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_4349866
_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         '0.25(C200 H88 Cu12 O60)'
_chemical_formula_sum            'C50 H22 Cu3 O15'
_chemical_formula_weight         1053.29
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_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                   31.038(2)
_cell_length_b                   31.038(2)
_cell_length_c                   20.6449(18)
_cell_measurement_reflns_used    2941
_cell_measurement_temperature    162.89(10)
_cell_measurement_theta_max      42.7670
_cell_measurement_theta_min      4.0290
_cell_volume                     19888(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      N~2~
_diffrn_ambient_temperature      162.89(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -69.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 91

  2 omega   -3.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -80.0000  -90.0000 28

  3 omega   24.00  111.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 87

  4 omega   37.00  118.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 81

  5 omega   35.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -180.0000 47

  6 omega   59.00   87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 28

  7 omega   37.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000    0.0000 67

  8 omega   35.00  132.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000    0.0000 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_UB_11      -0.0273387000
_diffrn_orient_matrix_UB_12      -0.0370566000
_diffrn_orient_matrix_UB_13      0.0286666000
_diffrn_orient_matrix_UB_21      0.0027298000
_diffrn_orient_matrix_UB_22      0.0211012000
_diffrn_orient_matrix_UB_23      0.0672198000
_diffrn_orient_matrix_UB_31      -0.0413771000
_diffrn_orient_matrix_UB_32      0.0255347000
_diffrn_orient_matrix_UB_33      -0.0143092000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.2720
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18347
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.837
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.704
_exptl_crystal_F_000             4232
_platon_squeeze_details
;
;
_refine_diff_density_max         1.842
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         9114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.2211
_refine_ls_R_factor_gt           0.1103
_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^)+(0.1534P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3025
_refine_ls_wR_factor_ref         0.3261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2379
_reflns_number_total             9114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00469b2.cif
_cod_data_source_block           UPC-34
_cod_database_code               4349866
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Cu'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C4(H4), C6(H6), C20(H20), C19(H19), C3(H3), C11(H11),
 C23(H23), C5(H5), C21(H21)
;
_shelx_res_checksum              2213
_shelx_hkl_checksum              70537
_olex2_submission_special_instructions 'No special instructions were received'