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_1514164
_publ_section_title
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 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 .2CH3CHO'
_chemical_formula_sum            'C34 H32 Cu3 O23'
_chemical_formula_weight         999.24
_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                   17.991(3)
_cell_length_b                   17.991(3)
_cell_length_c                   6.5371(11)
_cell_measurement_reflns_used    582
_cell_measurement_temperature    300
_cell_measurement_theta_max      16
_cell_measurement_theta_min      3
_cell_volume                     1832.4(5)
_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         3.0
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.908
_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  0.159
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4194
_diffrn_reflns_theta_full        13.073
_diffrn_reflns_theta_max         17.202
_diffrn_reflns_theta_min         3.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.82
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1014.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
See above for details
;
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1803
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         237
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.1868
_refine_ls_R_factor_gt           0.1204
_refine_ls_shift/su_max          0.0093316
_refine_ls_shift/su_mean         0.0011208
_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: 
 1.25 0.335 0.599 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2319
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1342
_reflns_limit_h_max              0
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              5
_reflns_limit_l_min              0
_reflns_number_gt                237
_reflns_number_total             389
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.04
_oxford_diffrn_Wilson_scale      54.73
_oxford_refine_ls_r_factor_ref   0.1204
_oxford_refine_ls_scale          0.163(3)
_oxford_reflns_number_all        379
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'ST2044 in P-3m1'
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           ST1015
_cod_original_cell_volume        1832.5(5)
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_original_sg_symbol_H-M      'P -3 m 1 '
_cod_original_formula_sum        'C34 H32.00 Cu3 O23.00'
_cod_database_code               1514164
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT O    (    1 ,X'S,U[ISO])  UNTIL C    (    7 ) 
END                                                                             
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_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 = O(2) TO C(1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(2) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00200 = C(2) TO C(5) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(1) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = O(4) TO C(6) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00200 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4,5,1,0,1) 
VIBR .0, 0.00500 = C(4) TO O(4) 
VIBR .0, 0.00500 = C(2,5,1,0,1) TO C(2) 
VIBR .0, 0.00500 = C(3) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(6) 
VIBR .0, 0.00500 = C(3,5,1,0,1) TO C(3) 
VIBR .0, 0.00200 = C(7) TO C(7,-4,1,1,2,-1) 
VIBR .0, 0.00500 = O(4) TO C(7,-4,1,1,2,-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 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(2) TO C(5) 
U(IJ) .0, 0.04000 = O(4) TO C(6) 
U(IJ) .0, 0.04000 = O(4) TO C(7) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(6) TO C(4) 
U(IJ) .0, 0.04000 = C(7) TO C(7,-4,1,1,2,-1) 
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                                                                             
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