Stabilization of Scandium Terephthalate MOFs against Reversible Amorphization and Structural Phase Transition by Guest Uptake at Extreme Pressure.
Graham, Alexander J.; Banu, Ana-Maria; Düren, Tina; Greenaway, Alex; McKellar, Scott C.; Mowat, John P. S.; Ward, Kenneth; Wright, Paul A.; Moggach, Stephen A.; Journal of the American Chemical Society 136 (2014) 8606–8613; doi:10.1021/ja411934f

data_4121954
_publ_section_title
;
 Stabilization of Scandium Terephthalate MOFs against Reversible
 Amorphization and Structural Phase Transition by Guest Uptake at Extreme
 Pressure.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8606
_journal_page_last               8613
_journal_paper_doi               10.1021/ja411934f
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H6 N3 O18 Sc2'
_chemical_formula_sum            'C24 H6 N3 O18 Sc2'
_chemical_formula_weight         714.23
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-04-25
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.365(4)
_cell_length_b                   31.823(5)
_cell_length_c                   8.7225(11)
_cell_measurement_reflns_used    1172
_cell_measurement_temperature    293
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     5097.7(15)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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_temperature      293
_diffrn_measured_fraction_theta_full 0.704
_diffrn_measured_fraction_theta_max 0.680
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2910
_diffrn_reflns_theta_full        14.928
_diffrn_reflns_theta_max         19.905
_diffrn_reflns_theta_min         3.221
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.82
_refine_ls_abs_structure_details 'Flack (1983), 364 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.6212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         803
_refine_ls_number_restraints     131
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.1407
_refine_ls_shift/su_max          0.0246341
_refine_ls_shift/su_mean         0.0014842
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3984
_refine_ls_wR_factor_gt          0.3745
_refine_ls_wR_factor_ref         0.3984
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                570
_reflns_number_total             804
_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   0.1747
_oxford_refine_ls_scale          0.0802(2)
_oxford_reflns_number_all        803
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'Sc2NO2BDC3 in Fdd2'
_cod_data_source_file            ScBDCNF5.cif
_cod_data_source_block           ScBDCNO2_FC77_@_1.73_GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4121943--4121962.cif.
;
_cod_original_cell_volume        5097.7(16)
_cod_original_sg_symbol_Hall     'F 2 -2d '
_cod_original_sg_symbol_H-M      'F d d 2 '
_cod_database_code               4121954
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT SC(1, U'S) 
CONT C(1, U[ISO]) UNTIL N(10) 
CONT ENANTIO 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST   1.505,.01= C(1) TO C(2) 
DIST   1.24,.01= C(1) TO O(1) 
DIST   1.24,.01= C(1) TO O(2) 
DIST   1.24,.01= C(8) TO O(3) 
DIST   1.24,.01= C(8) TO O(6) 
DIST   1.24,.01= C(12) TO O(4) 
DIST   1.24,.01= C(12) TO O(5) 
DIST   1.359,.01= C(2) TO C(3) 
DIST   1.375,.01= C(2) TO C(7) 
DIST   1.392,.01= C(3) TO C(4) 
DIST   1.375,.01= C(4) TO C(5) 
DIST   1.359,.01= C(5) TO C(6) 
DIST   1.499,.01= C(5) TO C(12,2,4,0,-1) 
DIST   1.392,.01= C(6) TO C(7) 
DIST   1.499,.01= C(8) TO C(9) 
DIST   1.375,.01= C(9) TO C(10) 
DIST   1.359,.01= C(9) TO C(11) 
DIST   1.392,.01= C(10) TO C(10,4,3,-1,1,-1) 
DIST   1.392,.01= C(11) TO C(11,4,3,-1,1,-1) 
DIST   1.22,.01= O(41) TO N(4) 
DIST   1.22,.01= O(42) TO N(4) 
DIST   1.22,.01= O(71) TO N(7) 
DIST   1.22,.01= O(72) TO N(7) 
DIST   1.22,.01= O(101) TO N(10) 
DIST   1.22,.01= O(102) TO N(10) 
DIST   1.424,.01= C(4) TO N(4) 
DIST   1.424,.01= C(7) TO N(7) 
DIST   1.424,.01= C(10) TO N(10) 
ANGL 118,1= O(1) TO C(1) TO C(2) 
ANGL 121,1= O(2) TO C(1) TO C(2) 
ANGL 122,1= O(2) TO C(1) TO O(1) 
ANGL 117,1= C(3) TO C(2) TO C(1) 
ANGL 122,1= C(7) TO C(2) TO C(1) 
ANGL 120,1= C(7) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 115,1= C(5) TO C(4) TO C(3) 
ANGL 118,1= N(4) TO C(4) TO C(3) 
ANGL 126,1= N(4) TO C(4) TO C(5) 
ANGL 124,1= C(6) TO C(5) TO C(4) 
ANGL 114,1= C(12,2,4,0,-1) TO C(5) TO C(4) 
ANGL 122,1= C(12,2,4,0,-1) TO C(5) TO C(6) 
ANGL 122,1= C(7) TO C(6) TO C(5) 
ANGL 118,1= C(6) TO C(7) TO C(2) 
ANGL 128,1= N(7) TO C(7) TO C(2) 
ANGL 114,1= N(7) TO C(7) TO C(6) 
ANGL 113,1= O(3) TO C(8) TO C(9) 
ANGL 114,1= O(6) TO C(8) TO C(9) 
ANGL 132,1= O(6) TO C(8) TO O(3) 
ANGL 122,1= C(10) TO C(9) TO C(8) 
ANGL 123,1= C(11) TO C(9) TO C(8) 
ANGL 115,1= C(11) TO C(9) TO C(10) 
ANGL 122,1= C(10,4,3,-1,1,-1) TO C(10) TO C(9) 
ANGL 128,1= N(10) TO C(10) TO C(9) 
ANGL 105,1= N(10) TO C(10) TO C(10,4,3,-1,1,-1) 
ANGL 124,1= C(11,4,3,-1,1,-1) TO C(11) TO C(9) 
ANGL 108,1= O(4) TO C(12) TO C(5,2,3,0,0,-1) 
ANGL 123,1= O(5) TO C(12) TO C(5,2,3,0,0,-1) 
ANGL 128,1= O(5) TO C(12) TO O(4) 
ANGL 106,1= N(10) TO O(102) TO O(102,4,3,-1,1,-1) 
ANGL 118,1= O(41) TO N(4) TO C(4) 
ANGL 112,1= O(42) TO N(4) TO C(4) 
ANGL 130,1= O(42) TO N(4) TO O(41) 
ANGL 105,1= O(71) TO N(7) TO C(7) 
ANGL 102,1= O(72) TO N(7) TO C(7) 
ANGL 148,1= O(72) TO N(7) TO O(71) 
ANGL 124,1= O(101) TO N(10) TO C(10) 
ANGL 118,1= O(102) TO N(10) TO C(10) 
ANGL 115,1= O(102) TO N(10) TO O(101) 
PLANAR 0.010000  C(10) O(101) O(102) N(10) 
PLANAR 0.010000  C(7) O(71) O(72) N(7) 
PLANAR 0.010000  C(4) O(41) O(42) N(4) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(7) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(7) TO C(1) 
VIBR .0, 0.00500 = C(7) TO C(3) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO C(12,2,4,0,-1) 
VIBR .0, 0.00200 = C(5) TO C(6) 
VIBR .0, 0.00500 = C(4) TO C(12,2,4,0,-1) 
VIBR .0, 0.00500 = C(6) TO C(12,2,4,0,-1) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(5) 
VIBR .0, 0.00500 = C(2) TO C(6) 
VIBR .0, 0.00200 = C(8) TO C(9) 
VIBR .0, 0.00200 = C(8) TO O(3) 
VIBR .0, 0.00200 = C(8) TO O(6) 
VIBR .0, 0.00500 = O(3) TO C(9) 
VIBR .0, 0.00500 = O(6) TO C(9) 
VIBR .0, 0.00500 = O(6) TO O(3) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00200 = C(9) TO C(11) 
VIBR .0, 0.00500 = C(10) TO C(8) 
VIBR .0, 0.00500 = C(11) TO C(8) 
VIBR .0, 0.00500 = C(11) TO C(10) 
VIBR .0, 0.00200 = C(10) TO C(10,4,3,-1,1,-1) 
VIBR .0, 0.00500 = C(9) TO C(10,4,3,-1,1,-1) 
VIBR .0, 0.00200 = C(11) TO C(11,4,3,-1,1,-1) 
VIBR .0, 0.00500 = C(9) TO C(11,4,3,-1,1,-1) 
VIBR .0, 0.00200 = C(12) TO O(4) 
VIBR .0, 0.00200 = C(12) TO O(5) 
VIBR .0, 0.00500 = O(4) TO C(5,2,3,0,0,-1) 
VIBR .0, 0.00500 = O(5) TO C(5,2,3,0,0,-1) 
VIBR .0, 0.00500 = O(5) TO O(4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.08000 = C(1) TO O(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(7) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.04000 = C(5) TO C(12,2,4,0,-1) 
U(IJ) .0, 0.04000 = C(5) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(8) TO C(9) 
U(IJ) .0, 0.08000 = C(8) TO O(3) 
U(IJ) .0, 0.08000 = C(8) TO O(6) 
U(IJ) .0, 0.04000 = C(9) TO C(10) 
U(IJ) .0, 0.04000 = C(9) TO C(11) 
U(IJ) .0, 0.04000 = C(10) TO C(10,4,3,-1,1,-1) 
U(IJ) .0, 0.04000 = C(11) TO C(11,4,3,-1,1,-1) 
U(IJ) .0, 0.08000 = C(12) TO O(4) 
U(IJ) .0, 0.08000 = C(12) TO O(5) 
VIBR .0, 0.00200 = O(41) TO N(4) 
VIBR .0, 0.00200 = O(42) TO N(4) 
VIBR .0, 0.00200 = O(71) TO N(7) 
VIBR .0, 0.00200 = O(72) TO N(7) 
VIBR .0, 0.00200 = O(101) TO N(10) 
VIBR .0, 0.00200 = O(102) TO N(10) 
VIBR .0, 0.00500 = O(42) TO O(41) 
VIBR .0, 0.00500 = O(72) TO O(71) 
VIBR .0, 0.00500 = O(101) TO O(102) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(41) TO N(4) 
U(IJ) .0, 0.08000 = O(42) TO N(4) 
U(IJ) .0, 0.08000 = O(71) TO N(7) 
U(IJ) .0, 0.08000 = O(72) TO N(7) 
U(IJ) .0, 0.08000 = O(101) TO N(10) 
U(IJ) .0, 0.08000 = O(102) TO N(10) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   END (DO NOT REMOV 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;