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_7120148
_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
'C48 H74 Cu24 Gd6 N14 Na O92, 31(O), 8(N O3), N2 O4'
_chemical_formula_sum            'C48 H211 Cu24 Gd6 N24 Na O151'
_chemical_formula_weight         6032.86
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cczwqcx
_audit_creation_date             2013-01-16
_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                87.087(3)
_cell_angle_beta                 71.317(3)
_cell_angle_gamma                64.441(4)
_cell_formula_units_Z            1
_cell_length_a                   17.0801(7)
_cell_length_b                   17.8312(7)
_cell_length_c                   17.9410(5)
_cell_measurement_reflns_used    17028
_cell_measurement_temperature    123.3(3)
_cell_measurement_theta_max      29.0736
_cell_measurement_theta_min      2.9200
_cell_volume                     4645.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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      123.3(3)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9837
_diffrn_measurement_details
;
1 omega -12.00 88.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 77.0000 -30.0000 100

2 omega 1.00 66.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 57.0000 90.0000 65

3 omega 28.00 54.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 -99.0000 -150.0000 26

4 omega -52.00 15.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 0.0000 60.0000 67

5 omega -8.00 18.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 37.0000 -30.0000 26

6 omega 4.00 41.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 19.0000 120.0000 37

7 omega 46.00 71.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 19.0000 120.0000 25

8 omega -11.00 88.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ frames
- 18.1935 77.0000 -180.0000 99
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0307068000
_diffrn_orient_matrix_UB_12      -0.0186809000
_diffrn_orient_matrix_UB_13      0.0115869000
_diffrn_orient_matrix_UB_21      0.0064883000
_diffrn_orient_matrix_UB_22      -0.0085080000
_diffrn_orient_matrix_UB_23      -0.0402897000
_diffrn_orient_matrix_UB_31      0.0373508000
_diffrn_orient_matrix_UB_32      -0.0392865000
_diffrn_orient_matrix_UB_33      -0.0016246000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35920
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2966
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.141
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1239
_refine_ls_number_reflns         16349
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+70.0758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                13574
_reflns_number_total             16349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc01136a2.cif
_cod_data_source_block           p121214n
_cod_original_cell_volume        4645.2(3)
_cod_database_code               7120148
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
{H24A,H24B} of O24, {H99A,H99B} of O99, {H2A,H2B} of N2, {H20A,H20B} of O20,
{H21A,H21B} of O21, {H9A,H9B} of N9, {H54A,H54B} of N54, {H3A,H3B} of N3,
{H1A,H1B} of N1, {H25A,H25B} of O25, {H33A,H33B} of O33, {H32A,H32B} of O32,
{H46A,H46B} of O46, {H48,H12B} of N48
At 1.5 times of:
{H8A,H8B,H8C} of C8, {H14A,H14B,H14C} of C14, {H18A,H18B,H18C} of C18
2. Restrained distances
N8-O91
1.28 with sigma of 0.01
N8-O57
1.28 with sigma of 0.01
C9-C23B
1.5 with sigma of 0.02
C15B-C24B
1.54 with sigma of 0.02
N10-O36
1.28 with sigma of 0.01
N10-O86 = N6-O84
1.28 with sigma of 0.01
N11-O1A = N11-O1B = N11-O1CB
1.25 with sigma of 0.01
O1A-O1B = O1A-O1CB
2.2 with sigma of 0.01
O83B-O91 ~ O57-O83B ~ O91-O57
with sigma of 0.02
N5-N5
with sigma of 0.02
3. Restrained planarity
O91, N8, O83B, O57
with sigma of 0.1
N11, O1A, O1B, O1CB
with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C23A) ~ Ueq, Uanis(C23B) ~ Ueq, Uanis(N5) ~ Ueq, Uanis(N11) ~ Ueq: with si
Uanis(C12A) ~ Ueq, Uanis(C12B) ~ Ueq, Uanis(C13A) ~ Ueq, Uanis(C13B) ~ Ueq, Uani
Uanis(O83A) ~ Ueq, Uanis(O83B) ~ Ueq: with sigma of 0.01 and sigma for terminal
Uanis(O76A) ~ Ueq, Uanis(O76B) ~ Ueq: with sigma of 0.01 and sigma for terminal
Uanis(C17A) ~ Ueq, Uanis(C17B) ~ Ueq, Uanis(N6) ~ Ueq: with sigma of 0.01 and si
Uanis(O84) ~ Ueq, Uanis(O1E) ~ Ueq: with sigma of 0.01 and sigma for terminal at
Uanis(C18) ~ Ueq, Uanis(O86) ~ Ueq, Uanis(N10) ~ Ueq, Uanis(N8) ~ Ueq: with sigm
Uanis(C15A) ~ Ueq, Uanis(C15B) ~ Ueq, Uanis(C19A) ~ Ueq, Uanis(C19B) ~ Ueq, Uani
Uanis(O1I) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O1CB) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C23A) = Uanis(C23B)
Uanis(C15A) = Uanis(C15B)
Uanis(C19A) = Uanis(C19B)
Uanis(C20A) = Uanis(C20B)
Uanis(C17A) = Uanis(C17B)
Uanis(C12A) = Uanis(C12B)
Uanis(C13A) = Uanis(C13B)
Uanis(C24A) = Uanis(C24B)
Uanis(C21A) = Uanis(C21B)
Uanis(C16A) = Uanis(C16B)
Uanis(O72A) = Uanis(O72B)
Uanis(O83A) = Uanis(O83B)
Uanis(O76A) = Uanis(O76B)
Uanis(O84) = Uanis(O1E)
5. Others
Sof(O72A)=1-Sof(O72B)
1-Sof(C23A)=Sof(C23A)
1-Sof(C19B)=1-Sof(C19B)=1-Sof(C19B)=Sof(C20A)=Sof(C19A)=Sof(C15A)
1-Sof(C17A)=Sof(C17A)
1-Sof(C13B)=1-Sof(C13B)=1-Sof(C13B)=1-Sof(C13B)=Sof(C21A)=Sof(C13A)=Sof(C12A)=
Sof(C24A)
1-Sof(C3B)=1-Sof(C3B)=Sof(C3A)=Sof(C16A)
1-Sof(O83A)=Sof(O83A)
1-Sof(O76A)=Sof(O76A)
Fixed Sof: O84(0.5) O1E(0.5) O1H(0.5) N6(0.5) O1I(0.5) O1A(0.5) O1B(0.5)
N11(0.5) O1CB(0.5)
6.a Riding coordinates:
O20(H20A,H20B), O21(H21A,H21B), O24(H24A,H24B), O25(H25A,H25B), O32(H32A,
H32B), O33(H33A,H33B), O46(H46A,H46B), O99(H99A,H99B)
6.b Secondary CH2 refined with riding coordinates:
N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N48(H48,H12B), N9(H9A,H9B), N54(H54A,
H54B)
6.c Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;