Molecular Sieving and Direct Visualization of CO<sub>2</sub> in Binding Pockets of an Ultramicroporous Lanthanide Metal-Organic Framework Platform.
Han, Lin; Pham, Tony; Zhuo, Mingjing; Forrest, Katherine A.; Suepaul, Shanelle; Space, Brian; Zaworotko, Michael J.; Shi, Wei; Chen, Yao; Cheng, Peng; Zhang, Zhenjie; ACS applied materials & interfaces 11 (2019) 23192–23197; doi:10.1021/acsami.9b04619

data_4514511
_publ_section_title
;
 Molecular Sieving and Direct Visualization of CO<sub>2</sub> in Binding
 Pockets of an Ultramicroporous Lanthanide Metal-Organic Framework
 Platform.
;
_journal_issue                   26
_journal_name_full               'ACS applied materials &amp; 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 Dy N3 O9, C O2'
_chemical_formula_sum            'C13 H8 Dy N3 O11'
_chemical_formula_weight         544.72
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.080(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0804(3)
_cell_length_b                   16.9849(4)
_cell_length_c                   11.1414(4)
_cell_measurement_reflns_used    2993
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      25.3090
_cell_measurement_theta_min      3.3640
_cell_volume                     1802.77(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     56.00  88.00   1.00    3.25    --   18.63  77.00  30.00   32
  2  \w    -11.00  86.00   1.00    3.25    --   18.63  77.00 -60.00   97
  3  \w    -48.00  42.00   1.00    3.25    --  -19.72  77.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0240672000
_diffrn_orient_matrix_UB_12      -0.0225902000
_diffrn_orient_matrix_UB_13      -0.0564928000
_diffrn_orient_matrix_UB_21      0.0215225000
_diffrn_orient_matrix_UB_22      -0.0350133000
_diffrn_orient_matrix_UB_23      0.0358429000
_diffrn_orient_matrix_UB_31      -0.0670730000
_diffrn_orient_matrix_UB_32      -0.0031451000
_diffrn_orient_matrix_UB_33      0.0074173000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6780
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3296
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+1.4992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                2687
_reflns_number_total             3296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am9b04619_si_007.cif
_cod_data_source_block           CO2@NKMOF-3-Dy
_cod_original_cell_volume        1802.77(9)
_cod_database_code               4514511
_chemical_oxdiff_formula         'C N O Ho'
_chemical_oxdiff_usercomment     b4
_reflns_odcompleteness_completeness 89.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C3 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C1(H1), C5(H5), C11(H11), C6(H6), C8(H8), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.830