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_1514153
_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 O21.2CH3OH'
_chemical_formula_sum            'C35 H38 Cu3 O23'
_chemical_formula_weight         981.27
_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                   18.6631(14)
_cell_length_b                   18.6631(14)
_cell_length_c                   6.9006(5)
_cell_measurement_reflns_used    2252
_cell_measurement_temperature    293
_cell_measurement_theta_max      15
_cell_measurement_theta_min      2
_cell_volume                     2081.5(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 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 0.781
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Rigaku Saturn 724+'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -16
_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            11549
_diffrn_reflns_theta_full        15.408
_diffrn_reflns_theta_max         15.723
_diffrn_reflns_theta_min         1.492
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
see above for details
;
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1519
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         664
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.0008504
_refine_ls_shift/su_mean         0.0000396
_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: 
 0.288 0.159 0.898E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0742
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0467
_reflns_limit_h_max              0
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                664
_reflns_number_total             876
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0407
_oxford_refine_ls_scale          0.1270(5)
_oxford_reflns_number_all        871
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c3nr04161a2.cif
_cod_data_source_block           st1004
_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_sg_symbol_H-M      'P -3 m 1 '
_cod_database_code               1514153
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE O   (   4,X'S) H   (   4,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 0.82, 0.01 = O(4) TO H(4) 
DIST   1.489,.01= C(1) TO C(2) 
DIST   1.252,.01= C(1) TO O(1) 
DIST   1.252,.01= C(1) TO O(1,6,1,1,1) 
DIST   1.388,.01= C(2) TO C(3) 
DIST   1.388,.01= C(2) TO C(3,6,1,1,1) 
DIST   1.389,.01= C(3) TO C(4) 
DIST   1.392,.01= C(4) TO C(5) 
DIST   1.495,.01= C(4) TO C(6) 
DIST   1.248,.01= C(6) TO O(2) 
DIST   1.248,.01= C(6) TO O(3) 
DIST   1.420,.01= C(7) TO O(1) 
DIST   1.383,.01= C(8) TO O(4) 
ANGL 118,1= O(1) TO C(1) TO C(2) 
ANGL 118,1= O(1,6,1,1,1) TO C(1) TO C(2) 
ANGL 125,1= O(1,6,1,1,1) TO C(1) TO O(1) 
ANGL 120,1= C(3) TO C(2) TO C(1) 
ANGL 120,1= C(3,6,1,1,1) TO C(2) TO C(1) 
ANGL 120,1= C(3,6,1,1,1) 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 120,1= C(6) TO C(4) TO C(3) 
ANGL 120,1= C(6) TO C(4) TO C(5) 
ANGL 120,1= C(4,6,1,1,1) TO C(5) TO C(4) 
ANGL 117,1= O(2) TO C(6) TO C(4) 
ANGL 117,1= O(3) TO C(6) TO C(4) 
ANGL 125,1= O(3) TO C(6) TO O(2) 
ANGL 126,1= C(7) TO O(1) TO C(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, 0.00200 = C(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00500 = C(2) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(1) TO O(1,6,1,1,1) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00200 = C(2) TO C(3,6,1,1,1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3,6,1,1,1) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00500 = C(3) TO C(3,6,1,1,1) 
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(4,6,1,1,1) TO C(4) 
VIBR .0, 0.00200 = C(6) TO O(2) 
VIBR .0, 0.00200 = C(6) TO O(3) 
VIBR .0, 0.00500 = O(2) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO O(2) 
VIBR .0, 0.00200 = C(7) TO O(1) 
VIBR .0, 0.00200 = C(8) TO O(4) 
VIBR .0, 0.00500 = C(1) TO C(7) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO O(1,6,1,1,1) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.04000 = C(1) TO O(1) 
U(IJ) .0, 0.04000 = C(2) TO C(3,6,1,1,1) 
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) 
U(IJ) .0, 0.08000 = C(6) TO O(2) 
U(IJ) .0, 0.08000 = C(6) TO O(3) 
U(IJ) .0, 0.08000 = C(7) TO O(1) 
U(IJ) .0, 0.08000 = C(8) TO O(4) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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