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_4121958
_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_formula_moiety         'Sc2(BDC)3. 5.25MeOH'
_chemical_formula_sum            'C29.25 H33 O17.25 Sc2'
_chemical_formula_weight         750.48
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-04-23
_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                   8.8041(15)
_cell_length_b                   20.625(2)
_cell_length_c                   34.062(5)
_cell_measurement_reflns_used    1242
_cell_measurement_temperature    293
_cell_measurement_theta_max      19
_cell_measurement_theta_min      4
_cell_volume                     6185.1(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 0.810
_diffrn_measured_fraction_theta_max 0.769
_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  0.136
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            5980
_diffrn_reflns_theta_full        15.690
_diffrn_reflns_theta_max         20.920
_diffrn_reflns_theta_min         2.585
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.35
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         630
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.1444
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.0007803
_refine_ls_shift/su_mean         0.0000204
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.18P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3144
_refine_ls_wR_factor_gt          0.2676
_refine_ls_wR_factor_ref         0.3144
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                385
_reflns_number_total             636
_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   0.1444
_oxford_refine_ls_scale          0.015850(7)
_oxford_reflns_number_all        630
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'SCBDC05 in Fddd'
_cod_data_source_file            scbdc05.cif
_cod_data_source_block           scbdc05
_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        6185.2(16)
_cod_original_sg_symbol_Hall     '-F 2uv 2vw '
_cod_original_sg_symbol_H-M      'F d d d '
_cod_original_formula_sum        'Sc2 C29.25 O17.25 H33'
_cod_database_code               4121958
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT SC(1, U'S) UNTIL C(7) 
CONT C(40, U[ISO]) UNTIL C(50) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST   1.255,.01= O(1) TO C(1) 
DIST   1.247,.01= C(1) TO O(2) 
DIST   1.496,.01= C(1) TO C(2) 
DIST   1.369,.01= C(2) TO C(3) 
DIST   1.377,.01= C(2) TO C(4,-1,2,0,0,1) 
DIST   1.384,.01= C(3) TO C(4) 
DIST   1.251,.01= O(3) TO C(5) 
DIST   1.492,.01= C(5) TO C(6) 
DIST   1.372,.01= C(6) TO C(7) 
DIST   1.372,.01= C(6) TO C(7,-3,1,0,0,1) 
DIST   1.384,.01= C(7) TO C(7,-2,1,0,1,1) 
ANGL 124,1= O(2) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(2) 
ANGL 121,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(4,-1,2,0,0,1) TO C(2) TO C(1) 
ANGL 119,1= C(4,-1,2,0,0,1) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(3) TO C(4) TO C(2,-1,2,0,0,1) 
ANGL 124,1= O(3,-3,1,0,0,1) TO C(5) TO O(3) 
ANGL 118,1= C(6) TO C(5) TO O(3) 
ANGL 118,1= C(6) TO C(5) TO O(3,-3,1,0,0,1) 
ANGL 120,1= C(7) TO C(6) TO C(5) 
ANGL 120,1= C(7,-3,1,0,0,1) TO C(6) TO C(5) 
ANGL 119,1= C(7,-3,1,0,0,1) TO C(6) TO C(7) 
ANGL 120,1= C(7,-2,1,0,1,1) TO C(7) TO C(6) 
DIST 1.43, 0.01 = O(5) TO C(50) 
DIST 1.43, 0.01 = O(4) TO C(40) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00200 = C(2) TO C(4,-1,2,0,0,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(4,-1,2,0,0,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(4,-1,2,0,0,1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(2,-1,2,0,0,1) TO C(3) 
VIBR .0, 0.00200 = O(3) TO C(5) 
VIBR .0, 0.00200 = C(5) TO C(6) 
VIBR .0, 0.00500 = O(3,-3,1,0,0,1) TO O(3) 
VIBR .0, 0.00500 = C(6) TO O(3) 
VIBR .0, 0.00500 = C(6) TO O(3,-3,1,0,0,1) 
VIBR .0, 0.00200 = C(6) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00500 = C(7,-3,1,0,0,1) TO C(5) 
VIBR .0, 0.00500 = C(7) TO C(5) 
VIBR .0, 0.00500 = C(7) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00200 = C(7) TO C(7,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(6) TO C(7,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(40) TO O(4,4,2,1,-1,-1) 
VIBR .0, 0.00200 = C(40) TO O(4) 
VIBR .0, 0.00500 = O(4) TO O(4,4,2,1,-1,-1) 
VIBR .0, 0.00200 = O(5) TO C(50) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = O(1) TO C(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(4,-1,2,0,0,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = O(3) TO C(5) 
U(IJ) .0, 0.04000 = C(5) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO C(7,-3,1,0,0,1) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-2,1,0,1,1) 
U(IJ) .0, 0.04000 = C(40) TO O(4,4,2,1,-1,-1) 
U(IJ) .0, 0.04000 = C(40) TO O(4) 
U(IJ) .0, 0.08000 = O(5) TO C(50) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;