Pressure and Guest-Mediated Pore Shape Modification in a Small Pore MOF to 1200 bar
McMonagle, Charles J.; Turner, Gemma; Jones, Isabelle; Allan, David Robert; Warren, Mark R.; Kamenev, K.; Parsons, Simon; Wright, Paul; Moggach, Stephen A.; Chemical Communications  (2022) –; doi:10.1039/D2CC04649K

data_7130742
_publ_section_title
;
 Pressure and Guest-Mediated Pore Shape Modification in a Small Pore MOF
 to 1200 bar
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04649K
_journal_year                    2022
_chemical_formula_moiety         'C12 H6 O6 Sc1, 0.478(C5 H12)'
_chemical_formula_sum            'C14.4 H11.7 O6 Sc'
_chemical_formula_weight         291.13
_chemical_name_common            Sc2BDC3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2017-08-02
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   8.7579(3)
_cell_length_b                   20.7370(5)
_cell_length_c                   34.3224(9)
_cell_measurement_pressure       60000
_cell_measurement_reflns_used    6166
_cell_measurement_temperature    298
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     6233.4(3)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_pressure         60000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Pilatus 300K'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            14843
_diffrn_reflns_theta_full        29.490
_diffrn_reflns_theta_max         29.490
_diffrn_reflns_theta_min         2.224
_diffrn_source_type              'Diamond Light Source I19'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2378
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.0056687
_refine_ls_shift/su_mean         0.0001527
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +12.80P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1078
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1078
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              48
_reflns_limit_l_min              0
_reflns_number_gt                2078
_reflns_number_total             2386
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0413
_oxford_refine_ls_scale          1.607(13)
_oxford_reflns_number_all        2378
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'xcalibur in C:\frames\Diamond\S At 17:35 on '
_cod_data_source_file            d2cc04649k2.cif
_cod_data_source_block           np-600bar
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' 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 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C14.4 H11.7 O6 Sc1'
_cod_database_code               7130742
_platon_squeeze_void_probe_radius 1.20