Scalable Room-Temperature Synthesis of Highly Robust Ethane-Selective Metal-Organic Frameworks for Efficient Ethylene Purification.
Geng, Shubo; Lin, En; Li, Xia; Liu, Wansheng; Wang, Ting; Wang, Zhifang; Sensharma, Debobroto; Darwish, Shaza; Andaloussi, Yassin H.; Pham, Tony; Cheng, Peng; Zaworotko, Michael J.; Chen, Yao; Zhang, Zhenjie; Journal of the American Chemical Society 143 (2021) 8654–8660; doi:10.1021/jacs.1c02108

data_4135632
_publ_section_title
;
 Scalable Room-Temperature Synthesis of Highly Robust Ethane-Selective
 Metal-Organic Frameworks for Efficient Ethylene Purification.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8654
_journal_page_last               8660
_journal_paper_doi               10.1021/jacs.1c02108
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C6 H3 Cu N4'
_chemical_formula_sum            'C6 H3 Cu N4'
_chemical_formula_weight         194.66
_chemical_name_systematic        11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9436(11)
_cell_length_b                   8.6154(10)
_cell_length_c                   10.0156(9)
_cell_measurement_reflns_used    546
_cell_measurement_temperature    120(3)
_cell_measurement_theta_max      26.7450
_cell_measurement_theta_min      3.6180
_cell_volume                     944.31(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.918
_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    -54.00  -5.00   1.00   27.50    --   18.78 -37.00-120.00   49
  2  \w    -34.00  92.00   1.00   27.50    --   18.78   0.00  60.00  126
  3  \w    -96.00 -64.00   1.00   27.50    --  -19.88-178.00  60.00   32
;
_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      -0.0044843000
_diffrn_orient_matrix_UB_12      0.0540756000
_diffrn_orient_matrix_UB_13      0.0533937000
_diffrn_orient_matrix_UB_21      0.0554147000
_diffrn_orient_matrix_UB_22      -0.0205482000
_diffrn_orient_matrix_UB_23      0.0342303000
_diffrn_orient_matrix_UB_31      0.0324199000
_diffrn_orient_matrix_UB_32      0.0427148000
_diffrn_orient_matrix_UB_33      -0.0513307000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.1277
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2944
_diffrn_reflns_point_group_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.080
_diffrn_reflns_theta_min         3.633
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         955
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1291P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                544
_reflns_number_total             955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja1c02108_si_005.cif
_cod_data_source_block           p191218f5
_cod_depositor_comments
'Adding full bibliography for 4135632--4135635.cif.'
_cod_original_cell_volume        944.30(16)
_cod_database_code               4135632
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.661
_shelx_estimated_absorpt_t_min   0.661
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C007) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C004) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5)
4.a Idealised Me refined as rotating group:
 C007(H00A,H00B,H00C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19816
_shelx_hkl_checksum              55028
_shelx_fab_checksum              31153
_olex2_date_sample_data_collection 2019-12-19
_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 1.481
_oxdiff_exptl_absorpt_empirical_full_min 0.791