A fivefold linker length reduction in an interpenetrated metal-organic framework via sequential solvent-assisted linker exchange.
Cao, Li-Hui; Liu, Xin; Tang, Xiao-Han; Liu, Junyi; Xu, Xiao-Qian; Zang, Shuang-Quan; Ma, Yang-Min; Chemical communications (Cambridge, England) 55 (2019) 12671–12674; doi:10.1039/c9cc06739f

data_7125417
_publ_section_title
;
 A fivefold linker length reduction in an interpenetrated metal-organic
 framework via sequential solvent-assisted linker exchange.
;
_journal_issue                   84
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12671
_journal_page_last               12674
_journal_paper_doi               10.1039/c9cc06739f
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C66 H40 N2 O12 Zn3'
_chemical_formula_sum            'C66 H40 N2 O12 Zn3'
_chemical_formula_weight         1249.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-22 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.8382(4)
_cell_length_b                   28.3102(3)
_cell_length_c                   19.3354(3)
_cell_measurement_reflns_used    23168
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.1820
_cell_measurement_theta_min      2.7570
_cell_volume                     17427.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -75.00 -37.00   0.50    0.50    --   -0.90 -57.00-150.00   76
  2  \w    -13.00  29.00   0.50    0.50    --   -0.90 -57.00-150.00   84
  3  \w    -85.00  21.00   0.50    0.50    --    0.90 -82.00  90.00  212
  4  \w     22.00  81.00   0.50    0.50    --    0.90  57.00-180.00  118
  5  \w     69.00 148.00   0.50   10.00    --   98.40  77.00 -60.00  158
  6  \w    149.00 175.00   0.50   10.00    --   98.40  45.00-180.00   52
  7  \w     10.00 128.00   0.50   10.00    --   98.40 -61.00  60.00  236
  8  \w     98.00 125.00   0.50   10.00    --   98.40 -45.00 150.00   54
  9  \w     10.00 117.00   0.50   10.00    --   98.40 -82.00  60.00  214
 10  \w     26.00  62.00   0.50   10.00    --   98.40 -45.00  60.00   72
 11  \w     79.00 104.00   0.50   10.00    --   98.40 -45.00  60.00   50
 12  \w     19.00  79.00   0.50   10.00    --   98.40 -45.00 150.00  120
 13  \w     69.00 180.00   0.50   10.00    --   98.40  45.00 -90.00  222
 14  \w     74.00 152.00   0.50   10.00    --   98.40  45.00-120.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0083900000
_diffrn_orient_matrix_UB_12      -0.0249483000
_diffrn_orient_matrix_UB_13      -0.0694115000
_diffrn_orient_matrix_UB_21      0.0409933000
_diffrn_orient_matrix_UB_22      -0.0282990000
_diffrn_orient_matrix_UB_23      0.0083875000
_diffrn_orient_matrix_UB_31      -0.0243010000
_diffrn_orient_matrix_UB_32      -0.0392242000
_diffrn_orient_matrix_UB_33      0.0381883000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            79050
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        62.499
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         2.285
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_description       block
_exptl_crystal_F_000             5088
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.856
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         13924
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.1247
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.4500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4500
_refine_ls_wR_factor_ref         0.4700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10973
_reflns_number_total             13924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06739f2.cif
_cod_data_source_block           Zn-BPE
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               7125417
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.751
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C61, C64, C63, N2, C66, C65
 with sigma of 0.01
3. Rigid bond restraints
 N2, C27, C60, C61, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N2 \\sim C27 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim
C66: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C21(H21), C22(H22),
 C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58), C59(H59), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66)
;
_shelx_res_checksum              50199
_shelx_fab_checksum              90354
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.527