Zr(IV)-Based Metal-Organic Framework with T-Shaped Ligand: Unique Structure, High Stability, Selective Detection, and Rapid Adsorption of Cr<sub>2</sub>O<sub>7</sub><sup>2-</sup> in Water.
He, Tao; Zhang, Yong-Zheng; Kong, Xiang-Jing; Yu, Jiamei; Lv, Xiu-Liang; Wu, Yufeng; Guo, Zhen-Ji; Li, Jian-Rong; ACS applied materials & interfaces 10 (2018) 16650–16659; doi:10.1021/acsami.8b03987

data_4515349
_publ_section_title
;
 Zr(IV)-Based Metal-Organic Framework with T-Shaped Ligand: Unique
 Structure, High Stability, Selective Detection, and Rapid Adsorption of
 Cr<sub>2</sub>O<sub>7</sub><sup>2-</sup> in Water.
;
_journal_issue                   19
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              16650
_journal_page_last               16659
_journal_paper_doi               10.1021/acsami.8b03987
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.25(C168 H84 N12 O64 Zr12)'
_chemical_formula_sum            'C42 H21 N3 O16 Zr3'
_chemical_formula_weight         1097.28
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-25
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   23.3072(3)
_cell_length_b                   23.3072(3)
_cell_length_c                   21.8206(9)
_cell_measurement_reflns_used    5154
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      74.3350
_cell_measurement_theta_min      3.7570
_cell_volume                     10265.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_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    -15.00  33.00   1.00   12.50    --  -41.94  77.00  30.00   48
  2  \w    -62.00   1.00   1.00   12.50    --  -41.94  77.00 -93.00   63
  3  \w     75.00 167.00   1.00   47.50    --  107.13  77.00-180.00   92
  4  \w     84.00 146.00   1.00   47.50    --  107.13  77.00 -93.00   62
  5  \w    128.00 160.00   1.00   47.50    --  107.13  77.00-150.00   32
  6  \w     81.00 156.00   1.00   47.50    --  107.13  77.00 -60.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0340136000
_diffrn_orient_matrix_UB_12      -0.0473507000
_diffrn_orient_matrix_UB_13      -0.0542900000
_diffrn_orient_matrix_UB_21      -0.0249638000
_diffrn_orient_matrix_UB_22      0.0458639000
_diffrn_orient_matrix_UB_23      -0.0238465000
_diffrn_orient_matrix_UB_31      0.0636147000
_diffrn_orient_matrix_UB_32      0.0384608000
_diffrn_orient_matrix_UB_33      -0.0382999000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22202
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.793
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.710
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.850
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 1738 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.482(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         5781
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2088
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    0.744
_reflns_Friedel_fraction_max     0.764
_reflns_number_gt                4650
_reflns_number_total             5781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b03987_si_002.cif
_cod_data_source_block           exp_693-t-zr-smart
_cod_database_code               4515349
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O N Zr'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(C14) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.004
Uanis(O7) = Uanis(O6)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C14(H14), C4(H4), C13(H13), C9(H9)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.845