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_1514151
_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         'C33 H30 Cu3 O21.1.5CH3OH'
_chemical_formula_sum            'C34.5 H36 Cu3 O22.5'
_chemical_formula_weight         1001.28
_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     other
_audit_creation_date             12-10-02
_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                   18.695(3)
_cell_length_b                   18.695(3)
_cell_length_c                   6.9489(9)
_cell_measurement_reflns_used    1422
_cell_measurement_temperature    293
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2103.3(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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.880
_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  0.119
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4723
_diffrn_reflns_theta_full        15.812
_diffrn_reflns_theta_max         20.805
_diffrn_reflns_theta_min         3.190
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.59
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
see above for details
;
_refine_diff_density_max         1.91
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         467
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.0001609
_refine_ls_shift/su_mean         0.0000194
_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: 
 0.882 0.459 0.520 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1452
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0797
_reflns_limit_h_max              0
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              0
_reflns_number_gt                467
_reflns_number_total             725
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.71
_oxford_diffrn_Wilson_scale      111.94
_oxford_refine_ls_r_factor_ref   0.0730
_oxford_refine_ls_scale          0.1329(11)
_oxford_reflns_number_all        685
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           ST1002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2103.2(5)
_cod_original_sg_symbol_H-M      'P -3 m 1 '
_cod_original_formula_sum        'C34.5 H36 Cu3 O22.5 '
_cod_database_code               1514151
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT CU(1, U'S) UNTIL C(8) 
CONT H(4, X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 0.84, 0.01 = O(4) TO H(4) 
DIST   1.39, 0.01 = O(4) TO C(8) 
DIST   1.39, 0.01 = O(5) TO C(9) 
DIST   1.258,.01= O(1) TO C(1) 
DIST   1.430,.01= O(1) TO C(7) 
DIST   1.265,.01= O(2) TO C(6) 
DIST   1.261,.01= O(3) TO C(6) 
DIST   1.499,.01= C(1) TO C(2) 
DIST   1.395,.01= C(2) TO C(3) 
DIST   1.395,.01= C(2) TO C(3,4,1,1) 
DIST   1.399,.01= C(3) TO C(4) 
DIST   1.399,.01= C(4) TO C(5) 
DIST   1.503,.01= C(4) TO C(6) 
ANGL 125,1= C(7) TO O(1) TO C(1) 
ANGL 124,1= O(1,4,1,1) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1) 
ANGL 118,1= C(2) TO C(1) TO O(1,4,1,1) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,4,1,1) TO C(2) TO C(1) 
ANGL 120,1= C(3,4,1,1) TO C(2) TO C(3) 
ANGL 120,1= C(4) TO C(3) TO C(2) 
ANGL 120,1= C(5) TO C(4) TO C(3) 
ANGL 121,1= C(6) TO C(4) TO C(3) 
ANGL 119,1= C(6) TO C(4) TO C(5) 
ANGL 120,1= C(4,4,1,1) TO C(5) TO C(4) 
ANGL 126,1= O(3) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(2) 
ANGL 117,1= C(4) TO C(6) TO O(3) 
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(1) TO C(7) 
VIBR .0, 0.00500 = C(7) TO C(1) 
VIBR .0, 0.00200 = O(2) TO C(6) 
VIBR .0, 0.00200 = O(3) TO C(6) 
VIBR .0, 0.00200 = O(4) TO C(8) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00500 = O(1) TO O(1,4,1,1) 
VIBR .0, 0.00500 = C(2) TO O(1,4,1,1) 
VIBR .0, 0.00500 = C(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3,4,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,4,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,4,1,1) 
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(5) 
VIBR .0, 0.00200 = C(4) TO C(6) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(3) 
VIBR .0, 0.00500 = C(6) TO C(5) 
VIBR .0, 0.00500 = C(4) TO C(4,4,1,1) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(2) TO O(3) 
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, 0.08000 = O(1) TO C(7) 
U(IJ) .0, 0.08000 = O(2) TO C(6) 
U(IJ) .0, 0.08000 = O(3) TO C(6) 
U(IJ) .0, 0.08000 = O(4) TO C(8) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3,4,1,1) 
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(5) 
U(IJ) .0, 0.04000 = C(4) TO C(6) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
VIBRATION 0.0, 0.020000 = O(5) TO C(9) 
U(IJ)'S  0.0, 0.010000 = O(5) TO C(9) 
END                                                                             
;