Cluster-based MOFs with accelerated chemical conversion of CO2 through C‒C bond formation
Xiong, Gang; Yu, Bing; Dong, Jie; Shi, Ying; Zhao, Bin; He, Liang-Nian; Chem. Commun.  (2017) –; doi:10.1039/C7CC01136A

data_7120149
_publ_section_title
;
 Cluster-based MOFs with accelerated chemical conversion of CO2 through
 C--C bond formation
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC01136A
_journal_year                    2017
_chemical_formula_moiety         'C47.4 Cu24 Dy6 N12 Na O82, 4(O), 0.6(C)'
_chemical_formula_sum            'C48 H251 Cu24 Dy6 N24 Na O151'
_chemical_formula_weight         6064.36
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cczwqbw
_audit_creation_date             2013-01-17
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2013-01-17 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                87.132(3)
_cell_angle_beta                 71.317(4)
_cell_angle_gamma                64.300(4)
_cell_formula_units_Z            1
_cell_length_a                   17.0964(7)
_cell_length_b                   17.8161(7)
_cell_length_c                   17.8597(7)
_cell_measurement_reflns_used    5531
_cell_measurement_temperature    125.2(4)
_cell_measurement_theta_max      29.0822
_cell_measurement_theta_min      2.8803
_cell_volume                     4618.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      125.2(4)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega 0.00 27.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 57.0000 -180.0000 27

2 omega -12.00 87.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 77.0000 -60.0000 99

3 omega 46.00 83.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 -136.0000 93.0000 37

4 omega -50.00 46.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 -77.0000 -180.0000 96

5 omega -1.00 39.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 57.0000 -60.0000 40

6 omega 9.00 37.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 -99.0000 60.0000 28

7 omega 17.00 42.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 37.0000 -150.0000 25

8 omega -16.00 87.00 1.0000 37.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 19.0000 120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0018194000
_diffrn_orient_matrix_UB_12      -0.0325578000
_diffrn_orient_matrix_UB_13      0.0249339000
_diffrn_orient_matrix_UB_21      0.0221813000
_diffrn_orient_matrix_UB_22      -0.0297211000
_diffrn_orient_matrix_UB_23      -0.0339832000
_diffrn_orient_matrix_UB_31      0.0434391000
_diffrn_orient_matrix_UB_32      -0.0054932000
_diffrn_orient_matrix_UB_33      0.0005916000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35642
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2978
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         2.212
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         16262
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                9214
_reflns_number_total             16262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc01136a2.cif
_cod_data_source_block           p120914j
_cod_original_cell_volume        4618.2(3)
_cod_database_code               7120149
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1JA) ~ Ueq, Uanis(C1JB) ~ Ueq, Uanis(C2A) ~ Ueq, Uanis(C2B) ~ Ueq, Uanis(N1) ~ Ueq, Uanis(N2B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C1FA) ~ Ueq, Uanis(C1FB) ~ Ueq, Uanis(C11A) ~ Ueq, Uanis(C11B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C3A) ~ Ueq, Uanis(C3B) ~ Ueq, Uanis(C5A) ~ Ueq, Uanis(C5B) ~ Ueq, Uanis(N24B) ~ Ueq, Uanis(N24A) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C8) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C3) ~ Ueq, Uanis(C4) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C6) ~ Ueq, Uanis(C5) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C10A) ~ Ueq, Uanis(C10B) ~ Ueq, Uanis(C18A) ~ Ueq, Uanis(C18B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C1CA) ~ Ueq, Uanis(C1CB) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C0AA) ~ Ueq, Uanis(C0AB) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C1A) ~ Ueq, Uanis(C1B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C1JA) = Uanis(C1JB)
Uanis(C2A) = Uanis(C2B)
Uanis(N2B) = Uanis(N1)
Uanis(C1FA) = Uanis(C1FB)
Uanis(C11A) = Uanis(C11B)
Uanis(C3A) = Uanis(C3B)
Uanis(C5A) = Uanis(C5B)
Uanis(N24B) = Uanis(N24A)
Uanis(C6) = Uanis(C5)
Uanis(C10A) = Uanis(C10B)
Uanis(C18A) = Uanis(C18B)
Uanis(C1CA) = Uanis(C1CB)
Uanis(C0AA) = Uanis(C0AB)
Uanis(C1) = Uanis(C1B)
2. Others
1-Sof(C2B)=1-Sof(C2B)=1-Sof(C2B)=Sof(N1)=Sof(C2A)=Sof(C1JA)
1-Sof(C1FB)=1-Sof(C1FB)=Sof(C11A)=Sof(C1FA)
1-Sof(C3B)=1-Sof(C3B)=1-Sof(C3B)=Sof(C3A)=Sof(N24A)=Sof(C5A)
1-Sof(C18B)=1-Sof(C18B)=Sof(C18A)=Sof(C10A)
1-Sof(C1CA)=Sof(C1CA)
1-Sof(C0AB)=Sof(C0AB)
1-Sof(C1)=Sof(C1)
Fixed Sof: C3(0.5) C4(0.5) C5(0.5) C6(0.5)
;