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_4121947
_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         'C24 H6 N3 O18 Sc2'
_chemical_formula_sum            'C24 H6 N3 O18 Sc2'
_chemical_formula_weight         714.23
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 110.632(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6860(4)
_cell_length_b                   34.208(2)
_cell_length_c                   11.0156(10)
_cell_measurement_reflns_used    2793
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     3063.1(4)
_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 0.672
_diffrn_measured_fraction_theta_max 0.636
_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  0.107
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12772
_diffrn_reflns_theta_full        17.523
_diffrn_reflns_theta_max         23.365
_diffrn_reflns_theta_min         2.575
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9628
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         1001
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.1792
_refine_ls_R_factor_gt           0.1326
_refine_ls_shift/su_max          0.0002941
_refine_ls_shift/su_mean         0.0000121
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.19 2.35 1.32 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1598
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1398
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                1001
_reflns_number_total             1422
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.69
_oxford_diffrn_Wilson_scale      129.10
_oxford_refine_ls_r_factor_ref   0.1326
_oxford_refine_ls_scale          0.1039(12)
_oxford_reflns_number_all        1414
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'Sc2NO2BDC3 in C2/c'
_cod_data_source_file            ScBDCN3.cif
_cod_data_source_block           Sc2NO2BDC3_in_MeOH_@_1.15_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_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4121947
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT SC(1, U'S) UNTIL C(12) 
CONT N(4, U[ISO]) UNTIL N(12) 
CONT O(1, U'S) UNTIL O(6) 
CONT O(7, U[ISO]) UNTIL O(12) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST   1.478,.01= C(1) TO C(2) 
DIST   1.256,.01= C(1) TO O(1) 
DIST   1.243,.01= C(1) TO O(2) 
DIST   1.335,.01= C(2) TO C(3) 
DIST   1.371,.01= C(2) TO C(4) 
DIST   1.400,.01= C(3) TO C(4,-1,2,0,1) 
DIST   1.476,.01= C(4) TO N(4) 
DIST   1.512,.01= C(5) TO C(6) 
DIST   1.240,.01= C(5) TO O(3) 
DIST   1.247,.01= C(5) TO O(4) 
DIST   1.388,.01= C(6) TO C(7) 
DIST   1.373,.01= C(6) TO C(8) 
DIST   1.381,.01= C(7) TO C(8,2,1,1,0,1) 
DIST   1.508,.01= C(8) TO N(8) 
DIST   1.496,.01= C(9) TO C(10) 
DIST   1.250,.01= C(9) TO O(5) 
DIST   1.243,.01= C(9) TO O(6) 
DIST   1.362,.01= C(10) TO C(11) 
DIST   1.371,.01= C(10) TO C(12) 
DIST   1.397,.01= C(11) TO C(12,-1,1,0,1) 
DIST   1.423,.01= C(12) TO N(12) 
DIST   1.230,.01= N(4) TO O(7) 
DIST   1.230,.01= N(4) TO O(8) 
DIST   1.234,.01= N(8) TO O(9) 
DIST   1.223,.01= N(8) TO O(10) 
DIST   1.219,.01= N(12) TO O(11) 
DIST   1.227,.01= N(12) TO O(12) 
ANGL 118,1= O(1) TO C(1) TO C(2) 
ANGL 118,1= O(2) TO C(1) TO C(2) 
ANGL 124,1= O(2) TO C(1) TO O(1) 
ANGL 119,1= C(3) TO C(2) TO C(1) 
ANGL 123,1= C(4) TO C(2) TO C(1) 
ANGL 118,1= C(4) TO C(2) TO C(3) 
ANGL 121,1= C(4,-1,2,0,1) TO C(3) TO C(2) 
ANGL 121,1= C(3,-1,2,0,1) TO C(4) TO C(2) 
ANGL 123,1= N(4) TO C(4) TO C(2) 
ANGL 116,1= N(4) TO C(4) TO C(3,-1,2,0,1) 
ANGL 118,1= O(3) TO C(5) TO C(6) 
ANGL 117,1= O(4) TO C(5) TO C(6) 
ANGL 125,1= O(4) TO C(5) TO O(3) 
ANGL 119,1= C(7) TO C(6) TO C(5) 
ANGL 121,1= C(8) TO C(6) TO C(5) 
ANGL 119,1= C(8) TO C(6) TO C(7) 
ANGL 119,1= C(8,2,1,1,0,1) TO C(7) TO C(6) 
ANGL 121,1= C(7,2,1,1,0,1) TO C(8) TO C(6) 
ANGL 125,1= N(8) TO C(8) TO C(6) 
ANGL 113,1= N(8) TO C(8) TO C(7,2,1,1,0,1) 
ANGL 118,1= O(5) TO C(9) TO C(10) 
ANGL 119,1= O(6) TO C(9) TO C(10) 
ANGL 124,1= O(6) TO C(9) TO O(5) 
ANGL 120,1= C(11) TO C(10) TO C(9) 
ANGL 121,1= C(12) TO C(10) TO C(9) 
ANGL 119,1= C(12) TO C(10) TO C(11) 
ANGL 122,1= C(12,-1,1,0,1) TO C(11) TO C(10) 
ANGL 119,1= C(11,-1,1,0,1) TO C(12) TO C(10) 
ANGL 125,1= N(12) TO C(12) TO C(10) 
ANGL 115,1= N(12) TO C(12) TO C(11,-1,1,0,1) 
ANGL 118,1= O(7) TO N(4) TO C(4) 
ANGL 118,1= O(8) TO N(4) TO C(4) 
ANGL 124,1= O(8) TO N(4) TO O(7) 
ANGL 118,1= O(9) TO N(8) TO C(8) 
ANGL 118,1= O(10) TO N(8) TO C(8) 
ANGL 125,1= O(10) TO N(8) TO O(9) 
ANGL 117,1= O(11) TO N(12) TO C(12) 
ANGL 118,1= O(12) TO N(12) TO C(12) 
ANGL 124,1= O(12) TO N(12) TO O(11) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
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(4) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(4) TO C(1) 
VIBR .0, 0.00500 = C(4) TO C(3) 
VIBR .0, 0.00200 = C(3) TO C(4,-1,2,0,1) 
VIBR .0, 0.00500 = C(2) TO C(4,-1,2,0,1) 
VIBR .0, 0.00500 = C(2) TO C(3,-1,2,0,1) 
VIBR .0, 0.00200 = C(5) TO C(6) 
VIBR .0, 0.00200 = C(5) TO O(3) 
VIBR .0, 0.00200 = C(5) TO O(4) 
VIBR .0, 0.00500 = O(3) TO C(6) 
VIBR .0, 0.00500 = O(4) TO C(6) 
VIBR .0, 0.00500 = O(4) TO O(3) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00200 = C(6) TO C(8) 
VIBR .0, 0.00500 = C(7) TO C(5) 
VIBR .0, 0.00500 = C(8) TO C(5) 
VIBR .0, 0.00500 = C(8) TO C(7) 
VIBR .0, 0.00200 = C(7) TO C(8,2,1,1,0,1) 
VIBR .0, 0.00500 = C(8,2,1,1,0,1) TO C(6) 
VIBR .0, 0.00500 = C(6) TO C(7,2,1,1,0,1) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00200 = C(9) TO O(5) 
VIBR .0, 0.00200 = C(9) TO O(6) 
VIBR .0, 0.00500 = O(5) TO C(10) 
VIBR .0, 0.00500 = O(6) TO C(10) 
VIBR .0, 0.00500 = O(6) TO O(5) 
VIBR .0, 0.00200 = C(10) TO C(11) 
VIBR .0, 0.00200 = C(10) TO C(12) 
VIBR .0, 0.00500 = C(11) TO C(9) 
VIBR .0, 0.00500 = C(12) TO C(9) 
VIBR .0, 0.00500 = C(12) TO C(11) 
VIBR .0, 0.00200 = C(11) TO C(12,-1,1,0,1) 
VIBR .0, 0.00500 = C(10) TO C(12,-1,1,0,1) 
VIBR .0, 0.00500 = C(10) TO C(11,-1,1,0,1) 
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(4) 
U(IJ) .0, 0.04000 = C(3) TO C(4,-1,2,0,1) 
U(IJ) .0, 0.04000 = C(5) TO C(6) 
U(IJ) .0, 0.08000 = C(5) TO O(3) 
U(IJ) .0, 0.08000 = C(5) TO O(4) 
U(IJ) .0, 0.04000 = C(6) TO C(7) 
U(IJ) .0, 0.04000 = C(6) TO C(8) 
U(IJ) .0, 0.04000 = C(7) TO C(8,2,1,1,0,1) 
U(IJ) .0, 0.04000 = C(9) TO C(10) 
U(IJ) .0, 0.08000 = C(9) TO O(5) 
U(IJ) .0, 0.08000 = C(9) TO O(6) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.04000 = C(10) TO C(12) 
U(IJ) .0, 0.04000 = C(11) TO C(12,-1,1,0,1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(4) TO O(7) 
VIBR .0, 0.00200 = N(4) TO O(8) 
VIBR .0, 0.00500 = O(8) TO O(7) 
VIBR .0, 0.00200 = N(8) TO O(9) 
VIBR .0, 0.00200 = N(8) TO O(10) 
VIBR .0, 0.00500 = O(10) TO O(9) 
VIBR .0, 0.00200 = N(12) TO O(11) 
VIBR .0, 0.00200 = N(12) TO O(12) 
VIBR .0, 0.00500 = O(12) TO O(11) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.08000 = N(4) TO O(7) 
U(IJ) .0, 0.08000 = N(4) TO O(8) 
U(IJ) .0, 0.08000 = N(8) TO O(9) 
U(IJ) .0, 0.08000 = N(8) TO O(10) 
U(IJ) .0, 0.08000 = N(12) TO O(11) 
U(IJ) .0, 0.08000 = N(12) TO O(12) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;