A Robust Ethane-Trapping Metal-Organic Framework with a High Capacity for Ethylene Purification.
Qazvini, Omid T.; Babarao, Ravichandar; Shi, Zhao-Lin; Zhang, Yue-Biao; Telfer, Shane G.; Journal of the American Chemical Society 141 (2019) 5014–5020; doi:10.1021/jacs.9b00913

data_4129022
_publ_section_title
;
 A Robust Ethane-Trapping Metal-Organic Framework with a High Capacity for
 Ethylene Purification.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5014
_journal_page_last               5020
_journal_paper_doi               10.1021/jacs.9b00913
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C20 H13 Co3 O12, 4[CH3OH]'
_chemical_formula_sum            'C32 H61 Co3 O24'
_chemical_formula_weight         1006.59
_chemical_name_systematic        MUF-15
_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   mixed
_audit_creation_date             2019-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.714(2)
_cell_length_b                   21.1265(7)
_cell_length_c                   10.9460(3)
_cell_measurement_reflns_used    5893
_cell_measurement_temperature    293
_cell_measurement_theta_max      50.2
_cell_measurement_theta_min      2.1
_cell_volume                     6640.1(5)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.236
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax-HF Confocal Optical System'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.236
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16306
_diffrn_reflns_point_group_measured_fraction_full 0.236
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         35.120
_diffrn_reflns_theta_min         6.022
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    12.580
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         1426
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0878
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2481
_refine_ls_wR_factor_ref         0.2680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1066
_reflns_number_total             1426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00913_si_002.cif
_cod_data_source_block           muf-15
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4129022
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.366
_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. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(C18) \\sim Ueq, : with sigma of 0.05 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O9, O11, O6, O10, C10, C12, C15, C14, C13, C11, C9, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O3, O4, O2, C4, C2, C3, C7, C6, C5, C8, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, O7, C20, C19, C18, C21, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(O12)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Fixed X: H1(0.55807)
 Fixed Y: H1(0.40802)
 Fixed Z: H1(1.142241)
5.a Rotating group:
 O12(H12A,H12B), O12A(H12C,H12D)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C13(H13), C11(H11), C20(H20), C19(H19), C4(H4), C3(H3),
 C6(H6), C5(H5), C21(H21)
5.c Fitted hexagon refined as free rotating group:
 C10(C12,C15,C14,C13,C11), C4(C2,C3,C7,C6,C5)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 582.0 electrons were found in a volume of 2654.0\%A^3 in 1 void. This is consistent with the presence of 4[CH3OH] per formula unit which account for 576.0 electrons. Methanol was chosen as uncoordianted molecules in the pores as it was the main solvent used for MUF-15 synthesis.
;
_shelx_res_checksum              66443
_shelx_hkl_checksum              34477
_shelx_fab_checksum              3467
_olex2_diffrn_ambient_temperature_device 293
_olex2_submission_original_sample_id MUF-15
_olex2_submission_special_instructions 'No special instructions were received'