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_4135633
_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         'Br0.5 C2.5 Cu0.5 N2, 0.25(C H2)'
_chemical_formula_sum            'C2.75 H0.5 Br0.5 Cu0.5 N2'
_chemical_formula_weight         133.28
_chemical_name_systematic        br-yx
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-13
_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            8
_cell_length_a                   10.9748(3)
_cell_length_b                   8.5812(3)
_cell_length_c                   10.0596(4)
_cell_measurement_reflns_used    2914
_cell_measurement_temperature    120(3)
_cell_measurement_theta_max      25.3090
_cell_measurement_theta_min      3.6210
_cell_volume                     947.38(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     44.00  76.00   1.00    4.50    --   18.78-125.00  48.00   32
  2  \w     -8.00  58.00   1.00    4.50    --   18.78  77.00-120.00   66
  3  \w     -2.00  73.00   1.00    4.50    --   18.78  57.00-180.00   75
  4  \w    -89.00 -62.00   1.00    4.50    --  -19.88-178.00-150.00   27
  5  \w    -95.00 -64.00   1.00    4.50    --  -19.88-178.00 -30.00   31
  6  \w    -36.00  26.00   1.00    4.50    --  -19.88  37.00  30.00   62
  7  \w    -80.00  53.00   1.00    4.50    --  -19.88   0.00 -30.00  133
;
_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      0.0028551000
_diffrn_orient_matrix_UB_12      0.0618506000
_diffrn_orient_matrix_UB_13      0.0466841000
_diffrn_orient_matrix_UB_21      0.0643983000
_diffrn_orient_matrix_UB_22      0.0010199000
_diffrn_orient_matrix_UB_23      -0.0056974000
_diffrn_orient_matrix_UB_31      -0.0044289000
_diffrn_orient_matrix_UB_32      0.0548667000
_diffrn_orient_matrix_UB_33      -0.0525249000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6260
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         3.120
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53530
_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            'metallic light white'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         866
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.9315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                808
_reflns_number_total             866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja1c02108_si_002.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 4135632--4135635.cif.'
_cod_original_formula_sum        'C2.75 H0.50 Br0.50 Cu0.50 N2'
_cod_database_code               4135633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.358
_shelx_estimated_absorpt_t_min   0.358
_reflns_odcompleteness_completeness 89.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C1-C1_$1
 1.4 with sigma of 0.02
 H1B-H1A
 1.568 with sigma of 0.01
 H1A_$1-H1B_$1
 1.568 with sigma of 0.01
 C1-H1B = C1-H1A = C1_$1-H1B_$1 = C1_$1-H1A_$1
 0.96 with sigma of 0.001
 H1B-H1A_$1
 2.537 with sigma of 0.01
 H1A-H1B_$1
 2.537 with sigma of 0.01
 H1B-H1B_$1
 2.966 with sigma of 0.001
 C1-H1A \\sim C1-H1B
 with sigma of 0.0001
2. Restrained planarity
 C1_$1, C1, H1A_$1, H1B_$1, H1A, H1B
 with sigma of 0.001
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: C1(0.25) H1A(0.25) H1B(0.25)
;
_shelx_res_checksum              50999
_shelx_hkl_checksum              88354
_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 1.548
_oxdiff_exptl_absorpt_empirical_full_min 0.768