Solvent-induced framework-interpenetration isomers of Cu MOFs for efficient light hydrocarbon separation
Wang, Yutong; Fan, Weidong; Wang, Xia; Han, Yinfeng; Zhang, Liangliang; Liu, Di; Dai, Fangna; Sun, Daofeng; Inorganic Chemistry Frontiers 5 (2018) 2408–; doi:10.1039/C8QI00469B

data_4349867
_publ_section_title
;
 Solvent-induced framework-interpenetration isomers of Cu MOFs for
 efficient light hydrocarbon separation
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2408
_journal_paper_doi               10.1039/C8QI00469B
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         '0.13(C400 H208 Cu24 O120)'
_chemical_formula_sum            'C50 H26 Cu3 O15'
_chemical_formula_weight         1057.33
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.3382(11)
_cell_length_b                   31.3382(11)
_cell_length_c                   39.0786(10)
_cell_measurement_reflns_used    3093
_cell_measurement_temperature    273.45(10)
_cell_measurement_theta_max      46.5040
_cell_measurement_theta_min      4.4500
_cell_volume                     38378(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      273.45(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_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    -25.00   4.00   1.00    4.04    --    0.00  97.00-130.00   29
  2  \w    -21.00  16.00   1.00    4.04    --    0.00  61.00 133.00   37
  3  \w     23.00 112.00   1.00   16.16    --   54.00-125.00  30.00   89
  4  \w     91.00 121.00   1.00   16.16    --   54.00  77.00 150.00   30
  5  \w     25.00  74.00   1.00   16.16    --   54.00-125.00-180.00   49
  6  \w    139.00 166.00   1.00   16.16    --  108.00  97.00-130.00   27
  7  \w    100.00 178.00   1.00   16.16    --  108.00 111.00 -60.00   78
  8  \w    114.00 163.00   1.00   16.16    --  108.00 111.00 -90.00   49
  9  \w     81.00 178.00   1.00   16.16    --  108.00  77.00 -30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0460262000
_diffrn_orient_matrix_UB_12      0.0152757000
_diffrn_orient_matrix_UB_13      0.0066609000
_diffrn_orient_matrix_UB_21      0.0038614000
_diffrn_orient_matrix_UB_22      0.0317918000
_diffrn_orient_matrix_UB_23      -0.0298758000
_diffrn_orient_matrix_UB_31      -0.0170025000
_diffrn_orient_matrix_UB_32      -0.0341271000
_diffrn_orient_matrix_UB_33      -0.0248794000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            34407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.059
_diffrn_reflns_theta_max         67.059
_diffrn_reflns_theta_min         3.616
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.366
_exptl_crystal_description       block
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         8965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.731
_refine_ls_R_factor_all          0.1478
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2543
_reflns_number_total             8965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00469b2.cif
_cod_data_source_block           UPC-35
_cod_original_cell_volume        38378(3)
_cod_database_code               4349867
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Cu'
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.949
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1A(0.25) H1B(0.25) H2A(0.25) H2B(0.25)
3.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C4(H4), C3(H3), C5(H5), C11(H11), C7(H7)
;
_shelx_res_checksum              61176
_shelx_hkl_checksum              40481
_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 2.251
_oxdiff_exptl_absorpt_empirical_full_min 0.674