A diamantane-4,9-dicarboxylate based UiO-66 analogue: challenging larger hydrocarbon cage platforms
Gvilava, Vasily; Vieten, Maximilian; Oestreich, Robert; Woschko, Dennis; Steinert, Moritz; Boldog, Ishtvan; Bulanek, Roman; Fokina, Natalie A.; Schreiner, Peter Richard; Janiak, Christoph; CrystEngComm  (2022) –; doi:10.1039/D2CE01170K

data_7245558
_publ_section_title
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 A diamantane-4,9-dicarboxylate based UiO-66 analogue: challenging larger
 hydrocarbon cage platforms
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01170K
_journal_year                    2022
_chemical_compound_source
'Crystallization from a solution of ZrCl4 and 4,9-diamantanedicarboxylic acid in a mixture of DMF and formic acid at 120 degrees Celsius.'
_chemical_formula_moiety
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Zr6, O4, (OH)4, (HCOO)2.86, (C16H18O4)4.56, (O)6.34 
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_chemical_formula_sum            'C75.963 H82.238 O38.341 Zr6'
_chemical_formula_weight         2156
_chemical_name_systematic
'catena-[hexakis(\m~4~-4,9-diamantanedicarboxylate)-tetra(\m~3~-oxo)-tetra(\m~3~-hydroxo)-hexazirconium];Additional note: the compound is modulated by formiate. The refined 4,9-diamantanedicarboxylate:formiate ratio is 4.56:2.86,which corresponds to [Zr6O4(OH)4(HCOO)2.86(C16H18O4)4.56] compositioncompared with the idealized, non-modulated [Zr6O4(OH)4(C16H18O4)6].The residual guest molecules in the pores are modeled by O-atoms.'
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      225
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_audit_update_record
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2022-02-28 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.49022(13)
_cell_length_b                   23.49022(13)
_cell_length_c                   23.49022(13)
_cell_volume                     12961.68(12)
_diffrn_ambient_temperature      295
_diffrn_detector                 'solid state plate'
_diffrn_detector_type
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D/teX Ultra silicon strip detector
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_diffrn_measurement_device       'powder XRD diffractometer'
_diffrn_measurement_device_type  'Rigaku MiniFlex'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MiniFlex'
_exptl_absorpt_coefficient_mu    4.331
_exptl_crystal_density_diffrn    1.1048
_exptl_crystal_F_000             4339
_pd_char_colour                  colorless
_pd_char_particle_morphology
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Cubic microcrystals, ~1-10 um size. The size is controlled by crystallization.
No additional grinding or sieving were applied. 
;
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        99.990
_pd_meas_2theta_range_min        2.000
_pd_meas_number_of_points        9800
_pd_meas_scan_method             cont
_pd_prep_temperature             395
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        99.99
_pd_proc_2theta_range_min        5.01
_pd_proc_ls_background_function  '36 Legendre polynoms'
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_prof_R_factor        0.0315
_pd_proc_ls_prof_wR_expected     0.0076
_pd_proc_ls_prof_wR_factor       0.0450
_pd_spec_mounting                'indented low-background sample holder'
_pd_spec_mount_mode              reflection
_pd_spec_orientation             horizontal
_pd_spec_preparation
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The synthesized crystals were washed by DMF and dried at 10-2 Torr and 120 C. 
The treatment removed the free DMF and also a part of the DMF in the pores 
(the sample could be classified as partially activated. This treatment allowed
to retain maximally the crystallinity of the sample). 
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_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              ~5
_pd_spec_size_equat              ~5
_pd_spec_size_thick              ~0.4
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.26
_refine_ls_goodness_of_fit_all   5.90
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    52
_refine_ls_number_parameters     59
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0045
_refine_ls_shift/su_mean         0.0001
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0508
_refine_ls_wR_factor_gt          0.0508
_cod_data_source_file            d2ce01170k2.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
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_cod_original_sg_symbol_Hall     -F_4_2_3
_cod_database_code               7245558