Catalysis through Dynamic Spacer Installation of Multivariate Functionalities in Metal-Organic Frameworks.
Cao, Chen-Chen; Chen, Cheng-Xia; Wei, Zhang-Wen; Qiu, Qian-Feng; Zhu, Neng-Xiu; Xiong, Yang-Yang; Jiang, Ji-Jun; Wang, Dawei; Su, Cheng-Yong; Journal of the American Chemical Society 141 (2019) 2589–2593; doi:10.1021/jacs.8b12372

data_4128165
_publ_section_title
;
 Catalysis through Dynamic Spacer Installation of Multivariate
 Functionalities in Metal-Organic Frameworks.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2589
_journal_page_last               2593
_journal_paper_doi               10.1021/jacs.8b12372
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C152 H60 F48 N4 O64 Zr12)'
_chemical_formula_sum            'C76 H30 F24 N2 O32 Zr6'
_chemical_formula_weight         2486.34
_chemical_name_common            LIFM-28-BPYDC
_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_Hall           '-P 4c 2'
_space_group_name_H-M_alt        'P 42/m m c'
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.0084(5)
_cell_length_b                   23.0084(5)
_cell_length_c                   18.8119(7)
_cell_measurement_reflns_used    6381
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.5480
_cell_measurement_theta_min      4.2750
_cell_volume                     9958.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.980
_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   -109.00 -19.00   1.00   30.00    --  -38.50 -37.00-150.00   90
  2  \w     91.00 151.00   1.00   75.00    --   96.88  45.00 150.00   60
  3  \w     40.00 122.00   1.00   75.00    --   96.88-125.00  60.00   82
  4  \w     78.00 152.00   1.00   75.00    --   96.88  45.00 -90.00   74
;
_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      -0.0030320000
_diffrn_orient_matrix_UB_12      0.0022893000
_diffrn_orient_matrix_UB_13      -0.0817483000
_diffrn_orient_matrix_UB_21      -0.0141062000
_diffrn_orient_matrix_UB_22      0.0653216000
_diffrn_orient_matrix_UB_23      0.0036738000
_diffrn_orient_matrix_UB_31      0.0654712000
_diffrn_orient_matrix_UB_32      0.0141918000
_diffrn_orient_matrix_UB_33      -0.0029353000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19475
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.739
_diffrn_reflns_theta_min         4.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    0.829
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1272P)^2^+29.9360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2242
_refine_ls_wR_factor_ref         0.2318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4259
_reflns_number_total             5016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            LIFM-28-BPYDC.cif
_cod_data_source_block           LIFM-28-BPYDC
_cod_original_cell_volume        9958.8(6)
_cod_database_code               4128165
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     IR
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.863
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C1
 1.39 with sigma of 0.01
 C1-C3 = C2-C4 = C3-C5 = C4-C6 = C5-C1 = C6-C2
 2.4 with sigma of 0.01
 C1-C4 = C2-C5 = C3-C6
 2.8 with sigma of 0.01
 C10-C11 = C11-C12 = C12-C13 = C13-N1 = N1-C11_$1
 1.39 with sigma of 0.01
 C10-C12 = C11-C13 = C12-N1 = N1-C10
 2.4 with sigma of 0.01
 C10-C13 = C11-N1 = C12-C11_$1
 2.8 with sigma of 0.01
 C9-C10 = C13-C13_$2
 1.49 with sigma of 0.01
 C2-C8 = C6-C8A
 1.49 with sigma of 0.01
 C8-F1 = C8-F2 = C8-F3
 1.33 with sigma of 0.01
 C8A-F1A = C8A-F2A = C8A-F3A
 1.33 with sigma of 0.01
 C2-F1 = C2-F2 = C2-F3
 2.35 with sigma of 0.01
 C6-F1A = C6-F2A = C6-F3A
 2.35 with sigma of 0.01
 C1-C8A \\sim C5-C8A \\sim C1-C8 \\sim C3-C8
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C8A
 with sigma of 0.01
4. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C8A, F1, F2, F3, F1A, F2A, F3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C10, C11, C12, C13, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zr1, Zr2, O4, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C8A
\\sim F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim N1: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Zr1 \\sim Zr2 \\sim O4 \\sim O5: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(N1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(H2)=Sof(C8A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(H6)=Sof(C8)=FVAR(1)
 Fixed Sof: N1(0.25) H11(0.25) H11A(0.25) C12(0.25) H12(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C11(H11), C11(H11A), C12(H12)
;
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.670