#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:54:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179546 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/15/4501540.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_4501540
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         'C20 H18 La N O11'
_chemical_formula_sum            'C20 H18 La N O11'
_chemical_formula_weight         587.26
_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                93.381(5)
_cell_angle_beta                 97.716(4)
_cell_angle_gamma                110.242(5)
_cell_formula_units_Z            2
_cell_length_a                   9.404(3)
_cell_length_b                   9.957(5)
_cell_length_c                   11.459(8)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.7
_cell_volume                     991.2(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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8842
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.7762
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.263
_refine_diff_density_min         -1.770
_refine_diff_density_rms         0.398
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_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+26.8250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                4203
_reflns_number_total             4724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100078b_si_002.cif
_cod_data_source_block           Compound1c
_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               4501540
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 0.21553(5) -0.54726(5) 0.51807(4) 0.01182(14) Uani 1 1 d .
O1 O 0.4436(7) -0.3356(6) 0.5343(5) 0.0182(12) Uani 1 1 d .
O2 O 0.6756(6) -0.2661(6) 0.4815(5) 0.0142(11) Uani 1 1 d .
O3 O 1.0407(7) 0.2452(6) 0.6157(5) 0.0166(12) Uani 1 1 d .
O4 O 0.9164(6) 0.3924(6) 0.5757(5) 0.0123(11) Uani 1 1 d .
O5 O 0.4415(6) 0.1045(6) 0.7744(5) 0.0151(11) Uani 1 1 d .
O6 O 0.7879(7) 0.3899(7) 1.2976(5) 0.0180(12) Uani 1 1 d .
O7 O 0.6212(7) 0.5005(6) 1.2679(5) 0.0173(12) Uani 1 1 d .
N1 N 0.965(5) 0.902(7) 0.994(4) 0.49(6) Uiso 1 1 d D
C1 C 0.5717(9) -0.2432(9) 0.5312(7) 0.0151(15) Uiso 1 1 d .
C2 C 0.6098(8) -0.0924(8) 0.5906(7) 0.0113(14) Uani 1 1 d .
C3 C 0.5080(8) -0.0614(8) 0.6569(7) 0.0120(14) Uani 1 1 d .
H3 H 0.4173 -0.1334 0.6666 0.014 Uiso 1 1 calc R
C4 C 0.5447(9) 0.0777(9) 0.7074(7) 0.0137(15) Uani 1 1 d .
C5 C 0.6731(9) 0.1886(8) 0.6900(7) 0.0130(15) Uani 1 1 d .
H5 H 0.6921 0.2827 0.7213 0.016 Uiso 1 1 calc R
C6 C 0.7762(9) 0.1567(8) 0.6232(7) 0.0122(15) Uani 1 1 d .
C7 C 0.9196(9) 0.2713(9) 0.6038(7) 0.0140(15) Uani 1 1 d .
C8 C 0.7452(8) 0.0173(8) 0.5760(7) 0.0110(14) Uani 1 1 d .
H8 H 0.8144 -0.0041 0.5343 0.013 Uiso 1 1 calc R
C9 C 0.5044(9) 0.1778(8) 0.8877(7) 0.0133(15) Uani 1 1 d .
C10 C 0.4354(10) 0.2680(9) 0.9293(7) 0.0162(16) Uani 1 1 d .
H10 H 0.3544 0.2814 0.8816 0.019 Uiso 1 1 calc R
C11 C 0.4894(10) 0.3400(10) 1.0456(8) 0.0197(17) Uani 1 1 d .
H11 H 0.4404 0.3976 1.0759 0.024 Uiso 1 1 calc R
C12 C 0.6139(9) 0.3254(8) 1.1143(7) 0.0132(15) Uani 1 1 d .
C13 C 0.6778(9) 0.4101(9) 1.2337(7) 0.0143(15) Uani 1 1 d .
C14 C 0.6795(10) 0.2293(9) 1.0710(7) 0.0164(16) Uani 1 1 d .
H14 H 0.7603 0.2152 1.1183 0.020 Uiso 1 1 calc R
C15 C 0.6237(10) 0.1544(9) 0.9565(7) 0.0181(16) Uani 1 1 d .
H15 H 0.6665 0.0904 0.9279 0.022 Uiso 1 1 calc R
C16 C 0.889(4) 0.833(4) 0.881(4) 0.190(16) Uiso 1 1 d D
H16 H 0.8650 0.8783 0.8159 0.228 Uiso 1 1 calc R
C17 C 0.856(3) 0.690(4) 0.882(3) 0.150(12) Uiso 1 1 d D
H17 H 0.8060 0.6321 0.8114 0.180 Uiso 1 1 calc R
C18 C 0.890(2) 0.618(3) 0.9783(18) 0.098(7) Uani 1 1 d D
H18 H 0.8605 0.5186 0.9636 0.117 Uiso 1 1 calc R
C19 C 0.959(3) 0.676(3) 1.087(2) 0.139(11) Uiso 1 1 d D
H19 H 0.9793 0.6287 1.1511 0.167 Uiso 1 1 calc R
C20 C 0.995(5) 0.829(4) 1.086(6) 0.30(3) Uiso 1 1 d D
H20 H 1.0448 0.8855 1.1572 0.363 Uiso 1 1 calc R
OW1 O 0.0093(7) -0.7198(7) 0.3545(6) 0.0193(13) Uani 1 1 d D
OW2 O 0.3139(7) -0.5429(8) 0.3163(6) 0.0221(13) Uani 1 1 d D
OW3 O 0.1114(8) 0.0127(7) 0.6956(7) 0.0271(15) Uani 1 1 d D
OW4 O 1.042(4) 0.510(3) 1.105(3) 0.251(14) Uiso 1 1 d D
H1W1 H -0.056(8) -0.690(9) 0.309(6) 0.01(2) Uiso 1 1 d D
H1W3 H 0.213(4) 0.059(14) 0.717(13) 0.06(4) Uiso 1 1 d D
H2W3 H 0.084(18) 0.089(11) 0.681(14) 0.07(5) Uiso 1 1 d D
H1W2 H 0.413(5) -0.523(15) 0.310(13) 0.03(4) Uiso 1 1 d D
H2W2 H 0.28(2) -0.49(4) 0.26(3) 0.04(3) Uiso 1 1 d D
H2W1 H -0.021(15) -0.816(2) 0.339(12) 0.03(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'
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'
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(2) . 2_646
O1 La1 O4 84.2(2) . 2_656
O2 La1 O4 154.93(19) 2_646 2_656
O1 La1 OW1 138.2(2) . .
O2 La1 OW1 84.3(2) 2_646 .
O4 La1 OW1 76.08(19) 2_656 .
O1 La1 O6 75.0(2) . 2_657
O2 La1 O6 125.23(19) 2_646 2_657
O4 La1 O6 79.84(19) 2_656 2_657
OW1 La1 O6 134.7(2) . 2_657
O1 La1 O3 149.4(2) . 1_445
O2 La1 O3 73.09(19) 2_646 1_445
O4 La1 O3 114.24(18) 2_656 1_445
OW1 La1 O3 72.0(2) . 1_445
O6 La1 O3 84.17(19) 2_657 1_445
O1 La1 OW2 72.6(2) . .
O2 La1 OW2 76.2(2) 2_646 .
O4 La1 OW2 82.1(2) 2_656 .
OW1 La1 OW2 68.5(2) . .
O6 La1 OW2 144.2(2) 2_657 .
O3 La1 OW2 131.6(2) 1_445 .
O1 La1 O7 69.6(2) . 2_657
O2 La1 O7 76.61(19) 2_646 2_657
O4 La1 O7 127.50(18) 2_656 2_657
OW1 La1 O7 149.58(19) . 2_657
O6 La1 O7 50.25(18) 2_657 2_657
O3 La1 O7 79.83(19) 1_445 2_657
OW2 La1 O7 127.5(2) . 2_657
O1 La1 O4 135.40(19) . 1_445
O2 La1 O4 119.46(17) 2_646 1_445
O4 La1 O4 67.62(19) 2_656 1_445
OW1 La1 O4 68.76(19) . 1_445
O6 La1 O4 66.76(17) 2_657 1_445
O3 La1 O4 47.61(17) 1_445 1_445
OW2 La1 O4 132.12(19) . 1_445
O7 La1 O4 100.35(18) 2_657 1_445
O1 La1 C13 68.6(2) . 2_657
O2 La1 C13 101.4(2) 2_646 2_657
O4 La1 C13 103.3(2) 2_656 2_657
OW1 La1 C13 151.5(2) . 2_657
O6 La1 C13 25.2(2) 2_657 2_657
O3 La1 C13 82.9(2) 1_445 2_657
OW2 La1 C13 140.0(2) . 2_657
O7 La1 C13 25.2(2) 2_657 2_657
O4 La1 C13 84.51(19) 1_445 2_657
O1 La1 C7 152.2(2) . 1_445
O2 La1 C7 95.13(19) 2_646 1_445
O4 La1 C7 90.90(19) 2_656 1_445
OW1 La1 C7 65.6(2) . 1_445
O6 La1 C7 77.2(2) 2_657 1_445
O3 La1 C7 23.43(19) 1_445 1_445
OW2 La1 C7 133.9(2) . 1_445
O7 La1 C7 92.5(2) 2_657 1_445
O4 La1 C7 24.51(18) 1_445 1_445
C13 La1 C7 86.0(2) 2_657 1_445
C1 O1 La1 168.0(6) . .
C1 O2 La1 134.4(5) . 2_646
C7 O3 La1 101.2(5) . 1_665
C7 O4 La1 152.5(5) . 2_656
C7 O4 La1 87.8(5) . 1_665
La1 O4 La1 112.38(19) 2_656 1_665
C9 O5 C4 116.2(6) . .
C13 O6 La1 95.3(5) . 2_657
C13 O7 La1 92.1(5) . 2_657
C20 N1 C16 123(7) . .
C20 N1 N1 122(5) . 2_777
C16 N1 N1 114(5) . 2_777
O1 C1 O2 124.6(8) . .
O1 C1 C2 118.8(7) . .
O2 C1 C2 116.6(7) . .
C8 C2 C3 120.0(7) . .
C8 C2 C1 119.7(7) . .
C3 C2 C1 120.3(7) . .
C4 C3 C2 118.7(7) . .
C5 C4 C3 122.4(7) . .
C5 C4 O5 120.3(7) . .
C3 C4 O5 117.2(7) . .
C4 C5 C6 118.6(7) . .
C8 C6 C5 120.0(7) . .
C8 C6 C7 118.8(7) . .
C5 C6 C7 121.2(7) . .
O3 C7 O4 121.7(8) . .
O3 C7 C6 118.2(7) . .
O4 C7 C6 120.1(7) . .
O3 C7 La1 55.4(4) . 1_665
O4 C7 La1 67.7(4) . 1_665
C6 C7 La1 166.2(5) . 1_665
C6 C8 C2 120.2(7) . .
C10 C9 C15 121.9(8) . .
C10 C9 O5 116.5(7) . .
C15 C9 O5 121.5(7) . .
C9 C10 C11 119.1(8) . .
C12 C11 C10 120.6(8) . .
C11 C12 C14 119.1(7) . .
C11 C12 C13 120.4(7) . .
C14 C12 C13 120.5(7) . .
O7 C13 O6 121.8(8) . .
O7 C13 C12 119.1(7) . .
O6 C13 C12 119.1(7) . .
O7 C13 La1 62.7(4) . 2_657
O6 C13 La1 59.5(4) . 2_657
C12 C13 La1 173.4(5) . 2_657
C12 C14 C15 120.5(7) . .
C9 C15 C14 118.7(8) . .
C17 C16 N1 108(5) . .
C16 C17 C18 128(4) . .
C19 C18 C17 127(3) . .
C19 C18 OW4 120.4(19) . 2_767
C17 C18 OW4 97.6(18) . 2_767
C18 C19 C20 105(4) . .
N1 C20 C19 129(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O1 2.407(6) .
La1 O2 2.412(6) 2_646
La1 O4 2.496(6) 2_656
La1 OW1 2.562(6) .
La1 O6 2.566(6) 2_657
La1 O3 2.577(6) 1_445
La1 OW2 2.601(6) .
La1 O7 2.636(6) 2_657
La1 O4 2.844(5) 1_445
La1 C13 2.964(8) 2_657
La1 C7 3.072(9) 1_445
O1 C1 1.244(10) .
O2 C1 1.272(10) .
O2 La1 2.412(6) 2_646
O3 C7 1.245(9) .
O3 La1 2.577(6) 1_665
O4 C7 1.275(9) .
O4 La1 2.496(6) 2_656
O4 La1 2.844(5) 1_665
O5 C9 1.397(9) .
O5 C4 1.398(9) .
O6 C13 1.268(10) .
O6 La1 2.566(6) 2_657
O7 C13 1.262(10) .
O7 La1 2.636(6) 2_657
N1 C20 1.37(8) .
N1 C16 1.40(7) .
N1 N1 1.83(13) 2_777
C1 C2 1.513(11) .
C2 C8 1.399(10) .
C2 C3 1.402(10) .
C3 C4 1.376(11) .
C4 C5 1.373(11) .
C5 C6 1.417(11) .
C6 C8 1.376(11) .
C6 C7 1.489(12) .
C7 La1 3.072(9) 1_665
C9 C10 1.375(11) .
C9 C15 1.378(12) .
C10 C11 1.415(11) .
C11 C12 1.376(12) .
C12 C14 1.406(11) .
C12 C13 1.496(11) .
C13 La1 2.964(8) 2_657
C14 C15 1.408(10) .
C16 C17 1.35(5) .
C17 C18 1.41(4) .
C18 C19 1.32(3) .
C18 OW4 1.88(4) 2_767
C19 C20 1.44(5) .
OW4 C18 1.88(4) 2_767
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 31(3) 2_646 .
O4 La1 O1 C1 -125(3) 2_656 .
OW1 La1 O1 C1 -63(3) . .
O6 La1 O1 C1 154(3) 2_657 .
O3 La1 O1 C1 106(3) 1_445 .
OW2 La1 O1 C1 -41(3) . .
O7 La1 O1 C1 102(3) 2_657 .
O4 La1 O1 C1 -174(3) 1_445 .
C13 La1 O1 C1 129(3) 2_657 .
C7 La1 O1 C1 155(3) 1_445 .
La1 O1 C1 O2 1(3) . .
La1 O1 C1 C2 -178(2) . .
La1 O2 C1 O1 -46.4(12) 2_646 .
La1 O2 C1 C2 133.3(6) 2_646 .
O1 C1 C2 C8 -172.3(7) . .
O2 C1 C2 C8 8.1(11) . .
O1 C1 C2 C3 5.7(11) . .
O2 C1 C2 C3 -173.9(7) . .
C8 C2 C3 C4 -0.5(11) . .
C1 C2 C3 C4 -178.5(7) . .
C2 C3 C4 C5 3.6(12) . .
C2 C3 C4 O5 -179.1(7) . .
C9 O5 C4 C5 -53.4(10) . .
C9 O5 C4 C3 129.3(8) . .
C3 C4 C5 C6 -3.8(12) . .
O5 C4 C5 C6 179.0(7) . .
C4 C5 C6 C8 1.0(11) . .
C4 C5 C6 C7 -178.4(7) . .
La1 O3 C7 O4 -14.3(9) 1_665 .
La1 O3 C7 C6 165.7(6) 1_665 .
La1 O4 C7 O3 151.3(8) 2_656 .
La1 O4 C7 O3 12.7(8) 1_665 .
La1 O4 C7 C6 -28.6(16) 2_656 .
La1 O4 C7 C6 -167.3(7) 1_665 .
La1 O4 C7 La1 138.7(11) 2_656 1_665
C8 C6 C7 O3 -43.6(11) . .
C5 C6 C7 O3 135.7(8) . .
C8 C6 C7 O4 136.3(8) . .
C5 C6 C7 O4 -44.3(11) . .
C8 C6 C7 La1 15(3) . 1_665
C5 C6 C7 La1 -165.6(18) . 1_665
C5 C6 C8 C2 2.0(11) . .
C7 C6 C8 C2 -178.7(7) . .
C3 C2 C8 C6 -2.2(11) . .
C1 C2 C8 C6 175.8(7) . .
C4 O5 C9 C10 147.2(7) . .
C4 O5 C9 C15 -36.4(10) . .
C15 C9 C10 C11 0.7(13) . .
O5 C9 C10 C11 177.1(7) . .
C9 C10 C11 C12 3.0(13) . .
C10 C11 C12 C14 -4.9(13) . .
C10 C11 C12 C13 175.5(8) . .
La1 O7 C13 O6 -7.7(8) 2_657 .
La1 O7 C13 C12 172.7(6) 2_657 .
La1 O6 C13 O7 8.0(8) 2_657 .
La1 O6 C13 C12 -172.5(6) 2_657 .
C11 C12 C13 O7 -3.7(11) . .
C14 C12 C13 O7 176.7(8) . .
C11 C12 C13 O6 176.8(8) . .
C14 C12 C13 O6 -2.9(11) . .
C11 C12 C14 C15 3.2(13) . .
C13 C12 C14 C15 -177.2(8) . .
C10 C9 C15 C14 -2.3(13) . .
O5 C9 C15 C14 -178.5(7) . .
C12 C14 C15 C9 0.4(13) . .
C20 N1 C16 C17 -1(2) . .
N1 N1 C16 C17 174(4) 2_777 .
N1 C16 C17 C18 0(2) . .
C16 C17 C18 C19 1(2) . .
C16 C17 C18 OW4 -137(2) . 2_767
C17 C18 C19 C20 -1(2) . .
OW4 C18 C19 C20 129(2) 2_767 .
C16 N1 C20 C19 1(3) . .
N1 N1 C20 C19 -174(4) 2_777 .
C18 C19 C20 N1 1(2) . .
