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_4515314
_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(C720 H408 O280 Zr48)'
_chemical_formula_sum            'C90 H51 O35 Zr6'
_chemical_formula_weight         2239.62
_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
_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                   32.7630(3)
_cell_length_b                   32.7630(3)
_cell_length_c                   32.7630(3)
_cell_measurement_reflns_used    3980
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.0800
_cell_measurement_theta_min      3.7860
_cell_volume                     35168.3(6)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.998
_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   -113.00 -53.00   1.00   40.00    --  -42.06-155.00 -80.00   60
  2  \w     83.00 153.00   1.00  100.00    --  107.13 -15.00   0.00   70
;
_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      0.0056371000
_diffrn_orient_matrix_UB_12      0.0130924000
_diffrn_orient_matrix_UB_13      -0.0447975000
_diffrn_orient_matrix_UB_21      -0.0222352000
_diffrn_orient_matrix_UB_22      0.0404294000
_diffrn_orient_matrix_UB_23      0.0090279000
_diffrn_orient_matrix_UB_31      0.0410715000
_diffrn_orient_matrix_UB_32      0.0201052000
_diffrn_orient_matrix_UB_33      0.0110309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.1367
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26321
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.027
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76565
_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            'light colourless'
_exptl_crystal_density_diffrn    0.846
_exptl_crystal_description       block
_exptl_crystal_F_000             8888
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2125 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.156(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10490
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6934
_reflns_number_total             10490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b09333_si_007.cif
_cod_data_source_block           BUT-46W
_cod_original_cell_volume        35168.3(10)
_cod_database_code               4515314
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O Zr'
_reflns_odcompleteness_completeness 99.73
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(O2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C29) = Uanis(C28)
3.a Rotating group:
 O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C21(H21), C27(H27), C26(H26), C15(H15), C23(H23), C18(H18),
 C16(H16), C12(H12), C9(H9), C19(H19), C4(H4), C3(H3), C7(H7), C6(H6)
;
_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.854