Investigation on the Catalytic Behavior of one Novel Thulium-Organic Framework with Planar Tetranuclear {Tm4} Cluster as Active Center for Chemical CO2 Fixation
Chen, Hongtai; Zhang, Zhengguo; Hongxiao, Lv; Liu, Shurong; Zhang, Xiutang; Dalton Transactions  (2021) –; doi:10.1039/D1DT03646G

data_7709025
_publ_section_title
;
 Investigation on the Catalytic Behavior of one Novel Thulium-Organic
 Framework with Planar Tetranuclear {Tm4} Cluster as Active Center for
 Chemical CO2 Fixation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03646G
_journal_year                    2021
_chemical_formula_moiety         'C57 H21 N2 O26 Tm4, 5[C3H7NO], 4[H2O]'
_chemical_formula_sum            'C72 H64 N7 O35 Tm4'
_chemical_formula_weight         2263.02
_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             2021-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-05 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.120(4)
_cell_length_b                   22.120(4)
_cell_length_c                   38.202(8)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.789
_cell_measurement_theta_min      2.445
_cell_volume                     16188(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            87793
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.128
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    3.326
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1207 before and 0.0887 after correction. The Ratio of minimum to maximum transmission is 0.8408. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             6606
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.244
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0573P)^2^+1.2335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4008
_reflns_number_total             5117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03646g2.cif
_cod_data_source_block           m5485_0m_a
_cod_original_cell_volume        16188(7)
_cod_database_code               7709025
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.502
_diffrn_source_source            'Incoatc Ius 3.0 '
_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
 C17-C17_$1
 2.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5)
 H18(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C15(H15), C16(H16), C17(H17), C18(H18), C12(H12), C14(H14)
5.b Fitted hexagon refined as free rotating group:
 C11(C15,C16,C8,C17,C18)
;
_shelx_res_checksum              68139
_shelx_fab_checksum              82347
_olex2_submission_special_instructions 'No special instructions were received'