Flexibility of a Metal–Organic Framework Enhances Gas Separation and Enables Quantum Sieving
Qazvini, Omid T.; Scott, Victoria-Jayne; Bondorf, Linda; Ducamp, Maxime; Hirscher, Michael; Coudert, François-Xavier; Telfer, Shane G.; Chemistry of Materials 33 (2021) 8886–8894; doi:10.1021/acs.chemmater.1c03170

data_4004054
_publ_section_title
;
 Flexibility of a Metal--Organic Framework Enhances Gas Separation and
 Enables Quantum Sieving
;
_journal_issue                   22
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8886
_journal_page_last               8894
_journal_paper_doi               10.1021/acs.chemmater.1c03170
_journal_volume                  33
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H40 Co6 O31, 2(H2 O), O, 2(H)'
_chemical_formula_sum            'C45 H46 Co6 O34'
_chemical_formula_weight         1484.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-13
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.57(5)
_cell_length_b                   28.68(6)
_cell_length_c                   10.94(3)
_cell_measurement_reflns_used    9684
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.47
_cell_measurement_theta_min      3.66
_cell_volume                     7082(3)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1463
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            158767
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        58.512
_diffrn_reflns_theta_max         58.512
_diffrn_reflns_theta_min         2.491
_diffrn_source                   'Bruker IuS DIAMOND'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.456
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.4463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2016)'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.425(13)
_refine_ls_extinction_coef       0.0079(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         9939
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.1107
_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          0.2647
_refine_ls_wR_factor_ref         0.2985
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                6669
_reflns_number_total             9939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c03170_si_002.cif
_cod_data_source_block           MUF-15-OMe
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        7082(29)
_cod_database_code               4004054
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.575(13)
 0.425(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C35_1-C34_1
 1.5 with sigma of 0.02
 Co4_1-H27A_1 \\sim Co4_1-H27B_1
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C45_1) \\sim Ueq, Uanis(C15_1) \\sim Ueq, Uanis(O31_1) \\sim Ueq,
Uanis(C43_1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3_1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: O5W(0.5) H5WA(0.5) H5WB(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5)
 Fixed Uiso: O5W(0.4) O1W(0.4) O3W(0.4) O2W(0.4)
 Fixed X: H11A(0.04616) H11B(0.046579) O5W(-0.0291) H5WA(-0.04841) H5WB(-
 0.003731) O1W(0.08015) H(0.10319) HA(0.086929) O3W(0.23738) H3WA(0.26057)
 H3WB(0.21007) O2W(0.105161) H2WA(0.093901) H2WB(0.101661)
 Fixed Y: H11A(0.46367) H11B(0.432189) O5W(0.075769) H5WA(0.06284)
 H5WB(0.09276) O1W(0.03183) H(0.05527) HA(0.01767) O3W(0.395761) H3WA(0.383341)
 H3WB(0.41039) O2W(0.36865) H2WA(0.3757) H2WB(0.33917)
 Fixed Z: H11A(0.01052) H11B(-0.0895) O5W(-0.063951) H5WA(-0.0065) H5WB(-
 0.0277) O1W(0.67325) H(0.67169) HA(0.60644) O3W(0.696429) H3WA(0.74827)
 H3WB(0.73372) O2W(0.72883) H2WA(0.80064) H2WB(0.72533)
6.a Free rotating group:
 O27(H27A,H27B)
6.b Rotating group:
 O12(H12A,H12B), O25(H25A,H25B)
6.c Ternary CH refined with riding coordinates:
 O2(H2), O4(H4)
6.d Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C)
6.e Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4A), C6(H6), C10(H10), C12(H12), C14(H14), C19(H19), C21(H21),
 C23(H23), C26(H26), C28(H28), C30(H30), C36(H36), C38(H38), C40(H40)
;
_shelx_res_checksum              34637
_shelx_hkl_checksum              77932
_olex2_submission_original_sample_id MUF-15-OMe
_olex2_submission_special_instructions 'No special instructions were received'