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_1514158
_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         'C32.00 H25.00 Cu3 N1.00 O20.00.2.5(CH3CN)'
_chemical_formula_sum            'C37 H32.5 Cu3 N3.5 O20'
_chemical_formula_weight         1036.805
_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             13-05-10
_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                   18.5488(13)
_cell_length_b                   18.5488(13)
_cell_length_c                   6.9375(4)
_cell_measurement_reflns_used    1372
_cell_measurement_temperature    298
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     2067.1(2)
_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         0.3
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.769
_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  0.108
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6642
_diffrn_reflns_theta_full        15.612
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         3.199
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.62
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1052.00
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
see above for details 
;
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9979
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         449
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.0001632
_refine_ls_shift/su_mean         0.0000079
_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: 
 0.723 0.165 0.128 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0994
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0654
_reflns_limit_h_max              0
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              0
_reflns_number_gt                449
_reflns_number_total             626
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.60
_oxford_diffrn_Wilson_scale      129.17
_oxford_refine_ls_r_factor_ref   0.0558
_oxford_refine_ls_scale          0.1364(10)
_oxford_reflns_number_all        608
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'st2016 in P-3m1'
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           ST1009
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_original_sg_symbol_H-M      'P -3 m 1 '
_cod_original_formula_sum        'C37 H32.50 Cu3 N3.50 O20.00'
_cod_database_code               1514158
_iucr_refine_instruction_details_constraints
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BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S) 
CONT N    (    1 ,X'S,U[ISO]) 
CONT O    (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO]) 
CONT O    (    4 ,X'S,U'S)  UNTIL C    (    7 ) 
CONT C    (    8 ,X'S,U[ISO])  UNTIL C    (    9 ) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
DISTANCE 1.450000 , 0.050000 = C(9) TO C(8) 
DISTANCE 1.130000 , 0.050000 = N(1) TO C(8) 
DISTANCE 2.180000 , 0.050000 = CU(1) TO N(1) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(71) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(72) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(3) 
ANGLE 170.000000 , 1.000000 = CU(1) TO N(1) TO C(8) 
ANGLE 90.000000 , 1.000000 = N(1) TO CU(1) TO O(1) 
ANGLE 180.000000 , 1.000000 = N(1) TO C(8) TO C(9) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(92) 
ANGLE 110.000000 , 1.000000 = C(8) TO C(9) TO H(91) 
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, 0.00500 = O(3) TO N(1) 
VIBR .0, 0.00500 = O(1) TO N(1) 
VIBR .0, 0.00500 = O(1) TO O(3) 
VIBR .0, 0.00200 = N(1) TO C(8) 
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, 0.00200 = 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(6) TO C(3) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00500 = O(4) TO C(4) 
VIBR .0, 0.00200 = O(4) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(6) 
VIBR .0, 0.00200 = C(9) TO C(8) 
VIBR .0, 0.00500 = N(1) TO C(9) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(1) TO C(8) 
U(IJ) .0, 0.04000 = O(1) TO C(1) 
U(IJ) .0, 0.04000 = 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(4,4,1,1) 
U(IJ) .0, 0.04000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = O(4) TO C(7) 
U(IJ) .0, 0.08000 = C(9) TO C(8) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 0.950000 , 0.050000 = C(7) TO H(73) 
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(9) TO H(91) 
DISTANCE 0.950000 , 0.050000 = C(9) TO H(92) 
DISTANCE 1.400000 , 0.050000 = C(2) TO C(5) 
DISTANCE 1.400000 , 0.050000 = C(3) TO C(4) 
END                                                                             
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