Cage-Interconnected Metal-Organic Framework with Tailored Apertures for Efficient C<sub>2</sub>H<sub>6</sub>/C<sub>2</sub>H<sub>4</sub> Separation under Humid Conditions.
Zeng, Heng; Xie, Xiao-Jing; Xie, Mo; Huang, Yong-Liang; Luo, Dong; Wang, Ting; Zhao, Yifang; Lu, Weigang; Li, Dan; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10923

data_4133765
_publ_section_title
;
 Cage-Interconnected Metal-Organic Framework with Tailored Apertures for
 Efficient C<sub>2</sub>H<sub>6</sub>/C<sub>2</sub>H<sub>4</sub>
 Separation under Humid Conditions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10923
_journal_year                    2019
_chemical_formula_moiety         '0.01(C1248 H768 Cu96 N864 O384 Zn192)'
_chemical_formula_sum            'C13 H8 Cu N9 O4 Zn2'
_chemical_formula_weight         548.56
_space_group_crystal_system      cubic
_space_group_IT_number           226
_space_group_name_Hall           '-F 4a 2 3'
_space_group_name_H-M_alt        'F m -3 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            96
_cell_length_a                   43.5489(3)
_cell_length_b                   43.5489(3)
_cell_length_c                   43.5489(3)
_cell_measurement_reflns_used    3732
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3360
_cell_measurement_theta_min      2.8630
_cell_volume                     82590.8(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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    -30.00   4.00   0.50   12.01    --   -0.90 -82.00-146.00   68
  2  \w     54.00  79.00   0.50   20.00    --  105.10 -82.00-146.00   50
  3  \w    116.00 194.00   0.50   20.00    --  105.10  82.00-180.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0014958000
_diffrn_orient_matrix_UB_12      -0.0261389000
_diffrn_orient_matrix_UB_13      -0.0238020000
_diffrn_orient_matrix_UB_21      -0.0319078000
_diffrn_orient_matrix_UB_22      0.0092015000
_diffrn_orient_matrix_UB_23      -0.0121645000
_diffrn_orient_matrix_UB_31      0.0151750000
_diffrn_orient_matrix_UB_32      0.0220282000
_diffrn_orient_matrix_UB_33      -0.0231513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            20115
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.604
_diffrn_reflns_theta_min         2.870
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       block
_exptl_crystal_F_000             25920
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+229.8520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2733
_reflns_number_total             3780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10923_si_002.cif
_cod_data_source_block           Desolvated_JNU-2
_cod_original_cell_volume        82590.8(17)
_cod_original_sg_symbol_Hall     '-F 4c 2 3'
_cod_database_code               4133765
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.784
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C11-N2
 1.365 with sigma of 0.007
 C3-N2
 1.352 with sigma of 0.013
 C3-N4
 1.318 with sigma of 0.009
 C5-N4
 1.387 with sigma of 0.007
 C11-C5
 1.389 with sigma of 0.009
 C5-C6
 1.409 with sigma of 0.01
 C6-N8
 1.35 with sigma of 0.01
 C6-N7
 1.337 with sigma of 0.014
 C9-N8
 1.334 with sigma of 0.011
 C9-N10
 1.334 with sigma of 0.011
 C11-N10
 1.343 with sigma of 0.013
 C11-C3
 2.176 with sigma of 0.014
 N4-N2
 2.239 with sigma of 0.015
 C5-C3
 2.128 with sigma of 0.012
 C11-N4
 2.28 with sigma of 0.013
 C6-N4
 2.555 with sigma of 0.016
 C11-C6
 2.382 with sigma of 0.04
 C5-N8
 2.36 with sigma of 0.017
 C5-N7
 2.419 with sigma of 0.02
 N8-N7
 2.306 with sigma of 0.021
 C9-C6
 2.308 with sigma of 0.018
 N8-N10
 2.405 with sigma of 0.017
 C9-C11
 2.267 with sigma of 0.04
 C5-N2
 2.197 with sigma of 0.012
 N10-N2
 2.418 with sigma of 0.02
 C5-N10
 2.441 with sigma of 0.017
 Cu1-N2 \\sim N2-Cu0A
 with sigma of 0.02
3. Restrained planarity
 C11, N2, C5, N10
 with sigma of 0.1
 C6, C5, N7, N8
 with sigma of 0.1
 C5, N4, C6, C11
 with sigma of 0.1
 N2, C3, N4, C5
 with sigma of 0.1
 C3, N4, C5, C11
 with sigma of 0.1
 N4, C5, C11, N2
 with sigma of 0.1
 C5, C11, N2, C3
 with sigma of 0.1
 C11, N2, C3, N4
 with sigma of 0.1
 C5, C6, N8, C9
 with sigma of 0.1
 C6, N8, C9, N10
 with sigma of 0.1
 N8, C9, N10, C11
 with sigma of 0.1
 C9, N10, C11, C5
 with sigma of 0.1
 N10, C11, C5, C6
 with sigma of 0.1
 C11, C5, C6, N8
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N2 \\sim C3 \\sim N4 \\sim C5 \\sim C6 \\sim N7 \\sim N8 \\sim C9 \\sim N10
\\sim C11: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 N2, C3, N4, C5, C6, N7, N8, C9, N10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N2(0.5) C3(0.5) H3(0.5) N4(0.5) C5(0.5) C6(0.5) N7(0.5) H7A(0.5)
 H7B(0.5) N8(0.5) C9(0.5) H9(0.5) N10(0.5) C11(0.5) Cu1(0.25) Cu0A(0.25)
7.a Free rotating group:
 N2(C3,N4,C5,C6,N7,N8,C9,N10,C11)
7.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C3(H3), C9(H9)
7.c X=CH2 refined with riding coordinates:
 N7(H7A,H7B)
;
_shelx_res_checksum              25003
_shelx_hkl_checksum              79224
_shelx_fab_checksum              97447
_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 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.910