Additive-Induced Supramolecular Isomerism and Enhancement of Robustness in Co(II)-Based MOFs for Efficiently Trapping Acetylene from Acetylene-Containing Mixtures.
Ye, Yingxiang; Chen, Shimin; Chen, Liangji; Huang, Jitao; Ma, Zhenlin; Li, Ziyin; Yao, Zizhu; Zhang, Jindan; Zhang, Zhangjing; Xiang, Shengchang; ACS applied materials & interfaces 10 (2018) 30912–30918; doi:10.1021/acsami.8b11999

data_4515408
_publ_section_title
;
 Additive-Induced Supramolecular Isomerism and Enhancement of Robustness
 in Co(II)-Based MOFs for Efficiently Trapping Acetylene from
 Acetylene-Containing Mixtures.
;
_journal_issue                   36
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              30912
_journal_page_last               30918
_journal_paper_doi               10.1021/acsami.8b11999
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.13(C216 H168 Co24 N72 O80)'
_chemical_formula_sum            'C27 H21 Co3 N9 O10'
_chemical_formula_weight         808.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7497(2)
_cell_length_b                   17.7497(2)
_cell_length_c                   61.8767(17)
_cell_measurement_reflns_used    6386
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.6210
_cell_measurement_theta_min      3.7630
_cell_volume                     19494.4(6)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            24079
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.232
_diffrn_reflns_theta_min         3.285
_exptl_absorpt_coefficient_mu    4.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44453
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    0.551
_exptl_crystal_description       bulk
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         5075
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0878
_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^)+(0.1840P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2544
_refine_ls_wR_factor_ref         0.2732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3348
_reflns_number_total             5075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b11999_si_003.cif
_cod_data_source_block           FJU-89
_cod_original_cell_volume        19494.4(7)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               4515408
_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,H) groups
2. Shared sites
{C2, N1AA}
{N0AA, C5}
3. Restrained distances
 O2-C1 = N3-C1
 1.05 with sigma of 0.02
 O3A-C1 = O2-C1
 1.25 with sigma of 0.02
 O2-C1 = O3A-C1
 1.2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C3 \\sim C0AA \\sim C5 \\sim C1AA \\sim C6 \\sim C7 \\sim C4: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
N1 \\sim C9 \\sim C2 \\sim C11 \\sim C13 \\sim C12: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C1AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N1) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N0AA) = Uanis(C5)
Uanis(C2) = Uanis(N1AA)
Uanis(N1) = Uanis(O1A)
Uanis(O3A) = Uanis(N3)
Uanis(O2) = Uanis(N2A)
5. Others
 Fixed Sof: C5(0.5) H6(0.5) C4(0.5) H4(0.5) C7(0.5) C1AA(0.5) H1AA(0.5)
 N1(0.5) C2(0.25) C9(0.25) C8(0.5) H8(0.5) H13(0.25) C12(0.25) H6A(0.25)
 H6B(0.25) C11(0.5) H11(0.5) N1AA(0.25) O2(0.5) N3(0.5) N2A(0.5) C3(0.5)
 H3(0.5) N0AA(0.5) C0AA(0.5) H0AA(0.5) C1(0.5) O1A(0.5) O3A(0.5)
6.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B)
6.b :
 N3(N2A,C3,N0AA,C0AA)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C1AA(H1AA), C8(H8), C13(H13), C11(H11), C3(H3), C0AA(H0AA)
;
_olex2_submission_special_instructions 'No special instructions were received'