#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:54:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179546 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/15/4501537.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_4501537
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         'C15 H13 La O13'
_chemical_formula_sum            'C15 H13 La O13'
_chemical_formula_weight         540.16
_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                92.979(6)
_cell_angle_beta                 97.836(5)
_cell_angle_gamma                110.330(3)
_cell_formula_units_Z            2
_cell_length_a                   9.376(5)
_cell_length_b                   9.940(4)
_cell_length_c                   11.377(7)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.20
_cell_volume                     979.3(9)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6235
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_T_max  0.7743
_exptl_absorpt_correction_T_min  0.6878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.793
_refine_diff_density_rms         0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4584
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0644
_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)+(0.0000P)²+26.6999P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                3680
_reflns_number_total             4584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100078b_si_002.cif
_cod_data_source_block           Compound1
_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               4501537
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 0.28444(7) 0.04771(6) -0.01678(6) 0.01975(17) Uani 1 1 d D
O1 O 0.0593(7) -0.1642(7) -0.0311(6) 0.0222(15) Uani 1 1 d .
O2 O -0.1776(7) -0.2352(7) 0.0175(7) 0.0221(15) Uani 1 1 d .
O3 O -0.5449(8) -0.7475(7) -0.1182(7) 0.0233(15) Uani 1 1 d .
O4 O -0.4179(8) -0.8936(7) -0.0786(6) 0.0215(14) Uiso 1 1 d .
O5 O 0.0608(7) -0.6034(7) -0.2741(6) 0.0208(14) Uani 1 1 d .
O6 O -0.2854(8) -0.8958(9) -0.7963(6) 0.0282(16) Uani 1 1 d .
O7 O -0.1140(8) -0.9988(7) -0.7707(7) 0.0266(16) Uani 1 1 d .
C1 C -0.0743(12) -0.2595(10) -0.0299(9) 0.024(2) Uani 1 1 d .
C2 C -0.1070(11) -0.4068(10) -0.0887(9) 0.0198(19) Uani 1 1 d .
C3 C -0.2458(11) -0.5189(10) -0.0797(9) 0.0191(18) Uani 1 1 d .
H3 H -0.3173 -0.4979 -0.0401 0.023 Uiso 1 1 calc R
C4 C -0.2785(10) -0.6570(10) -0.1270(9) 0.0207(19) Uani 1 1 d .
C5 C -0.4230(11) -0.7722(9) -0.1063(9) 0.0198(19) Uani 1 1 d .
C6 C -0.1741(12) -0.6886(11) -0.1911(9) 0.025(2) Uani 1 1 d .
H6 H -0.1922 -0.7827 -0.2219 0.030 Uiso 1 1 calc R
C7 C -0.0435(11) -0.5761(10) -0.2071(8) 0.0186(18) Uani 1 1 d .
C8 C -0.0056(11) -0.4369(10) -0.1546(9) 0.022(2) Uani 1 1 d .
H8 H 0.0862 -0.3649 -0.1632 0.027 Uiso 1 1 calc R
C9 C -0.0006(11) -0.6769(10) -0.3888(8) 0.0172(18) Uani 1 1 d .
C10 C -0.1240(11) -0.6579(10) -0.4578(9) 0.023(2) Uani 1 1 d .
H10 H -0.1700 -0.5966 -0.4290 0.028 Uiso 1 1 calc R
C11 C -0.1777(13) -0.7323(11) -0.5710(10) 0.028(2) Uani 1 1 d .
H11 H -0.2612 -0.7220 -0.6189 0.034 Uiso 1 1 calc R
C12 C -0.1055(11) -0.8230(11) -0.6130(9) 0.022(2) Uani 1 1 d .
C13 C -0.1712(12) -0.9087(10) -0.7326(9) 0.023(2) Uani 1 1 d .
C14 C 0.0206(13) -0.8358(11) -0.5442(9) 0.026(2) Uani 1 1 d .
H14 H 0.0697 -0.8939 -0.5737 0.031 Uiso 1 1 calc R
C15 C 0.0746(12) -0.7620(11) -0.4311(10) 0.027(2) Uani 1 1 d .
H15 H 0.1602 -0.7697 -0.3842 0.032 Uiso 1 1 calc R
OW1 O 0.4946(9) 0.2204(8) 0.1471(7) 0.0290(17) Uani 1 1 d D
OW2 O 0.1891(9) 0.0471(9) 0.1883(8) 0.0331(18) Uani 1 1 d D
OW3 O -0.6085(9) -0.5159(9) -0.2031(8) 0.0326(18) Uani 1 1 d D
OW4 O 0.384(3) 0.145(4) 0.4265(19) 0.27(2) Uani 1 1 d D
OW5 O 0.501(3) 0.067(4) 0.616(2) 0.31(3) Uani 1 1 d .
OW6 O 0.438(7) 0.450(5) 0.384(4) 0.55(5) Uani 1 1 d D
H1W1 H 0.55(2) 0.18(2) 0.186(18) 0.05(9) Uiso 1 1 d D
H2W1 H 0.517(17) 0.316(3) 0.154(13) 0.06(5) Uiso 1 1 d D
H1W2 H 0.263(9) 0.10(3) 0.250(6) 0.05(18) Uiso 1 1 d D
H2W2 H 0.090(5) 0.031(14) 0.192(12) 0.04(4) Uiso 1 1 d D
H2W3 H -0.591(14) -0.589(9) -0.168(9) 0.03(3) Uiso 1 1 d D
H1W3 H -0.712(3) -0.545(15) -0.211(13) 0.05(4) 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 101.9(2) . 2
O1 La1 O4 83.8(2) . 2_545
O2 La1 O4 154.6(2) 2 2_545
O1 La1 O6 75.2(2) . 2_544
O2 La1 O6 124.0(2) 2 2_544
O4 La1 O6 81.3(2) 2_545 2_544
O1 La1 O3 148.9(2) . 1_665
O2 La1 O3 72.6(2) 2 1_665
O4 La1 O3 114.6(2) 2_545 1_665
O6 La1 O3 82.7(2) 2_544 1_665
O1 La1 OW1 138.2(3) . .
O2 La1 OW1 84.4(2) 2 .
O4 La1 OW1 75.5(2) 2_545 .
O6 La1 OW1 134.7(2) 2_544 .
O3 La1 OW1 72.7(2) 1_665 .
O1 La1 OW2 73.5(2) . .
O2 La1 OW2 75.9(3) 2 .
O4 La1 OW2 82.3(2) 2_545 .
O6 La1 OW2 146.0(3) 2_544 .
O3 La1 OW2 131.3(2) 1_665 .
OW1 La1 OW2 68.1(3) . .
O1 La1 O7 68.9(2) . 2_544
O2 La1 O7 76.4(2) 2 2_544
O4 La1 O7 127.9(2) 2_545 2_544
O6 La1 O7 49.8(2) 2_544 2_544
O3 La1 O7 80.2(2) 1_665 2_544
OW1 La1 O7 150.4(2) . 2_544
OW2 La1 O7 126.6(2) . 2_544
O1 La1 O4 134.4(2) . 1_665
O2 La1 O4 119.2(2) 2 1_665
O4 La1 O4 67.7(2) 2_545 1_665
O6 La1 O4 66.2(2) 2_544 1_665
O3 La1 O4 47.8(2) 1_665 1_665
OW1 La1 O4 69.1(2) . 1_665
OW2 La1 O4 132.4(2) . 1_665
O7 La1 O4 101.0(2) 2_544 1_665
O1 La1 C13 68.1(2) . 2_544
O2 La1 C13 101.2(3) 2 2_544
O4 La1 C13 103.8(3) 2_545 2_544
O6 La1 C13 24.7(2) 2_544 2_544
O3 La1 C13 82.7(2) 1_665 2_544
OW1 La1 C13 151.9(3) . 2_544
OW2 La1 C13 140.0(3) . 2_544
O7 La1 C13 25.3(2) 2_544 2_544
O4 La1 C13 84.5(2) 1_665 2_544
O1 La1 C5 151.6(2) . 1_665
O2 La1 C5 94.6(2) 2 1_665
O4 La1 C5 91.1(2) 2_545 1_665
O6 La1 C5 76.3(2) 2_544 1_665
O3 La1 C5 23.5(2) 1_665 1_665
OW1 La1 C5 65.9(3) . 1_665
OW2 La1 C5 133.6(3) . 1_665
O7 La1 C5 93.2(2) 2_544 1_665
O4 La1 C5 24.7(2) 1_665 1_665
C13 La1 C5 86.2(3) 2_544 1_665
C1 O1 La1 167.8(7) . .
C1 O2 La1 135.3(6) . 2
C5 O3 La1 101.3(6) . 1_445
C5 O4 La1 152.7(6) . 2_545
C5 O4 La1 86.9(5) . 1_445
La1 O4 La1 112.3(2) 2_545 1_445
C9 O5 C7 116.8(7) . .
C13 O6 La1 97.6(6) . 2_544
C13 O7 La1 93.1(6) . 2_544
O2 C1 O1 123.8(9) . .
O2 C1 C2 118.8(9) . .
O1 C1 C2 117.4(9) . .
C8 C2 C3 118.6(9) . .
C8 C2 C1 121.8(9) . .
C3 C2 C1 119.6(9) . .
C4 C3 C2 122.1(9) . .
C3 C4 C6 119.4(9) . .
C3 C4 C5 119.0(9) . .
C6 C4 C5 121.6(9) . .
O3 C5 O4 122.0(8) . .
O3 C5 C4 118.9(8) . .
O4 C5 C4 119.2(8) . .
O3 C5 La1 55.2(5) . 1_445
O4 C5 La1 68.4(5) . 1_445
C4 C5 La1 166.1(6) . 1_445
C7 C6 C4 118.2(9) . .
C8 C7 C6 122.8(9) . .
C8 C7 O5 117.5(8) . .
C6 C7 O5 119.6(8) . .
C7 C8 C2 118.7(9) . .
C10 C9 C15 122.1(9) . .
C10 C9 O5 121.5(8) . .
C15 C9 O5 116.4(9) . .
C9 C10 C11 118.5(9) . .
C10 C11 C12 119.7(10) . .
C14 C12 C11 120.6(10) . .
C14 C12 C13 120.7(9) . .
C11 C12 C13 118.7(9) . .
O6 C13 O7 118.7(9) . .
O6 C13 C12 120.8(9) . .
O7 C13 C12 120.5(10) . .
O6 C13 La1 57.7(5) . 2_544
O7 C13 La1 61.6(5) . 2_544
C12 C13 La1 173.3(7) . 2_544
C12 C14 C15 120.0(10) . .
C9 C15 C14 119.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O1 2.388(6) .
La1 O2 2.403(7) 2
La1 O4 2.495(7) 2_545
La1 O6 2.546(7) 2_544
La1 O3 2.554(7) 1_665
La1 OW1 2.573(8) .
La1 OW2 2.609(8) .
La1 O7 2.630(8) 2_544
La1 O4 2.840(7) 1_665
La1 C13 2.985(10) 2_544
La1 C5 3.050(10) 1_665
O1 C1 1.283(11) .
O2 C1 1.256(12) .
O2 La1 2.403(7) 2
O3 C5 1.241(12) .
O3 La1 2.554(7) 1_445
O4 C5 1.278(11) .
O4 La1 2.495(7) 2_545
O4 La1 2.840(7) 1_445
O5 C9 1.404(11) .
O5 C7 1.406(11) .
O6 C13 1.258(13) .
O6 La1 2.546(7) 2_544
O7 C13 1.278(11) .
O7 La1 2.630(8) 2_544
C1 C2 1.489(13) .
C2 C8 1.387(13) .
C2 C3 1.409(13) .
C3 C4 1.362(13) .
C4 C6 1.404(14) .
C4 C5 1.497(13) .
C5 La1 3.050(10) 1_445
C6 C7 1.384(14) .
C7 C8 1.382(13) .
C9 C10 1.382(14) .
C9 C15 1.382(13) .
C10 C11 1.387(14) .
C11 C12 1.403(14) .
C12 C14 1.374(15) .
C12 C13 1.498(14) .
C13 La1 2.985(10) 2_544
C14 C15 1.384(15) .
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
O2 La1 O1 C1 -22(3) 2 .
O4 La1 O1 C1 133(3) 2_545 .
O6 La1 O1 C1 -145(3) 2_544 .
O3 La1 O1 C1 -98(3) 1_665 .
OW1 La1 O1 C1 73(3) . .
OW2 La1 O1 C1 49(3) . .
O7 La1 O1 C1 -92(3) 2_544 .
O4 La1 O1 C1 -177(3) 1_665 .
C13 La1 O1 C1 -120(3) 2_544 .
C5 La1 O1 C1 -146(3) 1_665 .
La1 O2 C1 O1 45.9(15) 2 .
La1 O2 C1 C2 -133.9(8) 2 .
La1 O1 C1 O2 -9(4) . .
La1 O1 C1 C2 171(3) . .
O2 C1 C2 C8 172.4(9) . .
O1 C1 C2 C8 -7.5(14) . .
O2 C1 C2 C3 -6.4(14) . .
O1 C1 C2 C3 173.7(9) . .
C8 C2 C3 C4 4.2(15) . .
C1 C2 C3 C4 -176.9(9) . .
C2 C3 C4 C6 -2.6(15) . .
C2 C3 C4 C5 175.6(9) . .
La1 O3 C5 O4 15.8(10) 1_445 .
La1 O3 C5 C4 -165.2(7) 1_445 .
La1 O4 C5 O3 -150.0(10) 2_545 .
La1 O4 C5 O3 -13.9(9) 1_445 .
La1 O4 C5 C4 31.0(19) 2_545 .
La1 O4 C5 C4 167.1(8) 1_445 .
La1 O4 C5 La1 -136.1(13) 2_545 1_445
C3 C4 C5 O3 44.7(14) . .
C6 C4 C5 O3 -137.1(10) . .
C3 C4 C5 O4 -136.3(9) . .
C6 C4 C5 O4 41.9(14) . .
C3 C4 C5 La1 -16(3) . 1_445
C6 C4 C5 La1 162(2) . 1_445
C3 C4 C6 C7 -2.2(15) . .
C5 C4 C6 C7 179.6(9) . .
C4 C6 C7 C8 5.6(15) . .
C4 C6 C7 O5 -178.0(8) . .
C9 O5 C7 C8 -130.5(9) . .
C9 O5 C7 C6 52.9(12) . .
C6 C7 C8 C2 -3.9(15) . .
O5 C7 C8 C2 179.6(8) . .
C3 C2 C8 C7 -1.0(14) . .
C1 C2 C8 C7 -179.8(9) . .
C7 O5 C9 C10 33.5(12) . .
C7 O5 C9 C15 -150.2(9) . .
C15 C9 C10 C11 3.0(15) . .
O5 C9 C10 C11 179.1(9) . .
C9 C10 C11 C12 -0.6(15) . .
C10 C11 C12 C14 -1.8(15) . .
C10 C11 C12 C13 176.5(9) . .
La1 O6 C13 O7 -9.1(10) 2_544 .
La1 O6 C13 C12 172.4(8) 2_544 .
La1 O7 C13 O6 8.7(9) 2_544 .
La1 O7 C13 C12 -172.7(8) 2_544 .
C14 C12 C13 O6 -179.1(9) . .
C11 C12 C13 O6 2.6(14) . .
C14 C12 C13 O7 2.4(14) . .
C11 C12 C13 O7 -175.9(9) . .
C11 C12 C14 C15 2.0(15) . .
C13 C12 C14 C15 -176.4(9) . .
C10 C9 C15 C14 -2.9(15) . .
O5 C9 C15 C14 -179.2(9) . .
C12 C14 C15 C9 0.4(15) . .
