A novel trigonal bipyramidal cage-based Zn(ii)-MOF featuring two types of trinuclear clusters with high gas sorption properties
Duan, Hai-Yu; Li, Xiu-Yuan; Zhang, Chen-Xu; He, Chaozheng; CrystEngComm  (2022) –; doi:10.1039/D2CE01399A

data_7245749
_publ_section_title
;
 A novel trigonal bipyramidal cage-based Zn(ii)-MOF featuring two types of
 trinuclear clusters with high gas sorption properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01399A
_journal_year                    2022
_chemical_formula_moiety         'C60 H28 O33 Zn6'
_chemical_formula_sum            'C60 H28 O33 Zn6'
_chemical_formula_weight         1669.04
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-10-07 deposited with the CCDC.	2022-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.5095(7)
_cell_length_b                   16.5095(7)
_cell_length_c                   24.5306(18)
_cell_measurement_reflns_used    8999
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      53.895
_cell_measurement_theta_min      3.1125
_cell_volume                     5790.4(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40722
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.245
_diffrn_reflns_theta_min         1.649
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6897
_refine_ls_number_restraints     713
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.011
_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          0.2551
_refine_ls_wR_factor_ref         0.2831
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                3530
_reflns_number_total             6897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01399a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5790.4(6)
_cod_database_code               7245749
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.428
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(4)
 0.45(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H11 of O11
 At 1.5 times of:
  All O(H,H) groups, H13 of O13
3. Restrained distances
 C15-C1
 1.46 with sigma of 0.01
 C4-O7
 1.45 with sigma of 0.01
 C20_$3-C19_$3 = C20_$3-C19_$4 = C20_$4-C19_$4 = C20_$4-C19 = C20-C19 = C20-
 C19_$3
 1.42 with sigma of 0.01
 C19-C19_$3 = C19_$3-C19_$4
 2.2 with sigma of 0.01
 C20-C20_$3 = C20_$3-C20_$4
 2.2 with sigma of 0.01
 O4-C13 = O8-C13
 1.2 with sigma of 0.01
 O2-C15 = O5-C15
 1.2 with sigma of 0.01
 O5-C1 = C1-O2
 2.3 with sigma of 0.02
 O9-C18 = O10-C18
 1.2 with sigma of 0.01
 C11-C13
 1.46 with sigma of 0.01
 Zn3-O12
 2 with sigma of 0.01
4. Restrained planarity
 C19_$3, C19, C19_$4, C20_$4, C20_$3, C20
 with sigma of 0.01
 O9_$1, O10_$1, C5_$1, C18_$1
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(O12) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H12A(0.33333) H12B(0.33333) O13(0.33333) H13(0.33333)
8.a Riding coordinates:
 O12(H12A,H12B), O13(H13)
8.b Ternary CH refined with riding coordinates:
 O11(H11)
8.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C12(H12), C17(H17), C19(H19)
8.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C8,C9,C10,C11,C12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66985
_shelx_hkl_checksum              89599
_shelx_fab_checksum              70473
_olex2_submission_special_instructions 'No special instructions were received'