Highly Robust {Ln4}-Organic Frameworks (Ln = Ho, Yb) for Excellent Catalytic Performance on Cycloaddition Reaction of Epoxides with CO2 and Knoevenagel Condensation
Zhang, Tao; Chen, Hongtai; Liu, Shurong; Lv, Hongxiao; Zhang, Xiutang; Li, Qiaoling; ACS Catalysis  (2021) 14916–14925; doi:10.1021/acscatal.1c04260

data_4519141
_publ_section_title
;
 Highly Robust {Ln4}-Organic Frameworks (Ln = Ho, Yb) for Excellent
 Catalytic Performance on Cycloaddition Reaction of Epoxides with CO2 and
 Knoevenagel Condensation
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              14916
_journal_page_last               14925
_journal_paper_doi               10.1021/acscatal.1c04260
_journal_year                    2021
_chemical_formula_moiety         '0.17(C342 H138 Ho24 N12 O156)'
_chemical_formula_sum            'C57 H27 Ho4 N2 O26'
_chemical_formula_weight         1815.52
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_Hall           '-P 6c 2'
_space_group_name_H-M_alt        'P 63/m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-10
_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                120
_cell_formula_units_Z            6
_cell_length_a                   22.209(9)
_cell_length_b                   22.209
_cell_length_c                   38.44(2)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.097
_cell_measurement_theta_min      2.434
_cell_volume                     16420(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            81115
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.368
_exptl_absorpt_coefficient_mu    2.907
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1153 before and 0.0882 after correction. The Ratio of minimum to maximum transmission is 0.8868. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             5154
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.301
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5186
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0504P)^2^+13.5288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4051
_reflns_number_total             5186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04260_si_002.cif
_cod_data_source_block           m5484_0m
_cod_original_cell_volume        16421(15)
_cod_database_code               4519141
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C19-H19
 0.97 with sigma of 0.02
 C8-C17
 1.42 with sigma of 0.02
 O7-H7
 0.85 with sigma of 0.02
 C17-C17_$1
 2.2 with sigma of 0.04
 C15-C15_$1
 2.2 with sigma of 0.04
 C16-C16_$1
 2.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C15)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5A) \\sim Ueq, Uanis(O5B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(O5B)=1-FVAR(1)
 Sof(O5A)=FVAR(1)
 Fixed Sof: C15(0.5) H15(0.5) C16(0.5) C8(0.5) C17(0.5) C18(0.5) H18(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C15(H15), C18(H18), C12(H12), C14(H14)
5.b Fitted hexagon refined as free rotating group:
 C11(C15,C16,C8,C17,C18)
;
_shelx_res_checksum              83076
_shelx_hkl_checksum              54462
_shelx_fab_checksum              64028
_olex2_submission_special_instructions 'No special instructions were received'