The effect of pressure on the post-synthetic modification of a nanoporous metal-organic framework.
McKellar, Scott C.; Graham, Alexander J.; Allan, David R.; Mohideen, M Infas H; Morris, Russell E.; Moggach, Stephen A.; Nanoscale 6 (2014) 4163–4173; doi:10.1039/c3nr04161a

data_1514166
_publ_section_title
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 The effect of pressure on the post-synthetic modification of a nanoporous
 metal-organic framework.
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_journal_issue                   8
_journal_name_full               Nanoscale
_journal_page_first              4163
_journal_page_last               4173
_journal_paper_doi               10.1039/c3nr04161a
_journal_volume                  6
_journal_year                    2014
_chemical_formula_moiety         'C18 H12 Cu3 O15 .13(H2O)'
_chemical_formula_sum            'C18 H38 Cu3 O28'
_chemical_formula_weight         890.813
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-06-03
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.370(3)
_cell_length_b                   26.370(3)
_cell_length_c                   26.370(3)
_cell_measurement_reflns_used    1060
_cell_measurement_temperature    298
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     18337(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         0.2
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.972
_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  0.188
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       3
_diffrn_reflns_number            5734
_diffrn_reflns_theta_full        16.666
_diffrn_reflns_theta_max         18.938
_diffrn_reflns_theta_min         3.090
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.46
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7292
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
see above for details
;
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0750
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         289
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0006501
_refine_ls_shift/su_mean         0.0000481
_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: 
 0.615 0.490 0.375 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0869
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0556
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              3
_reflns_number_gt                289
_reflns_number_total             411
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.56
_oxford_diffrn_Wilson_scale      3904.34
_oxford_refine_ls_r_factor_ref   0.0510
_oxford_refine_ls_scale          0.02201(17)
_oxford_reflns_number_all        405
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'ST2010_reprocess in Fm-3m'
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           HK1002
_cod_original_sg_symbol_H-M      'F m -3 m '
_cod_database_code               1514166
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
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(2) TO C(1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(2,-16,1,1,1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2,-16,1,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3,-6,3,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,-6,3,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,-6,3,1,1) 
VIBR .0, 0.00500 = C(2,11,2,1,-1,1) TO C(2) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(2) TO C(1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3,-6,3,1,1) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
END                                                                             
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