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_4514505
_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         '0.5(C48 H32 N12 Nd4 O36), C3 H7 N O'
_chemical_formula_sum            'C27 H23 N7 Nd2 O19'
_chemical_formula_weight         1038.00
_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                 109.892(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2658(3)
_cell_length_b                   17.4390(5)
_cell_length_c                   11.4882(3)
_cell_measurement_reflns_used    2580
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.6750
_cell_measurement_theta_min      3.0000
_cell_volume                     1933.97(11)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     35.00  64.00   1.00    7.50    --   18.63 178.00-150.00   29
  2  \w      3.00  61.00   1.00    7.50    --   18.63 -99.00-150.00   58
  3  \w    -87.00 -36.00   1.00    7.50    --  -19.56-178.00-150.00   51
  4  \w    -88.00  -4.00   1.00    7.50    --  -19.56 -57.00  30.00   84
;
_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      0.0144074000
_diffrn_orient_matrix_UB_12      0.0143077000
_diffrn_orient_matrix_UB_13      -0.0521122000
_diffrn_orient_matrix_UB_21      0.0487502000
_diffrn_orient_matrix_UB_22      -0.0298991000
_diffrn_orient_matrix_UB_23      0.0061977000
_diffrn_orient_matrix_UB_31      -0.0530420000
_diffrn_orient_matrix_UB_32      -0.0236162000
_diffrn_orient_matrix_UB_33      -0.0394151000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7141
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96969
_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 pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0410
_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/[\s^2^(Fo^2^)+(0.0387P)^2^+3.2968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                2623
_reflns_number_total             3398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am9b04619_si_003.cif
_cod_data_source_block           NKMOF-3-Nd
_cod_original_cell_volume        1933.97(10)
_cod_database_code               4514505
_chemical_oxdiff_formula         'Nd C N O'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: N4(0.5) O10(0.5) C15(0.5) H15(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 Fixed Uiso: H1(0.023) H2(0.023) H5(0.026) H6(0.028) H7(0.025) H11(0.022)
 H8(0.027) H12(0.024) H15(0.045) H13A(0.045) H13B(0.045) H13C(0.045) H14A(0.09)
 H14B(0.09) H14C(0.09)
 Fixed X: H1(0.3256) H2(0.5621) H5(-0.4838) H6(0.2812) H7(0.1509) H11(-0.0968)
 H8(0.0949) H12(-0.0443) H15(-0.3141) H13A(-0.3495) H13B(-0.4757) H13C(-0.4968)
 H14A(-0.6222) H14B(-0.6807) H14C(-0.6217)
 Fixed Y: H1(-0.1279) H2(-0.1082) H5(-0.0103) H6(-0.0274) H7(0.1975)
 H11(0.2874) H8(0.1845) H12(0.0959) H15(0.1567) H13A(0.1789) H13B(0.2323)
 H13C(0.1433) H14A(0.2097) H14B(0.1907) H14C(0.2726)
 Fixed Z: H1(0.4749) H2(0.5378) H5(0.2118) H6(0.1556) H7(0.2782) H11(0.3643)
 H8(0.6878) H12(-0.0414) H15(0.2157) H13A(0.0206) H13B(-0.0462) H13C(-0.0436)
 H14A(0.1894) H14B(0.0477) H14C(0.0921)
;
_olex2_date_sample_data_collection 2018-05-31
_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 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.906