Topology-Based Functionalization of Robust Chiral Zr-Based Metal-Organic Frameworks for Catalytic Enantioselective Hydrogenation.
Jiang, Hong; Zhang, Wenqiang; Kang, Xing; Cao, Ziping; Chen, Xu; Liu, Yan; Cui, Yong; Journal of the American Chemical Society 142 (2020) 9642–9652; doi:10.1021/jacs.0c00637

data_4134954
_publ_section_title
;
 Topology-Based Functionalization of Robust Chiral Zr-Based Metal-Organic
 Frameworks for Catalytic Enantioselective Hydrogenation.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9642
_journal_page_last               9652
_journal_paper_doi               10.1021/jacs.0c00637
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '0.13(C320 H176 O160 Zr24)'
_chemical_formula_sum            'C40 H22 O20 Zr3'
_chemical_formula_weight         1096.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1834(15)
_cell_length_b                   33.744(2)
_cell_length_c                   34.489(2)
_cell_measurement_reflns_used    6426
_cell_measurement_temperature    173
_cell_measurement_theta_max      45.732
_cell_measurement_theta_min      4.565
_cell_volume                     21162(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.572
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.572
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15639
_diffrn_reflns_point_group_measured_fraction_full 0.572
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.809
_diffrn_reflns_theta_min         1.181
_exptl_absorpt_coefficient_mu    0.323
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.688
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2937
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+212.8261P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1990
_reflns_number_total             2937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00637_si_002.cif
_cod_data_source_block           flu-CMOF-1
_cod_depositor_comments
'Adding full bibliography for 4134951--4134954.cif.'
_cod_original_cell_volume        21162(3)
_cod_database_code               4134954
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C7 \\sim C6 \\sim C10 \\sim C5 \\sim C3 \\sim C4 \\sim C11:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C3 \\sim C4 \\sim O1 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C11
\\sim C9 \\sim C10: within 1.7A with sigma of 0.04 and sigma for terminal atoms
of 0.08
O2 \\sim C11 \\sim O3 \\sim C8 \\sim C7 \\sim C6 \\sim C5 \\sim C10 \\sim C9
\\sim C3 \\sim C4 \\sim C2 \\sim O1: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C2) = Uanis(C1)
3. Rigid body (RIGU) restrains
 O2, C3, C4, H4, C9, H9, C7, H7, C8, C6, H6, C5, C11, C10, H10, O3, O1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C7(H7), C6(H6), C10(H10)
4.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              5864
_shelx_hkl_checksum              79861
_shelx_fab_checksum              52521
_olex2_submission_special_instructions 'No special instructions were received'