Metal‒Organic Frameworks with Tb4 Clusters as Nodes: Luminescent Detection of Chromium(VI) and Chemical Fixation of CO2
Dong, Jie; Xu, Hang; Hou, Sheng-Li; Wu, Zhi-Lei; Zhao, Bin; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00323

data_4345862
_publ_section_title
;
 Metal--Organic Frameworks with Tb4 Clusters as Nodes: Luminescent
 Detection of Chromium(VI) and Chemical Fixation of CO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00323
_journal_year                    2017
_chemical_formula_moiety         '0.5(C96 H88 N16 O56 Tb8), 10(H2 O), H4 O'
_chemical_formula_sum            'C48 H68 N8 O39 Tb4'
_chemical_formula_weight         2016.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-28
_audit_creation_method
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Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7100(4)
_cell_length_b                   21.7100(4)
_cell_length_c                   30.5654(12)
_cell_measurement_reflns_used    11592
_cell_measurement_temperature    122.15(10)
_cell_measurement_theta_max      28.8940
_cell_measurement_theta_min      3.1390
_cell_volume                     14406.2(7)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      122.15(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9027
_diffrn_measurement_details
;
  1 omega   20.00   60.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000 -150.0000 40

  2 omega   46.00   93.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000 -180.0000 47

  3 omega   61.00   92.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000   90.0000 31

  4 omega    1.00   32.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372    0.0000   90.0000 31
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0000871490
_diffrn_orient_matrix_UB_12      -0.0037462490
_diffrn_orient_matrix_UB_13      -0.0230614510
_diffrn_orient_matrix_UB_21      -0.0322510997
_diffrn_orient_matrix_UB_22      0.0051467003
_diffrn_orient_matrix_UB_23      -0.0003673003
_diffrn_orient_matrix_UB_31      0.0051892517
_diffrn_orient_matrix_UB_32      0.0320502517
_diffrn_orient_matrix_UB_33      -0.0026492517
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17191
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_min         3.253
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71091
_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
;
;
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description
;
;
_exptl_crystal_F_000             7872
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3176
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0338P)^2^+268.0753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2623
_reflns_number_total             3176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00323_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        14406.2(8)
_cod_database_code               4345862
_chemical_oxdiff_formula         C1GD1
_chemical_oxdiff_usercomment     DJ-GD
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26A,H26B} of O26, All O(H) groups
 At 1.5 times of:
  {H22A,H22B} of O22, {H24A,H24B} of O24, {H23A,H23B} of O23, {H21A,H21B} of O21
2. Restrained distances
 O-H
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: H22A(0.5) H22B(0.5)
4.a Riding coordinates:
 O2(H2), O24(H24A,H24B), O26(H26A,H26B), O22(H22A,H22B), O(H)
4.b Rotating group:
 O21(H21A,H21B), O23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'