Tuning Water Sorption in Highly Stable Zr(IV)-Metal-Organic Frameworks through Local Functionalization of Metal Clusters.
Zhang, Yong-Zheng; He, Tao; Kong, Xiang-Jing; Lv, Xiu-Liang; Wu, Xue-Qian; Li, Jian-Rong; ACS applied materials & interfaces 10 (2018) 27868–27874; doi:10.1021/acsami.8b09333

data_4515318
_publ_section_title
;
 Tuning Water Sorption in Highly Stable Zr(IV)-Metal-Organic Frameworks
 through Local Functionalization of Metal Clusters.
;
_journal_issue                   33
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              27868
_journal_page_last               27874
_journal_paper_doi               10.1021/acsami.8b09333
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.13(C744 H432 O280 Zr48)'
_chemical_formula_sum            'C93 H54 O35 Zr6'
_chemical_formula_weight         2278.68
_space_group_crystal_system      cubic
_space_group_IT_number           212
_space_group_name_Hall           'P 4acd 2ab 3'
_space_group_name_H-M_alt        'P 43 3 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-07
_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                90
_cell_formula_units_Z            8
_cell_length_a                   32.67104(13)
_cell_length_b                   32.67104(13)
_cell_length_c                   32.67104(13)
_cell_measurement_reflns_used    18213
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.5540
_cell_measurement_theta_min      4.0420
_cell_volume                     34873.0(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -101.00  -34.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 67

  2 omega  -38.00   90.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       55.2484  -30.0000  -60.0000 128

  3 omega   16.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4967  -25.0000 -150.0000 77

  4 omega   18.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.4967  -37.0000  -90.0000 74

  5 omega  -94.00  -41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 53
;
_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      0.0061636000
_diffrn_orient_matrix_UB_12      0.0374422000
_diffrn_orient_matrix_UB_13      0.0280223000
_diffrn_orient_matrix_UB_21      -0.0040469000
_diffrn_orient_matrix_UB_22      0.0285726000
_diffrn_orient_matrix_UB_23      -0.0372953000
_diffrn_orient_matrix_UB_31      -0.0465612000
_diffrn_orient_matrix_UB_32      0.0024734000
_diffrn_orient_matrix_UB_33      0.0068930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46126
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.053
_diffrn_reflns_theta_min         3.313
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68851
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    0.868
_exptl_crystal_description       block
_exptl_crystal_F_000             9056
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         10393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0680P)^2^+3.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9597
_reflns_number_total             10393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b09333_si_004.cif
_cod_data_source_block           BUT-46F
_cod_original_cell_volume        34873.0(4)
_cod_database_code               4515318
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'Zr C O H'
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O7(H7a,H7b)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C27(H27), C9(H9), C23(H23), C26(H26), C5(H5), C20(H20), C31(H31),
 C11(H11), C21(H21), C8(H8), C14(H14), C18(H18), C17(H17), C6(H6), C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'