#------------------------------------------------------------------------------
#$Date: 2019-10-28 05:20:03 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219691 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/45/4514506.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_4514506
loop_
_publ_author_name
'Han, Lin'
'Pham, Tony'
'Zhuo, Mingjing'
'Forrest, Katherine A.'
'Suepaul, Shanelle'
'Space, Brian'
'Zaworotko, Michael J.'
'Shi, Wei'
'Chen, Yao'
'Cheng, Peng'
'Zhang, Zhenjie'
_publ_section_title
;
 Molecular Sieving and Direct Visualization of CO₂ in Binding
 Pockets of an Ultramicroporous Lanthanide Metal-Organic Framework
 Platform.
;
_journal_issue                   26
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              23192
_journal_page_last               23197
_journal_paper_doi               10.1021/acsami.9b04619
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'C12 H8 La N3 O9, 0.75(C O2)'
_chemical_formula_sum            'C12.75 H8 La N3 O10.5'
_chemical_formula_weight         510.13
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.145(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3671(6)
_cell_length_b                   17.2965(6)
_cell_length_c                   11.4073(6)
_cell_measurement_reflns_used    2050
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.9860
_cell_measurement_theta_min      3.4760
_cell_volume                     1920.36(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7359
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77261
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'clear light cube'
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0557
_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)+(0.0410P)²+13.2040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                2577
_reflns_number_total             3910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am9b04619_si_005.cif
_cod_data_source_block           CO2@NKMOF-3-La
_cod_original_cell_volume        1920.35(16)
_cod_original_formula_sum        'C12.75 H8 La N3 O10.50'
_cod_database_code               4514506
_olex2_refinement_description
;
1. Others
 Fixed Sof: O10(0.75) C13(0.75) O11(0.75)
 Fixed Uiso: H7(0.04) H1(0.029) H2(0.037) H5(0.033) H6(0.029) H8(0.034)
 H12(0.029) H11(0.03)
 Fixed X: H7(1.1548) H1(1.3292) H2(1.5645) H5(1.5202) H6(1.2852) H8(1.1007)
 H12(0.939) H11(0.8899)
 Fixed Y: H7(-0.1941) H1(0.1309) H2(0.1138) H5(0.0189) H6(0.0329) H8(-0.3136)
 H12(-0.0921) H11(-0.289)
 Fixed Z: H7(0.268) H1(0.4838) H2(0.5468) H5(0.2176) H6(0.1587) H8(0.1763)
 H12(-0.0484) H11(0.3531)
;
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
La1 La 0.98352(4) -0.00202(3) 0.31243(4) 0.02044(16) Uani 1 1 d .
O5 O 1.1511(5) 0.0899(3) 0.2828(5) 0.0240(12) Uani 1 1 d .
O6 O 1.2141(5) -0.0519(3) 0.4546(5) 0.0264(13) Uani 1 1 d .
N3 N 1.2876(7) 0.0818(4) 0.3180(6) 0.0217(15) Uani 1 1 d .
N2 N 1.0509(7) -0.1335(4) 0.1163(6) 0.0243(15) Uani 1 1 d .
O8 O 1.0334(5) 0.0872(3) 0.4933(5) 0.0232(13) Uani 1 1 d .
O9 O 0.9251(6) -0.1450(3) 0.3250(5) 0.0307(14) Uani 1 1 d .
C7 C 1.0998(10) -0.1982(5) 0.1845(8) 0.033(2) Uani 1 1 d .
H7 H 1.1548 -0.1941 0.2680 0.040 Uiso 1 1 calc R
C1 C 1.3681(8) 0.1069(5) 0.4310(7) 0.0240(18) Uani 1 1 d .
H1 H 1.3292 0.1309 0.4838 0.029 Uiso 1 1 calc R
O7 O 0.7657(6) 0.0274(4) 0.3471(5) 0.0340(15) Uani 1 1 d .
C2 C 1.5085(9) 0.0970(5) 0.4683(8) 0.030(2) Uani 1 1 d .
H2 H 1.5645 0.1138 0.5468 0.037 Uiso 1 1 calc R
C5 C 1.4823(8) 0.0402(5) 0.2733(8) 0.0275(19) Uani 1 1 d .
H5 H 1.5202 0.0189 0.2176 0.033 Uiso 1 1 calc R
C10 C 0.9562(8) -0.1476(4) 0.4413(7) 0.0207(16) Uani 1 1 d .
C9 C 0.9862(8) -0.2250(5) 0.5049(8) 0.0232(17) Uani 1 1 d .
O1 O 0.8468(6) 0.0987(4) 0.1485(6) 0.0337(15) Uani 1 1 d .
C3 C 1.5663(8) 0.0620(5) 0.3886(7) 0.0224(18) Uani 1 1 d .
C4 C 1.7178(9) 0.0471(5) 0.4311(8) 0.0268(19) Uani 1 1 d .
O2 O 0.7804(8) -0.0231(5) 0.1011(7) 0.055(2) Uani 1 1 d .
C6 C 1.3419(8) 0.0491(5) 0.2373(7) 0.0241(18) Uani 1 1 d .
H6 H 1.2852 0.0329 0.1587 0.029 Uiso 1 1 calc R
O4 O 1.0843(6) -0.0640(3) 0.1696(5) 0.0286(13) Uani 1 1 d .
C8 C 1.0678(9) -0.2691(5) 0.1298(8) 0.0282(19) Uani 1 1 d .
H8 H 1.1007 -0.3136 0.1763 0.034 Uiso 1 1 calc R
O3 O 0.6608(8) 0.0720(5) -0.0079(7) 0.075(3) Uani 1 1 d .
C12 C 0.9725(8) -0.1372(5) -0.0039(7) 0.0239(19) Uani 1 1 d .
H12 H 0.9390 -0.0921 -0.0484 0.029 Uiso 1 1 calc R
C11 C 0.9413(8) -0.2917(5) 0.4378(7) 0.0247(18) Uani 1 1 d .
H11 H 0.8899 -0.2890 0.3531 0.030 Uiso 1 1 calc R
N1 N 0.7613(10) 0.0514(7) 0.0783(8) 0.054(3) Uani 1 1 d .
O10 O 0.4014(15) 0.1455(9) 0.7614(18) 0.114(6) Uani 0.75 1 d P
C13 C 0.396(3) 0.1727(15) 0.842(3) 0.144(15) Uani 0.75 1 d P
O11 O 0.364(2) 0.1908(9) 0.934(2) 0.146(8) Uani 0.75 1 d P
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'
La La -0.2871 2.4523 '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
O5 La1 La1 108.49(13) . 3_756
O5 La1 O6 75.69(18) . .
O5 La1 O8 75.99(18) . .
O5 La1 O8 135.13(17) . 3_756
O5 La1 O9 145.34(19) . .
O5 La1 O7 127.91(19) . .
O5 La1 C10 143.6(2) . .
O5 La1 O1 72.75(18) . .
O5 La1 O2 110.2(2) . .
O5 La1 O4 73.16(18) . .
O5 La1 N1 92.3(2) . .
O6 La1 La1 67.89(12) . 3_756
O6 La1 O8 66.73(16) . 3_756
O6 La1 O9 79.90(19) . .
O6 La1 C10 68.00(19) . .
O6 La1 O1 148.41(19) . .
O6 La1 O2 145.3(2) . .
O6 La1 N1 159.7(2) . .
O8 La1 La1 38.56(12) . 3_756
O8 La1 La1 34.75(11) 3_756 3_756
O8 La1 O6 78.42(18) . .
O8 La1 O8 73.31(19) . 3_756
O8 La1 O9 122.59(17) . .
O8 La1 C10 98.2(2) . .
O8 La1 C10 25.16(18) 3_756 .
O8 La1 O1 95.02(19) . .
O8 La1 O2 136.2(2) . .
O8 La1 N1 115.0(2) . .
O8 La1 N1 130.2(2) 3_756 .
O9 La1 La1 84.04(12) . 3_756
O9 La1 O8 49.29(17) . 3_756
O9 La1 C10 24.71(19) . .
O9 La1 O1 127.46(19) . .
O9 La1 O2 77.7(2) . .
O9 La1 N1 102.9(3) . .
O7 La1 La1 65.80(13) . 3_756
O7 La1 O6 132.79(18) . .
O7 La1 O8 71.33(19) . .
O7 La1 O8 70.29(18) . 3_756
O7 La1 O9 86.8(2) . .
O7 La1 C10 81.3(2) . .
O7 La1 O1 71.01(19) . .
O7 La1 O2 71.8(2) . .
O7 La1 N1 67.5(2) . .
C10 La1 La1 59.75(15) . 3_756
C10 La1 N1 121.6(3) . .
O1 La1 La1 124.04(14) . 3_756
O1 La1 O8 141.29(17) . 3_756
O1 La1 C10 143.4(2) . .
O1 La1 O2 50.5(2) . .
O1 La1 N1 24.7(2) . .
O2 La1 La1 134.49(16) . 3_756
O2 La1 O8 114.7(2) . 3_756
O2 La1 C10 98.8(2) . .
O2 La1 N1 25.9(3) . .
O4 La1 La1 141.41(14) . 3_756
O4 La1 O6 75.72(19) . .
O4 La1 O8 117.70(17) . 3_756
O4 La1 O8 143.64(18) . .
O4 La1 O9 77.26(18) . .
O4 La1 O7 144.4(2) . .
O4 La1 C10 95.3(2) . .
O4 La1 O1 93.81(19) . .
O4 La1 O2 73.8(2) . .
O4 La1 N1 85.2(2) . .
N1 La1 La1 132.23(17) . 3_756
N3 O5 La1 127.9(4) . .
C4 O6 La1 135.4(5) 3_856 .
O5 N3 C1 119.7(6) . .
O5 N3 C6 118.9(6) . .
C1 N3 C6 121.3(7) . .
O4 N2 C7 119.5(7) . .
C12 N2 C7 121.6(7) . .
C12 N2 O4 118.8(7) . .
La1 O8 La1 106.69(19) . 3_756
C10 O8 La1 162.3(5) 3_756 .
C10 O8 La1 89.0(4) 3_756 3_756
C10 O9 La1 96.6(5) . .
N2 C7 C8 119.7(8) . .
N3 C1 C2 119.8(8) . .
C4 O7 La1 142.3(5) 1_455 .
C1 C2 C3 120.0(8) . .
C3 C5 C6 121.2(8) . .
O8 C10 La1 65.8(4) 3_756 .
O8 C10 C9 119.3(7) 3_756 .
O9 C10 La1 58.7(4) . .
O9 C10 O8 122.2(7) . 3_756
O9 C10 C9 118.6(7) . .
C9 C10 La1 162.2(5) . .
C8 C9 C10 120.8(7) 4_556 .
C11 C9 C10 120.3(7) . .
C11 C9 C8 118.7(8) . 4_556
N1 O1 La1 96.4(5) . .
C2 C3 C4 120.2(8) . .
C5 C3 C2 118.6(7) . .
C5 C3 C4 121.2(7) . .
O6 C4 O7 125.3(8) 3_856 1_655
O6 C4 C3 118.5(7) 3_856 .
O7 C4 C3 116.2(7) 1_655 .
N1 O2 La1 93.7(6) . .
N3 C6 C5 119.1(7) . .
N2 O4 La1 126.1(4) . .
C7 C8 C9 120.1(8) . 4
N2 C12 C11 119.8(8) . 4
C9 C11 C12 120.0(8) . 4_556
O1 N1 La1 58.8(4) . .
O1 N1 O2 118.8(8) . .
O2 N1 La1 60.5(5) . .
O3 N1 La1 171.9(7) . .
O3 N1 O1 122.7(11) . .
O3 N1 O2 118.5(10) . .
O10 C13 O11 164(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 La1 4.1747(8) 3_756
La1 O5 2.462(5) .
La1 O6 2.533(5) .
La1 O8 2.484(5) .
La1 O8 2.716(5) 3_756
La1 O9 2.561(6) .
La1 O7 2.476(5) .
La1 C10 2.978(8) .
La1 O1 2.591(6) .
La1 O2 2.624(7) .
La1 O4 2.464(5) .
La1 N1 3.009(9) .
O5 N3 1.339(8) .
O6 C4 1.254(10) 3_856
N3 C1 1.344(10) .
N3 C6 1.356(10) .
N2 C7 1.357(11) .
N2 O4 1.338(8) .
N2 C12 1.333(10) .
O8 La1 2.716(5) 3_756
O8 C10 1.266(9) 3_756
O9 C10 1.253(9) .
C7 C8 1.365(12) .
C1 C2 1.380(12) .
O7 C4 1.269(10) 1_455
C2 C3 1.389(11) .
C5 C3 1.356(11) .
C5 C6 1.378(11) .
C10 O8 1.266(9) 3_756
C10 C9 1.504(11) .
C9 C8 1.387(11) 4_556
C9 C11 1.374(11) .
O1 N1 1.268(11) .
C3 C4 1.498(11) .
C4 O6 1.254(10) 3_856
C4 O7 1.269(10) 1_655
O2 N1 1.316(12) .
C8 C9 1.387(11) 4
O3 N1 1.214(11) .
C12 C11 1.381(11) 4
C11 C12 1.381(11) 4_556
O10 C13 1.05(3) .
C13 O11 1.25(4) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.368 0.250 0.500 110 8 ' '
2 0.632 0.750 0.250 111 9 ' '
