Pore modulation of zirconium-organic frameworks for high-efficiency detection of trace proteins.
Liu, Chun-Sen; Zhang, Zhi-Hong; Chen, Min; Zhao, Hui; Duan, Feng-He; Chen, Di-Ming; Wang, Ming-Hua; Zhang, Shuai; Du, Miao; Chemical communications (Cambridge, England) 53 (2017) 3941–; doi:10.1039/c7cc00029d

data_7119753
_publ_section_title
;
 Pore modulation of zirconium-organic frameworks for high-efficiency
 detection of trace proteins.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3941
_journal_paper_doi               10.1039/c7cc00029d
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         '0.13(C800 H1115 N146 O423 Zr48)'
_chemical_formula_sum            'C104 H145 N19 O55 Zr6'
_chemical_formula_weight         3088.7039
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.9025(7)
_cell_length_b                   38.9025(7)
_cell_length_c                   18.9223(11)
_cell_measurement_reflns_used    7860
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9130
_cell_measurement_theta_min      4.7170
_cell_volume                     28637.1(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3031
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -97.00   -6.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455  -19.0000   60.0000 91

  2 omega   67.00   92.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5455 -144.0000 -144.0000 25

  3 omega   37.00   98.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000 -120.0000 61

  4 omega   54.00   87.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000 -180.0000 33

  5 omega  111.00  177.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  125.0000 -120.0000 66

  6 omega   34.00   70.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000   90.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0184049000
_diffrn_orient_matrix_UB_12      0.0334677000
_diffrn_orient_matrix_UB_13      -0.0214693000
_diffrn_orient_matrix_UB_21      -0.0349199000
_diffrn_orient_matrix_UB_22      -0.0167104000
_diffrn_orient_matrix_UB_23      0.0170496000
_diffrn_orient_matrix_UB_31      0.0025898000
_diffrn_orient_matrix_UB_32      0.0130567000
_diffrn_orient_matrix_UB_33      0.0766607000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23798
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        64.995
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_min         4.133
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       Block
_exptl_crystal_F_000             8464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
TITL 20150821ZH3.res in I-42d
CELL   38.9025   38.9025   18.9223     90.00     90.00     90.00
SPGR I-42d
C101 0.507 0.641 0.296 !       2.98 eA-3
Q102 0.596 0.188 0.239 !       2.92 eA-3
Q103 0.484 0.804 0.429 !       2.30 eA-3
Q104 0.507 0.849 0.368 !       2.27 eA-3
C105 0.631 0.877 0.261 !       2.22 eA-3
Q106 0.660 0.015 0.137 !       2.21 eA-3
Q107 0.160 0.515 0.637 !       2.21 eA-3
Q108 0.662 0.984 0.109 !       2.11 eA-3
Q109 0.852 0.412 0.700 !       2.02 eA-3
Q110 0.352 0.912 0.200 !       2.02 eA-3
C111 0.041 0.812 0.331 !       1.99 eA-3
Q112 0.986 0.665 0.835 !       1.98 eA-3
C113 0.510 0.279 0.765 !       1.97 eA-3
C114 0.010 0.779 0.265 !       1.97 eA-3
Q115 0.691 0.587 0.144 !       1.96 eA-3
C116 0.996 0.726 0.093 !       1.93 eA-3
Q117 0.508 0.859 0.306 !       1.88 eA-3
Q118 1.000 0.662 0.839 !       1.87 eA-3
Q119 0.853 0.077 0.568 !       1.86 eA-3
Q120 1.002 0.352 0.824 !       1.84 eA-3
Q121 0.023 0.205 0.265 !       1.80 eA-3
C122 0.861 0.193 0.403 !       1.80 eA-3
C123 0.033 0.358 0.886 !       1.79 eA-3
C124 0.533 0.858 0.386 !       1.79 eA-3
C125 0.987 0.264 0.107 !       1.75 eA-3
Q126 0.641 0.989 0.084 !       1.73 eA-3
Q127 0.119 0.780 0.409 !       1.73 eA-3
Q128 0.619 0.280 0.909 !       1.73 eA-3
C129 0.342 0.338 0.467 !       1.73 eA-3
C130 0.960 0.963 0.486 !       1.69 eA-3
C131 0.320 0.368 0.089 !       1.69 eA-3
C132 0.571 0.197 0.420 !       1.66 eA-3
Q133 0.562 0.171 0.342 !       1.65 eA-3
C134 0.991 0.248 0.170 !       1.63 eA-3
C135 0.774 0.522 0.460 !       1.63 eA-3
C136 0.274 0.022 0.960 !       1.63 eA-3
C137 0.555 0.054 0.230 !       1.61 eA-3
C138 0.834 0.161 0.100 !       1.61 eA-3
C139 0.462 0.355 0.847 !       1.61 eA-3
C140 0.712 0.468 0.345 !       1.59 eA-3
C141 0.212 0.968 0.845 !       1.59 eA-3
C142 0.757 0.546 0.374 !       1.59 eA-3
C143 0.257 0.046 0.874 !       1.59 eA-3
Q144 0.991 0.875 0.464 !       1.58 eA-3
C145 0.867 0.866 0.409 !       1.58 eA-3
Q146 0.522 0.615 0.001 !       1.58 eA-3
C147 0.500 0.818 0.457 !       1.57 eA-3
C148 0.953 0.282 0.059 !       1.57 eA-3
C149 0.972 0.740 0.124 !       1.57 eA-3
C150 0.405 0.786 0.427 !       1.57 eA-3
C151 0.790 0.641 0.045 !       1.56 eA-3
Q152 0.362 0.843 0.265 !       1.54 eA-3
Q153 0.888 0.288 0.863 !       1.54 eA-3
Q154 0.342 0.697 0.184 !       1.54 eA-3
C155 0.568 0.249 0.458 !       1.53 eA-3
C156 0.040 0.842 0.324 !       1.52 eA-3
C157 0.540 0.342 0.824 !       1.52 eA-3
C158 0.479 0.021 0.356 !       1.51 eA-3
Q159 0.362 0.150 0.299 !       1.51 eA-3
Q160 0.662 0.953 0.132 !       1.51 eA-3
Q161 0.638 0.958 0.139 !       1.51 eA-3
Q162 0.460 0.638 0.886 !       1.51 eA-3
C163 0.113 0.836 0.455 !       1.50 eA-3
Q164 0.444 0.164 0.371 !       1.50 eA-3
Q165 0.944 0.664 0.871 !       1.50 eA-3
Q166 0.556 0.666 0.870 !       1.49 eA-3
Q167 0.892 0.185 0.407 !       1.49 eA-3
Q168 0.970 0.808 0.295 !       1.49 eA-3
C169 0.540 0.016 0.258 !       1.48 eA-3
C170 0.829 0.881 0.077 !       1.48 eA-3
Q171 0.038 0.179 0.281 !       1.47 eA-3
Q172 0.691 0.959 0.142 !       1.46 eA-3
Q173 0.073 0.868 0.471 !       1.46 eA-3
C174 0.493 0.062 0.184 !       1.46 eA-3
C175 0.903 0.565 0.698 !       1.46 eA-3
C176 0.403 0.065 0.198 !       1.46 eA-3
C177 0.852 0.172 0.048 !       1.45 eA-3
C178 0.740 0.579 0.346 !       1.45 eA-3
C179 0.240 0.079 0.846 !       1.45 eA-3
C180 0.258 0.445 0.185 !       1.44 eA-3
C181 0.827 0.310 0.172 !       1.44 eA-3
C182 0.860 0.161 0.061 !       1.44 eA-3
Q183 0.291 0.559 0.317 !       1.44 eA-3
C184 0.733 0.469 0.308 !       1.44 eA-3
Q185 0.524 0.115 0.345 !       1.43 eA-3
Q186 0.931 0.727 0.076 !       1.43 eA-3
C187 0.874 0.242 0.407 !       1.42 eA-3
C188 0.312 0.343 0.168 !       1.42 eA-3
C189 0.575 1.000 0.250 !       1.42 eA-3
C190 0.445 0.580-0.001 !       1.42 eA-3
C191 0.448 0.969 0.268 !       1.42 eA-3
C192 0.948 0.469 0.768 !       1.42 eA-3
C193 0.268 0.127 0.104 !       1.42 eA-3
C194 0.453 1.000 0.309 !       1.42 eA-3
C195 0.762 0.920 0.864 !       1.42 eA-3
C196 0.744 0.862 0.174 !       1.41 eA-3
Q197 0.840 0.951 0.694 !       1.41 eA-3
C198 0.961 0.272 0.083 !       1.41 eA-3
Q199 0.331 0.865 0.060 !       1.41 eA-3
;
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 2979 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.040(11)
_refine_ls_extinction_coef       0.000024(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10644
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1120P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9210
_reflns_number_total             10644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00029d2.cif
_cod_data_source_block           493-MOF-TATB
_cod_depositor_comments
'Adding full bibliography for 7119752--7119753.cif.'
_cod_original_cell_volume        28637.1(19)
_cod_database_code               7119753
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Zr'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(2) 0.46(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C26-C25
 1.51 with sigma of 0.01
 O7_$1-C25 = O7-C25
 1.26 with sigma of 0.01
 C30-C31 = C31-C32 = N4-C32
 1.39 with sigma of 0.01
 N4-C32 = N4-C33 = N5-C33
 1.39 with sigma of 0.01
 C32-C33
 2.38 with sigma of 0.01
 C32-N5
 2.78 with sigma of 0.01
 C33_$1-C45_$1 = C33_$1-C34_$1 = C33-C34 = C33-C45
 1.39 with sigma of 0.01
 O0AA-C46
 1.25 with sigma of 0.01
 O17-C46 = O0AA-C47
 1.24 with sigma of 0.01
 O16_$3-C46 = O16_$3-C47
 1.24 with sigma of 0.01
 C47-C42 = C46-C37
 1.51 with sigma of 0.01
 C29-C28
 1.39 with sigma of 0.01
4. Rigid bond restraints
 C26, C25, O7, O7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C38 \\sim C39 \\sim C34 \\sim C35 \\sim C36 \\sim C37: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C36 \\sim C35 \\sim C34 \\sim C39 \\sim C38 \\sim C37 \\sim C43 \\sim C44 \\sim
C45 \\sim C40 \\sim C41 \\sim C42 \\sim N4 \\sim C33 \\sim N4 \\sim C32 \\sim
N5 \\sim C33 \\sim C36 \\sim C35 \\sim C34 \\sim C39 \\sim C38 \\sim C37 \\sim
C43 \\sim C44 \\sim C45 \\sim C40 \\sim C41 \\sim C42 \\sim C29 \\sim C30 \\sim
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C27 \\sim C47 \\sim C46: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Zr3 \\sim Zr2 \\sim O11: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
6. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) O0AA(0.5) O17(0.5) C47(0.5) C46(0.5)
 C36(0.5) H36(0.5) C35(0.5) H35(0.5) C34(0.5) C39(0.5) H39(0.5) C38(0.5)
 H38(0.5) C37(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) C40(0.5)
 H40(0.5) C41(0.5) H41(0.5) C42(0.5)
7.a Me refined with riding coordinates:
 C26(H26A,H26B,H26C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C4(H4), C16(H16), C15(H15), C13(H13), C12(H12),
 C23(H23), C22(H22), C20(H20), C19(H19), C29(H29), C30(H30), C36(H36), C35(H35),
  C39(H39), C38(H38), C43(H43), C44(H44), C40(H40), C41(H41)
7.c Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4), C16(C15,C14,C13,C12,C11), C18(C23,C22,C21,C20,C19),
 C36(C35,C34,C39,C38,C37), C43(C44,C45,C40,C41,C42)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'