Green and rapid mechanosynthesis of high-porosity NU- and UiO-type metal-organic frameworks.
Fidelli, Athena M.; Karadeniz, Bahar; Howarth, Ashlee J.; Huskić, Igor; Germann, Luzia S.; Halasz, Ivan; Etter, Martin; Moon, Su-Young; Dinnebier, Robert E.; Stilinović, Vladimir; Farha, Omar K.; Friščić, Tomislav; UŽarević, Krunoslav; Chemical communications (Cambridge, England) 54 (2018) 6999–7002; doi:10.1039/c8cc03189d

data_7121717
_publ_section_title
;
 Green and rapid mechanosynthesis of high-porosity NU- and UiO-type
 metal-organic frameworks.
;
_journal_issue                   51
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6999
_journal_page_last               7002
_journal_paper_doi               10.1039/c8cc03189d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C51.2 H86.4 O71.2 Zr12'
_chemical_formula_weight         2935.84
_chemical_name_systematic        Zr12_acetate_solvate
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-14 deposited with the CCDC.
2018-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                116.322(6)
_cell_angle_beta                 93.693(6)
_cell_angle_gamma                106.969(5)
_cell_formula_units_Z            1
_cell_length_a                   12.5793(8)
_cell_length_b                   15.7491(8)
_cell_length_c                   16.7679(13)
_cell_measurement_reflns_used    3387
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      61.1090
_cell_measurement_theta_min      4.0420
_cell_volume                     2774.1(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      118(2)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17266
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        58.928
_diffrn_reflns_theta_max         58.928
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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_colour            colourless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       plate
_exptl_crystal_F_000             1443
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetic acid'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.048
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         7922
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0967P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5320
_reflns_number_total             7922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03189d2.cif
_cod_data_source_block           zr12_acetate_sq
_cod_depositor_comments
'Adding full bibliography for 7121717--7121718.cif.'
_cod_original_cell_volume        2774.1(3)
_cod_original_formula_sum        'C51.20 H86.40 O71.20 Zr12'
_cod_database_code               7121717
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              43147
_shelx_fab_checksum              66030