Pore Shape Modification of a Microporous Metal‒Organic Framework Using High Pressure: Accessing a New Phase with Oversized Guest Molecules
McKellar, Scott C.; Sotelo, Jorge; Greenaway, Alex; Mowat, John P. S.; Kvam, Odin; Morrison, Carole A.; Wright, Paul A.; Moggach, Stephen A.; Chemistry of Materials 28 (2016) 466–; doi:10.1021/acs.chemmater.5b02891

data_4003201
_publ_section_title
;
 Pore Shape Modification of a Microporous Metal--Organic Framework Using
 High Pressure: Accessing a New Phase with Oversized Guest Molecules
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              466
_journal_paper_doi               10.1021/acs.chemmater.5b02891
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         'C28.50 H12 O12 Sc2'
_chemical_formula_sum            'C28.5 H12 O12 Sc2'
_chemical_formula_weight         636.31
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      70
_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             15-06-08
_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                   8.779(3)
_cell_length_b                   20.742(3)
_cell_length_c                   34.287(7)
_cell_measurement_reflns_used    1723
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     6243(3)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         200000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.719
_diffrn_measured_fraction_theta_max 0.671
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.090
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            4145
_diffrn_reflns_theta_full        17.426
_diffrn_reflns_theta_max         23.234
_diffrn_reflns_theta_min         3.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.60
_refine_ls_extinction_coef       8.524
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8839
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         753
_refine_ls_number_restraints     149
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.0012940
_refine_ls_shift/su_mean         0.0000277
_refine_ls_structure_factor_coef Fsqd
_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: 
 9.42 12.3 6.05 1.84 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1602
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1602
_reflns_limit_h_max              6
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                530
_reflns_number_total             760
_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   0.0973
_oxford_refine_ls_scale          0.04993(3)
_oxford_reflns_number_all        753
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'ST2135s in Fddd'
_cod_data_source_file            cm5b02891_si_003.cif
_cod_data_source_block           SC2BDC3_np_I
_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/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6244(2)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C28.50 H12 O12 Sc2'
_cod_database_code               4003201
_iucr_refine_instruction_details_constraints
;
BLOCK X'S 
CONT SCALE 
CONT SC   (1 ,U'S)  UNTIL C(8) 
CONT C (10, U[ISO]) UNTIL C(14) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
DIST 1.39, 0.01 = C(6) TO C(7), C(7) TO C(8) 
CONT              C(8) TO C(6,4,2,0,0,-1) 
PLANAR 0.010000  C(6) C(7) C(8) C(6,4,2,0,0,-1) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = O(1) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(1) 
VIBR .0, 0.00200 = O(3) TO C(5) 
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,-1,4,0,0,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(4,-1,4,0,0,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(4,-1,4,0,0,1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(2,-1,4,0,0,1) TO C(3) 
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(8,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(6) TO C(8,4,2,0,0,-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(8,-2,1,0,1,1) TO C(5) 
VIBR .0, 0.00500 = C(8,4,2,0,0,-1) TO C(5) 
VIBR .0, 0.00500 = C(8,4,2,0,0,-1) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7,-3,1,0,0,1) TO C(5) 
VIBR .0, 0.00500 = C(7,-3,1,0,0,1) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7,-3,1,0,0,1) TO C(8,4,2,0,0,-1) 
VIBR .0, 0.00500 = C(7) TO C(5) 
VIBR .0, 0.00500 = C(7) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7) TO C(8,4,2,0,0,-1) 
VIBR .0, 0.00500 = C(7) TO C(7,-3,1,0,0,1) 
VIBR .0, 0.00200 = C(7) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00500 = C(8,-2,1,0,1,1) TO C(6) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00500 = C(8) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00200 = C(8) TO C(8,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7) TO C(6,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(8,-2,1,0,1,1) TO C(6,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(8,-2,1,0,1,1) TO C(7) 
VIBR .0, 0.00500 = C(7,-2,1,0,1,1) TO C(6,-2,1,0,1,1) 
VIBR .0, 0.00500 = C(7,-2,1,0,1,1) TO C(7) 
VIBR .0, 0.00500 = C(7,-2,1,0,1,1) TO C(8,-2,1,0,1,1) 
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 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = O(3) TO C(5) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(4,-1,4,0,0,1) 
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 = C(5) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO C(8,-2,1,0,1,1) 
U(IJ) .0, 0.04000 = C(6) TO C(8,4,2,0,0,-1) 
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(8,-2,1,0,1,1) 
U(IJ) .0, 0.04000 = C(7) TO C(8) 
U(IJ) .0, 0.04000 = C(8) TO C(8,-2,1,0,1,1) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.40000 , 0.010000 = C(13) TO C(7,-2,2) 
U(IJ) .0, 0.04000 = C(10) TO C(11) 
U(IJ) .0, 0.04000 = C(11) TO C(12) 
U(IJ) .0, 0.04000 = C(12) TO C(13) 
U(IJ) .0, 0.04000 = C(13) TO C(14) 
U(IJ) .0, 0.04000 = C(14) TO C(15) 
U(IJ) .0, 0.04000 = C(15) TO C(15,-1,4) 
VIBRATION 0.0, 0.020000 = C(10) TO C(11) 
VIBRATION 0.0, 0.020000 = C(11) TO C(12) 
VIBRATION 0.0, 0.020000 = C(12) TO C(13) 
VIBRATION 0.0, 0.020000 = C(13) TO C(14) 
VIBRATION 0.0, 0.020000 = C(14) TO C(15) 
VIBRATION 0.0, 0.020000 = C(15) TO C(15,-1,4) 
DISTANCE 1.540000 , 0.010000 = C(10) TO C(11) 
DISTANCE 1.540000 , 0.010000 = C(11) TO C(12) 
DISTANCE 1.540000 , 0.010000 = C(12) TO C(13) 
DISTANCE 1.540000 , 0.010000 = C(13) TO C(14) 
DISTANCE 1.540000 , 0.010000 = C(14) TO C(15) 
DISTANCE 1.540000 , 0.010000 = C(15) TO C(15,-1,4) 
ANGLE 113.000000 , 1.000000 = C(11,-2) TO C(10) TO C(11) 
ANGLE 113.000000 , 1.000000 = C(10) TO C(11) TO C(12) 
ANGLE 113.000000 , 1.000000 = C(11) TO C(12) TO C(13) 
ANGLE 113.000000 , 1.000000 = C(12) TO C(13) TO C(14) 
ANGLE 113.000000 , 1.000000 = C(13) TO C(14) TO C(15) 
ANGLE 113.000000 , 1.000000 = C(14) TO C(15) TO C(15,-1,4) 
END                                                                             
;