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_4515317
_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(C768 H480 O280 Zr48)'
_chemical_formula_sum            'C96 H60 O35 Zr6'
_chemical_formula_weight         2320.76
_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                   32.9225(9)
_cell_length_b                   32.9225(9)
_cell_length_c                   32.9225(9)
_cell_measurement_reflns_used    1291
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.9430
_cell_measurement_theta_min      3.7710
_cell_volume                     35684.4(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.945
_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   -116.00 -61.00   1.00   30.00    --  -41.94 -38.00  90.00   55
  2  \w     94.00 124.00   1.00   75.00    --  105.88 125.00-180.00   30
  3  \w    125.00 169.00   1.00   75.00    --  105.88 125.00 -90.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0084551000
_diffrn_orient_matrix_UB_12      -0.0415723000
_diffrn_orient_matrix_UB_13      -0.0197861000
_diffrn_orient_matrix_UB_21      -0.0104138000
_diffrn_orient_matrix_UB_22      0.0213090000
_diffrn_orient_matrix_UB_23      -0.0403453000
_diffrn_orient_matrix_UB_31      0.0448157000
_diffrn_orient_matrix_UB_32      -0.0029156000
_diffrn_orient_matrix_UB_33      -0.0131010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1726
_diffrn_reflns_av_unetI/netI     0.2337
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            25567
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.040
_diffrn_reflns_theta_min         3.798
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    0.864
_exptl_crystal_description       block
_exptl_crystal_F_000             9248
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.021
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 1384 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         10166
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5248
_reflns_number_total             10166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b09333_si_002.cif
_cod_data_source_block           BUT-46A
_cod_original_cell_volume        35684(3)
_cod_database_code               4515317
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O Zr'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. 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
2. Restrained planarity
 C69, C20, C18, C51, C45
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.002
Uanis(O6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) = Uanis(O12)
Uanis(O1) = Uanis(O4)
4.a Rotating group:
 O11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C27(H27), C28(H28), C29(H29), C32(H32), C35(H35),
 C47(H47), C37(H37), C40(H40), C44(H44), C49(H49), C55(H55), C64(H64), C2(H2)
4.c Fitted hexagon refined as free rotating group:
 C35(C45,C51,C47,C39,C42)
4.d Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.857