 2_656
O1 La1 OW2 71.5(3) . .
O2 La1 OW2 75.9(3) 2_667 .
O4 La1 OW2 82.8(3) 2_657 .
OW1 La1 OW2 68.8(3) . .
O3 La1 OW2 132.3(3) 1_665 .
O6 La1 OW2 142.5(3) 2_656 .
O1 La1 O7 69.7(3) . 2_656
O2 La1 O7 77.5(3) 2_667 2_656
O4 La1 O7 127.8(3) 2_657 2_656
OW1 La1 O7 149.6(3) . 2_656
O3 La1 O7 79.0(3) 1_665 2_656
O6 La1 O7 50.0(3) 2_656 2_656
OW2 La1 O7 127.0(3) . 2_656
O1 La1 O4 136.0(3) . 1_665
O2 La1 O4 118.8(3) 2_667 1_665
O4 La1 O4 67.2(3) 2_657 1_665
OW1 La1 O4 69.8(3) . 1_665
O3 La1 O4 48.0(2) 1_665 1_665
O6 La1 O4 67.4(3) 2_656 1_665
OW2 La1 O4 133.4(3) . 1_665
O7 La1 O4 99.6(3) 2_656 1_665
O1 La1 C13 68.8(3) . 2_656
O2 La1 C13 101.9(3) 2_667 2_656
O4 La1 C13 103.8(3) 2_657 2_656
OW1 La1 C13 152.2(3) . 2_656
O3 La1 C13 82.5(3) 1_665 2_656
O6 La1 C13 25.3(3) 2_656 2_656
OW2 La1 C13 139.0(3) . 2_656
O7 La1 C13 24.8(3) 2_656 2_656
O4 La1 C13 84.2(3) 1_665 2_656
O1 La1 C5 152.4(3) . 1_665
O2 La1 C5 94.3(3) 2_667 1_665
O4 La1 C5 90.6(3) 2_657 1_665
OW1 La1 C5 66.6(3) . 1_665
O3 La1 C5 23.5(3) 1_665 1_665
O6 La1 C5 78.2(3) 2_656 1_665
OW2 La1 C5 135.2(3) . 1_665
O7 La1 C5 91.6(3) 2_656 1_665
O4 La1 C5 24.8(3) 1_665 1_665
C13 La1 C5 85.6(3) 2_656 1_665
C1 O1 La1 170.4(8) . .
C1 O2 La1 135.5(8) . 2_667
C5 O3 La1 102.2(7) . 1_445
C5 O4 La1 152.5(8) . 2_657
C5 O4 La1 86.9(7) . 1_445
La1 O4 La1 112.8(3) 2_657 1_445
C9 O5 C7 116.4(9) . .
C13 O6 La1 96.2(7) . 2_656
C13 O7 La1 93.9(7) . 2_656
O2 C1 O1 125.3(10) . .
O2 C1 C2 116.4(11) . .
O1 C1 C2 118.3(11) . .
C3 C2 C8 120.3(10) . .
C3 C2 C1 119.3(11) . .
C8 C2 C1 120.4(11) . .
C2 C3 C4 120.3(11) . .
C6 C4 C3 120.5(11) . .
C6 C4 C5 121.3(11) . .
C3 C4 C5 118.2(11) . .
O3 C5 O4 121.3(10) . .
O3 C5 C4 119.6(10) . .
O4 C5 C4 119.1(10) . .
O3 C5 La1 54.2(6) . 1_445
O4 C5 La1 68.3(6) . 1_445
C4 C5 La1 164.7(8) . 1_445
C7 C6 C4 118.0(11) . .
C6 C7 C8 122.9(11) . .
C6 C7 O5 119.5(11) . .
C8 C7 O5 117.5(10) . .
C7 C8 C2 117.8(11) . .
O5 C9 C15 117.0(11) . .
O5 C9 C10 122.9(11) . .
C15 C9 C10 120.1(12) . .
C11 C10 C9 119.7(12) . .
C10 C11 C12 121.9(13) . .
C14 C12 C11 118.2(12) . .
C14 C12 C13 120.2(11) . .
C11 C12 C13 121.6(12) . .
O7 C13 O6 119.7(11) . .
O7 C13 C12 121.8(11) . .
O6 C13 C12 118.5(11) . .
O7 C13 La1 61.3(6) . 2_656
O6 C13 La1 58.6(6) . 2_656
C12 C13 La1 175.5(8) . 2_656
C12 C14 C15 122.2(12) . .
C9 C15 C14 117.7(12) . .
O8 C17 C18 115(3) . .
O8 C17 C16 121(3) . .
C18 C17 C16 124(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O1 2.409(8) .
La1 O2 2.456(9) 2_667
La1 O4 2.488(8) 2_657
La1 OW1 2.550(9) .
La1 O3 2.551(9) 1_665
La1 O6 2.560(9) 2_656
La1 OW2 2.601(9) .
La1 O7 2.623(8) 2_656
La1 O4 2.860(8) 1_665
La1 C13 2.983(12) 2_656
La1 C5 3.073(12) 1_665
O1 C1 1.270(16) .
O2 C1 1.218(16) .
O2 La1 2.456(9) 2_667
O3 C5 1.255(14) .
O3 La1 2.551(9) 1_445
O4 C5 1.289(14) .
O4 La1 2.488(8) 2_657
O4 La1 2.860(8) 1_445
O5 C9 1.384(15) .
O5 C7 1.401(14) .
O6 C13 1.280(15) .
O6 La1 2.560(9) 2_656
O7 C13 1.253(15) .
O7 La1 2.623(8) 2_656
O8 C17 1.271(18) .
C1 C2 1.485(13) .
C2 C3 1.381(16) .
C2 C8 1.399(16) .
C3 C4 1.396(16) .
C4 C6 1.393(17) .
C4 C5 1.500(16) .
C5 La1 3.073(11) 1_445
C6 C7 1.374(17) .
C7 C8 1.396(17) .
C9 C15 1.388(19) .
C9 C10 1.401(18) .
C10 C11 1.358(18) .
C11 C12 1.376(18) .
C12 C14 1.372(18) .
C12 C13 1.478(17) .
C13 La1 2.983(12) 2_656
C14 C15 1.403(18) .
C16 C17 1.46(5) .
C17 C18 1.46(7) .
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
La1 O2 C1 O1 40.6(18) 2_667 .
La1 O2 C1 C2 -141.3(9) 2_667 .
O2 C1 C2 C3 -8.2(17) . .
O1 C1 C2 C3 170.0(11) . .
O2 C1 C2 C8 171.5(11) . .
O1 C1 C2 C8 -10.2(17) . .
C8 C2 C3 C4 3.1(18) . .
C1 C2 C3 C4 -177.1(10) . .
C2 C3 C4 C6 -1.3(17) . .
C2 C3 C4 C5 177.4(11) . .
La1 O3 C5 O4 14.3(12) 1_445 .
La1 O3 C5 C4 -163.3(8) 1_445 .
La1 O4 C5 O3 -150.0(12) 2_657 .
La1 O4 C5 O3 -12.4(11) 1_445 .
La1 O4 C5 C4 28(2) 2_657 .
La1 O4 C5 C4 165.1(9) 1_445 .
La1 O4 C5 La1 -137.5(16) 2_657 1_445
C6 C4 C5 O3 -142.5(12) . .
C3 C4 C5 O3 38.8(15) . .
C6 C4 C5 O4 39.9(16) . .
C3 C4 C5 O4 -138.8(11) . .
C6 C4 C5 La1 155(2) . 1_445
C3 C4 C5 La1 -23(4) . 1_445
C3 C4 C6 C7 -2.7(17) . .
C5 C4 C6 C7 178.6(11) . .
C4 C6 C7 C8 5.1(19) . .
C4 C6 C7 O5 -177.3(10) . .
C9 O5 C7 C6 58.3(15) . .
C9 O5 C7 C8 -123.9(12) . .
C6 C7 C8 C2 -3.2(19) . .
O5 C7 C8 C2 179.1(11) . .
C3 C2 C8 C7 -1.0(18) . .
C1 C2 C8 C7 179.3(11) . .
C7 O5 C9 C15 -147.4(12) . .
C7 O5 C9 C10 33.2(16) . .
O5 C9 C10 C11 -178.7(12) . .
C15 C9 C10 C11 2(2) . .
C9 C10 C11 C12 -1(2) . .
C10 C11 C12 C14 -2(2) . .
C10 C11 C12 C13 178.1(12) . .
La1 O7 C13 O6 5.3(11) 2_656 .
La1 O7 C13 C12 -176.2(10) 2_656 .
La1 O6 C13 O7 -5.4(12) 2_656 .
La1 O6 C13 C12 176.0(9) 2_656 .
C14 C12 C13 O7 4.6(19) . .
C11 C12 C13 O7 -175.3(12) . .
C14 C12 C13 O6 -176.9(12) . .
C11 C12 C13 O6 3.2(18) . .
C11 C12 C14 C15 4(2) . .
C13 C12 C14 C15 -175.5(13) . .
O5 C9 C15 C14 -178.9(12) . .
C10 C9 C15 C14 0(2) . .
C12 C14 C15 C9 -4(2) . .
