Particle size effects in the kinetic trapping of a structurally-locked form of a flexible MOF
Linder-Patton, Oliver M.; Bloch, Witold M.; Coghlan, Campbell J.; Sumida, Kenji; Kitagawa, Susumu; Furukawa, Shuhei; Doonan, Christian J.; Sumby, Christopher J.; CrystEngComm 18 (2016) 4172–; doi:10.1039/C6CE00082G

data_7225386
_publ_section_title
;
 Particle size effects in the kinetic trapping of a structurally-locked
 form of a flexible MOF
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4172
_journal_paper_doi               10.1039/C6CE00082G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C21 H16 Cu N4 O12'
_chemical_formula_weight         579.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4000(2)
_cell_length_b                   19.5102(3)
_cell_length_c                   14.7022(2)
_cell_measurement_reflns_used    6774
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0667
_cell_measurement_theta_min      2.5006
_cell_volume                     2696.32(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'X-Seed (Barbour, 2003)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_details
;
  1 omega   65.00   94.00   1.0000   57.5300
omega____ theta____ kappa____ phi______ frames
    -       18.8463  179.0000  -30.0000 29

  2 omega  -74.00   46.00   1.0000   57.5300
omega____ theta____ kappa____ phi______ frames
    -      -19.6276    0.0000  -30.0000 120

  3 omega  -13.00   51.00   1.0000   57.5300
omega____ theta____ kappa____ phi______ frames
    -       18.8463   77.0000 -180.0000 64

  4 omega  -54.00   46.00   1.0000   57.5300
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -37.0000   60.0000 100

;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15996
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3341
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+2.7276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                2943
_reflns_number_total             3341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00082g2.cif
_cod_data_source_block           Cu-bcppm-H2O-water
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7225386