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_1514157
_publ_section_title
;
 The effect of pressure on the post-synthetic modification of a nanoporous
 metal-organic framework.
;
_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         'C30 H24 Cu3 O21.8.5(H2O)'
_chemical_formula_sum            'C30 H37 Cu3 O27.5'
_chemical_formula_weight         1028.24
_space_group_IT_number           164
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"'
_symmetry_space_group_name_H-M   'P -3 m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-04-29
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.623(2)
_cell_length_b                   18.623(2)
_cell_length_c                   6.8973(7)
_cell_measurement_reflns_used    1241
_cell_measurement_temperature    298
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     2071.6(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         0.1
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.099
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7248
_diffrn_reflns_theta_full        17.416
_diffrn_reflns_theta_max         23.222
_diffrn_reflns_theta_min         2.953
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.62
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
See above for details.
;
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1183
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         595
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.0004248
_refine_ls_shift/su_mean         0.0000439
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F) + ( 0.00P)^2^ + 0.13P] 
 ,where P=(max(Fo,0) + 2Fc)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1262
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0715
_reflns_limit_h_max              0
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                595
_reflns_number_total             974
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.24
_oxford_diffrn_Wilson_scale      49.06
_oxford_refine_ls_r_factor_ref   0.0630
_oxford_refine_ls_scale          0.1579(9)
_oxford_reflns_number_all        963
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'st2007 in P-3m1'
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           ST1008
_cod_original_cell_volume        2071.5(4)
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_original_sg_symbol_H-M      'P -3 m 1 '
_cod_original_formula_sum        'C30 H37 Cu3 O27.50'
_cod_database_code               1514157
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
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(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(5) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(5) 
VIBR .0, 0.00500 = C(2,5) TO C(2) 
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(6) 
VIBR .0, 0.00500 = C(3,5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3,5) 
VIBR .0, 0.00200 = C(6) TO O(4,5) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4,5) TO C(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
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(5) 
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(4) TO C(6) 
U(IJ) .0, 0.04000 = C(6) TO O(4,5) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.150000 , 0.050000 = CU(1) TO O(3) 
DISTANCE 1.950000 , 0.050000 = CU(1) TO O(1) 
DISTANCE 1.250000 , 0.050000 = O(1) TO C(1) 
DISTANCE 1.250000 , 0.050000 = C(1) TO O(2) 
DISTANCE 1.490000 , 0.050000 = C(1) TO C(2) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
DISTANCE 1.510000 , 0.050000 = C(4) TO C(6) 
DISTANCE 1.260000 , 0.050000 = C(6) TO O(4) 
DISTANCE 1.430000 , 0.050000 = O(4) TO C(7) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
ANGLE 94.800000 , 1.000000 = O(3) TO CU(1) TO O(1) 
ANGLE 123.000000 , 1.000000 = CU(1) TO O(1) TO C(1) 
ANGLE 120.000000 , 1.000000 = C(1) TO C(2) TO C(5) 
ANGLE 120.000000 , 1.000000 = C(5) TO C(2) TO C(3) 
ANGLE 120.000000 , 1.000000 = C(2) TO C(3) TO C(4) 
ANGLE 120.000000 , 1.000000 = C(3) TO C(4) TO C(6) 
ANGLE 118.000000 , 1.000000 = C(4) TO C(6) TO O(4) 
ANGLE 124.000000 , 1.000000 = C(6) TO O(4) TO C(7) 
ANGLE 118.000000 , 1.000000 = O(2) TO C(1) TO C(2) 
PLANAR 0.010000  C(1) C(2) C(5) C(3) C(4) C(6) O(4) C(7) 
END                                                                             
;