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_1514159
_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         'C32.00 H24 Cu3 N1.00 O20.00.1.5(CH3CN)'
_chemical_formula_sum            'C35 H31 Cu3 N2.5 O21'
_chemical_formula_weight         992.235
_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             12-10-30
_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                   18.5877(5)
_cell_length_b                   18.5877(5)
_cell_length_c                   6.8740(2)
_cell_measurement_reflns_used    3570
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2056.80(10)
_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_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.118
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20617
_diffrn_reflns_theta_full        26.394
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         1.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.62
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1004.00
_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         1.91
_refine_diff_density_min         -1.99
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9830
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1542
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.0004673
_refine_ls_shift/su_mean         0.0000245
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +15.03P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1599
_reflns_limit_h_max              0
_reflns_limit_h_min              -19
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1159
_reflns_number_total             1553
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.07
_oxford_diffrn_Wilson_scale      111.54
_oxford_refine_ls_r_factor_ref   0.0798
_oxford_refine_ls_scale          0.14163(18)
_oxford_reflns_number_all        1542
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ST2019 in P-3m1'
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           ST1010
_cod_original_sg_symbol_Hall     '-P 3 2'
_cod_original_sg_symbol_H-M      'P -3 m 1 '
_cod_original_formula_sum        'C35 H31.00 Cu3 N2.50 O21'
_cod_database_code               1514159
_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
;
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(73) 
DISTANCE 2.000000 , 0.050000 = CU(1) TO N(1) 
DISTANCE 0.780000 , 0.050000 = O(3) TO H(101) 
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) 
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) 
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 = N(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = N(1) TO O(2,-1,1,1,1,2) 
VIBR .0, 0.00500 = N(1) TO O(2,-6,1,0,0,2) 
VIBR .0, 0.00500 = O(3) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(3) TO O(2,-1,1,1,1,2) 
VIBR .0, 0.00500 = O(3) TO O(2,-6,1,0,0,2) 
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 = 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 = 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, 0.04000 = N(1) TO C(8) 
U(IJ) .0, 0.08000 = C(9) TO C(8) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
VIBRATION 0.0, 0.020000 = O(4) TO C(7) 
VIBRATION 0.0, 0.020000 = C(6) TO C(7) 
VIBRATION 0.0, 0.020000 = C(4) TO O(4) 
END                                                                             
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