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_4128032
_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         '0.17(C336 H180 O96 Zr18)'
_chemical_formula_sum            'C56 H30 O16 Zr3'
_chemical_formula_weight         1232.46
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m m'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   50.5058(8)
_cell_length_b                   50.5058(8)
_cell_length_c                   14.8247(6)
_cell_measurement_reflns_used    9397
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.4810
_cell_measurement_theta_min      3.6580
_cell_volume                     32749.1(15)
_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 0.998
_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   -103.00 -76.00   0.50   10.00    --  -38.80 -55.00  26.00   54
  2  \w    -49.00 -18.00   0.50   10.00    --  -38.80 -55.00  26.00   62
  3  \w   -128.00 -16.00   0.50   30.00    -- -104.00  55.00 170.00  224
  4  \w   -192.00 -81.00   0.50   30.00    -- -104.00  -1.00  68.00  222
  5  \w   -119.00 -14.00   0.50   10.00    --  -38.80 -64.00 141.02  210
  6  \w    -61.00 -35.00   0.50   10.00    --  -38.80   1.00 -98.00   52
  7  \w   -128.00 -63.00   0.50   30.00    -- -104.00  57.00 -60.00  130
  8  \w   -183.00 -84.00   0.50   30.00    -- -104.00 -19.00   0.00  198
  9  \w   -116.00 -91.00   0.50   30.00    -- -104.00 -19.00 -90.00   50
 10  \w   -179.00-153.00   0.50   30.00    -- -104.00 -19.00 -90.00   52
 11  \w   -123.00 -77.00   0.50   30.00    -- -104.00  19.00-150.00   92
 12  \w    -84.00 -59.00   0.50   30.00    -- -104.00  57.00  30.00   50
 13  \w   -111.00 -48.00   0.50   30.00    -- -104.00  38.00   0.00  126
 14  \w   -177.00-151.00   0.50   30.00    -- -104.00 -25.00  17.00   52
;
_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      -0.0038203000
_diffrn_orient_matrix_UB_12      -0.0040695000
_diffrn_orient_matrix_UB_13      -0.1030631000
_diffrn_orient_matrix_UB_21      0.0302516000
_diffrn_orient_matrix_UB_22      0.0302435000
_diffrn_orient_matrix_UB_23      -0.0133078000
_diffrn_orient_matrix_UB_31      0.0176672000
_diffrn_orient_matrix_UB_32      -0.0175489000
_diffrn_orient_matrix_UB_33      0.0007021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            119841
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73400
_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    0.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         10627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0541
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6745
_reflns_number_total             10627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02947_si_001.cif
_cod_data_source_block           BUT-92
_cod_original_cell_volume        32749.1(17)
_cod_database_code               4128032
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Zr C O'
_reflns_odcompleteness_completeness 99.78
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14)
;
_shelx_res_checksum              9379
_shelx_hkl_checksum              95787
_shelx_fab_checksum              94895
_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 1.432
_oxdiff_exptl_absorpt_empirical_full_min 0.784