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_7119752
_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(C808 H1282 N169 O400 Zr48)'
_chemical_formula_sum            'C105 H168 N22 O52 Zr6'
_chemical_formula_weight         3117.9185
_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   mixed
_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                   38.8511(3)
_cell_length_b                   38.8511(3)
_cell_length_c                   18.7521(8)
_cell_measurement_reflns_used    5332
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8310
_cell_measurement_theta_min      3.5900
_cell_volume                     28304.6(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -77.00  -50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -180.0000 27

  2 omega  -64.00  -37.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 27

  3 omega  -77.00  -51.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   90.0000 26

  4 omega  -14.00   38.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0974  -57.0000    0.0000 52

  5 omega   38.00   66.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0974   57.0000 -180.0000 28

  6 omega   42.00  116.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0974   57.0000 -150.0000 74

  7 omega   37.00   89.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -25.0000  150.0000 52

  8 omega   62.00   93.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -25.0000    0.0000 31

  9 omega   62.00   93.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -50.0000   90.0000 31

 10 omega   40.00   79.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -37.0000  -90.0000 39

 11 omega   94.00  158.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947   50.0000 -180.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0061227000
_diffrn_orient_matrix_UB_12      0.0249212000
_diffrn_orient_matrix_UB_13      -0.0626277000
_diffrn_orient_matrix_UB_21      0.0390435000
_diffrn_orient_matrix_UB_22      -0.0013120000
_diffrn_orient_matrix_UB_23      0.0141169000
_diffrn_orient_matrix_UB_31      0.0032710000
_diffrn_orient_matrix_UB_32      -0.0307847000
_diffrn_orient_matrix_UB_33      -0.0513377000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         3.217
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_F_000             7456
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
TITL 1 in I-42d
CELL   38.8511   38.8511   18.7521     90.00     90.00     90.00
SPGR I-42d
C101 0.586 0.485 0.108 !       2.28 eA-3
C102 0.345 0.249 0.279 !       2.21 eA-3
C103 0.326 0.624 0.438 !       2.07 eA-3
Q104 0.789 0.912 0.154 !       2.04 eA-3
Q105 0.547 0.722 0.356 !       1.98 eA-3
Q106 0.047 0.222 0.856 !       1.98 eA-3
C107 0.364 0.226 0.297 !       1.97 eA-3
C108 0.860 0.828 0.418 !       1.91 eA-3
Q109 0.547 0.791 0.872 !       1.89 eA-3
Q110 0.602 0.728 0.330 !       1.88 eA-3
C111 0.369 0.262 0.313 !       1.87 eA-3
C112 0.024 0.291 0.464 !       1.85 eA-3
C113 0.790 0.009 0.217 !       1.84 eA-3
C114 0.265 0.627 0.126 !       1.82 eA-3
Q115 0.587 0.008 0.093 !       1.80 eA-3
C116 0.697 0.257 0.093 !       1.79 eA-3
C117 0.782 0.530 0.017 !       1.73 eA-3
C118 0.334 0.226 0.283 !       1.73 eA-3
C119 0.141 0.236 0.420 !       1.69 eA-3
C120 0.670 0.765 0.128 !       1.67 eA-3
C121 0.273 0.823 0.154 !       1.67 eA-3
C122 0.356 0.227 0.048 !       1.67 eA-3
C123 0.336 0.662 0.046 !       1.58 eA-3
C124 0.023 0.717 0.436 !       1.58 eA-3
C125 0.155 0.182 0.401 !       1.57 eA-3
Q126 0.835 0.408 0.280 !       1.57 eA-3
C127 0.344 0.356 0.920 !       1.56 eA-3
C128 0.844 0.856 0.420 !       1.56 eA-3
Q129 0.493 0.360 0.421 !       1.56 eA-3
C130 0.368 0.224 0.411 !       1.55 eA-3
C131 0.482 0.216 0.032 !       1.55 eA-3
C132 0.991 0.282 0.503 !       1.55 eA-3
C133 0.491 0.782 0.003 !       1.55 eA-3
C134 0.125 0.848 0.096 !       1.51 eA-3
C135 0.695 0.839 0.400 !       1.50 eA-3
C136 0.514 0.443 0.059 !       1.50 eA-3
C137 0.005 0.570 0.860 !       1.49 eA-3
C138 0.505 0.070 0.360 !       1.49 eA-3
Q139 0.393 0.495 0.124 !       1.49 eA-3
C140 0.976 0.914 0.438 !       1.49 eA-3
C141 0.839 0.356 0.203 !       1.48 eA-3
C142 0.275 0.315 0.879 !       1.48 eA-3
C143 0.775 0.815 0.379 !       1.48 eA-3
C144 0.656 0.636 0.924 !       1.48 eA-3
C145 0.228 0.845 0.407 !       1.47 eA-3
C146 0.305 0.220 0.358 !       1.47 eA-3
C147 0.634 0.223 0.263 !       1.47 eA-3
C148 0.782 0.892 0.300 !       1.47 eA-3
C149 0.998 0.306 0.403 !       1.45 eA-3
C150 0.947 0.484 0.261 !       1.45 eA-3
C151 0.662 0.765 0.190 !       1.45 eA-3
C152 0.844 0.644 0.830 !       1.45 eA-3
Q153 0.905 0.664 0.277 !       1.44 eA-3
C154 0.859 0.144 0.045 !       1.43 eA-3
C155 0.367 0.702 0.392 !       1.42 eA-3
C156 0.509 0.062 0.246 !       1.41 eA-3
C157 0.672 0.175 0.138 !       1.40 eA-3
C158 0.133 0.818 0.434 !       1.40 eA-3
C159 0.719 0.894 0.390 !       1.39 eA-3
C160 0.319 0.365 0.016 !       1.38 eA-3
C161 0.272 0.006 0.453 !       1.38 eA-3
C162 0.725 0.673 0.871 !       1.38 eA-3
Q163 0.522 0.889 0.397 !       1.38 eA-3
C164 0.336 0.640 0.124 !       1.37 eA-3
C165 0.366 0.180 0.373 !       1.37 eA-3
C166 0.140 0.336 0.874 !       1.37 eA-3
C167 0.350 0.783 0.043 !       1.36 eA-3
C168 0.961 0.940 0.002 !       1.35 eA-3
C169 0.298 0.889 0.434 !       1.34 eA-3
C170 0.882 0.735 0.487 !       1.34 eA-3
C171 0.637 0.315 0.032 !       1.34 eA-3
Q172 0.330 0.626 0.386 !       1.34 eA-3
C173 0.600 0.785 0.015 !       1.33 eA-3
Q174 0.594 0.180 0.663 !       1.33 eA-3
Q175 0.094 0.680 0.163 !       1.33 eA-3
Q176 0.263 0.781 0.281 !       1.33 eA-3
C177 0.108 0.679 0.190 !       1.32 eA-3
C178 0.507 0.250 0.125 !       1.32 eA-3
C179 0.648 0.798 0.298 !       1.32 eA-3
C180 0.180 0.199 0.374 !       1.32 eA-3
C181 0.586 0.799-0.005 !       1.31 eA-3
C182 0.227 0.459 0.954 !       1.31 eA-3
C183 0.727 0.959 0.454 !       1.31 eA-3
C184 0.585 0.515 0.094 !       1.31 eA-3
C185 0.085 0.015 0.594 !       1.31 eA-3
C186 0.838 0.652 0.317 !       1.30 eA-3
C187 0.749 1.004 0.421 !       1.30 eA-3
C188 0.227 0.165 0.262 !       1.30 eA-3
C189 0.016 0.586 0.843 !       1.30 eA-3
C190 0.667 0.249 0.080 !       1.30 eA-3
C191 0.751 0.663 0.834 !       1.
;
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1964 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         11323
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0641P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6580
_reflns_number_total             11323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00029d2.cif
_cod_data_source_block           493-MOF-BA
_cod_depositor_comments
'Adding full bibliography for 7119752--7119753.cif.'
_cod_original_cell_volume        28304.6(13)
_cod_database_code               7119752
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'O H N C Zr'
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.454
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(2) 0.49(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C25-C26
 1.45 with sigma of 0.002
 O11-C25
 1.43 with sigma of 0.002
 C28-C31
 2.789 with sigma of 0.0001
 C31-C28
 2.789 with sigma of 0.0001
 C29-C28 = C30-C29 = C31-C30
 1.39 with sigma of 0.0001
 C28-C27 = C2-C1 = C23-C12
 1.5 with sigma of 0.01
 C31-C29 = C30-C28
 2.415 with sigma of 0.0001
4. Restrained planarity
 C28, C29, C30, C31
 with sigma of 0.001
5. Rigid bond restraints
 C26, C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11, C25, C26
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 1.7A with sigma
of 0.002 and sigma for terminal atoms of 0.004
O11 \\sim C25 \\sim C26: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(O11) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
7. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5)
8.a Riding coordinates:
 C29(H29), C30(H30), C31(H31), O17(H17A,H17B)
8.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'