Ligand Rigidification for Enhancing the Stability of Metal-Organic Frameworks.
Lv, Xiu-Liang; Yuan, Shuai; Xie, Lin-Hua; Darke, Hannah F.; Chen, Ya; He, Tao; Dong, Chen; Wang, Bin; Zhang, Yong-Zheng; Li, Jian-Rong; Zhou, Hong-Cai; Journal of the American Chemical Society 141 (2019) 10283–10293; doi:10.1021/jacs.9b02947

data_4128034
_publ_section_title
;
 Ligand Rigidification for Enhancing the Stability of Metal-Organic
 Frameworks.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10283
_journal_page_last               10293
_journal_paper_doi               10.1021/jacs.9b02947
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.25(C248 H96 O64 Zr12)'
_chemical_formula_sum            'C62 H24 O16 Zr3'
_chemical_formula_weight         1298.47
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3176(5)
_cell_length_b                   22.3176(5)
_cell_length_c                   38.8607(8)
_cell_measurement_reflns_used    5082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.9630
_cell_measurement_theta_min      4.4130
_cell_volume                     19355.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (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, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -10.00  15.00   0.50   10.00    --  -42.10  20.00 179.00   50
  2  \w    -83.00 -57.00   0.50   10.00    --  -42.10 -20.00  11.00   52
  3  \w    -70.00 -44.00   0.50   60.00    -- -101.60  20.00 179.00   52
  4  \w   -123.00 -72.00   0.50   60.00    -- -101.60  20.00 179.00  102
  5  \w    -52.00 -27.00   0.50   10.00    --    5.00 -20.00  11.00   50
  6  \w    -65.00  46.00   0.50   10.00    --  -42.10  44.00  -5.96  222
  7  \w   -103.00 -13.00   0.50   60.00    -- -101.60  57.00 -30.00  180
  8  \w   -123.00 -59.00   0.50   60.00    -- -101.60  38.00 -90.00  128
  9  \w    -46.00 -12.00   0.50   60.00    -- -101.60  38.00 -90.00   68
 10  \w   -152.00 -78.00   0.50   60.00    -- -101.60 -38.00  90.00  148
 11  \w    -76.00 -33.00   0.50   60.00    -- -101.60  57.00-120.00   86
 12  \w   -116.00 -91.00   0.50   60.00    -- -101.60  57.00-120.00   50
 13  \w   -158.00-111.00   0.50   60.00    -- -101.60 -38.00-120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0454245000
_diffrn_orient_matrix_UB_12      0.0012074000
_diffrn_orient_matrix_UB_13      -0.0298484000
_diffrn_orient_matrix_UB_21      -0.0503010000
_diffrn_orient_matrix_UB_22      -0.0182479000
_diffrn_orient_matrix_UB_23      0.0250219000
_diffrn_orient_matrix_UB_31      -0.0129937000
_diffrn_orient_matrix_UB_32      0.0665747000
_diffrn_orient_matrix_UB_33      0.0074075000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            61292
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         3.608
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (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    0.446
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.029
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         8681
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0920P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3352
_reflns_number_total             8681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02947_si_001.cif
_cod_data_source_block           BUT-95
_cod_original_cell_volume        19355.6(10)
_cod_database_code               4128034
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O Zr'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.425
_reflns_odcompleteness_completeness 99.52
_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. Restrained distances
 C2-C7 \\sim C7-C6 \\sim C6-C5 \\sim C5-C4 \\sim C4-C3 \\sim C3-C2 \\sim C6-C8
\\sim C8-C9 \\sim C9-C10 \\sim C10-
 C11 \\sim C11-C5 \\sim C5-C6
 with sigma of 0.02
3. Rigid bond restraints
 C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C11 \\sim C4: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C7 \\sim C2 \\sim C6: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C11 \\sim C5 \\sim C10: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11)
;
_shelx_res_checksum              47871
_shelx_hkl_checksum              7785
_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 2.158
_oxdiff_exptl_absorpt_empirical_full_min 0.600