Isolated π-Interaction Sites in Mesoporous MOF Backbone for Repetitive and Reversible Dynamics in Water.
Xu, Xiaohui; Li, Shenhui; Liu, Qi; Liu, Zhiyu; Yan, Wei; Zhao, Ligong; Zhang, Wenhao; Zhang, Liang; Deng, Feng; Cong, Hengjiang; Deng, Hexiang; ACS applied materials & interfaces 11 (2019) 973–981; doi:10.1021/acsami.8b19211

data_4515435
_publ_section_title
;
 Isolated \p-Interaction Sites in Mesoporous MOF Backbone for Repetitive
 and Reversible Dynamics in Water.
;
_journal_issue                   1
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              973
_journal_page_last               981
_journal_paper_doi               10.1021/acsami.8b19211
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'C288 Cu3 N12 O32 Zr6'
_chemical_formula_sum            'C288 Cu3 N12 O32 Zr6'
_chemical_formula_weight         4876.94
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-02
_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                90
_cell_formula_units_Z            1
_cell_length_a                   31.4167(2)
_cell_length_b                   31.4167(2)
_cell_length_c                   31.4167(2)
_cell_measurement_reflns_used    9409
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      49.98
_cell_measurement_theta_min      2.81
_cell_volume                     31008.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76742
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        49.978
_diffrn_reflns_theta_max         49.978
_diffrn_reflns_theta_min         1.989
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7499
_exptl_absorpt_correction_T_min  0.4265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.5687.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    0.261
_exptl_crystal_description       block
_exptl_crystal_F_000             2395
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         3137
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.292
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1407P)^2^+31.6165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2948
_reflns_number_total             3137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b19211_si_005.cif
_cod_data_source_block           1
_cod_original_cell_volume        31008.6(6)
_cod_database_code               4515435
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C10-C11
 1.38 with sigma of 0.01
 C11-C12
 1.38 with sigma of 0.01
 C12-C13
 1.38 with sigma of 0.01
 C10-C13
 2.9 with sigma of 0.01
 C11-C11_$5
 2.2 with sigma of 0.01
 C12-C12_$5
 2.2 with sigma of 0.01
 C7-C7_$5
 1.9 with sigma of 0.04
 C9_$1-C8_$1 \\sim C6_$1-C7_$1
 with sigma of 0.02
 C9_$1-C8_$2 \\sim C8_$1-C7_$1
 with sigma of 0.02
 C8_$1-C7_$1 \\sim C8_$2-C7_$2
 with sigma of 0.02
 C7_$2-C6_$1 \\sim C8_$1-C7_$1
 with sigma of 0.02
 C7-C7_$5 \\sim C8-C8_$5
 with sigma of 0.02
 C3-C3_$5 \\sim C7-C7_$5
 with sigma of 0.02
 C3-C3_$5 \\sim C4_$5-C4
 with sigma of 0.02
2. Restrained planarity
 C6_$3, C7_$3, C7_$4, C8_$3, C8_$4, C9_$3
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C6 \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C10 \\sim C11 \\sim C12 \\sim C13: within 2.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(N17)
\\sim Ueq, Uanis(Cu1) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.05
Uanis(C9) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.15
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.15
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5)
Uanis(C6) = Uanis(C7) = Uanis(C9) = Uanis(C8)
Uanis(C16) = Uanis(C14) = Uanis(C15)
Uanis(Cu1) = Uanis(N17)
4. Others
 Fixed Sof: Cu1(0.0625) N17(0.25) C14(0.25) C15(0.5) C16(0.5)
;
_shelx_res_checksum              23359
_shelx_hkl_checksum              10412
_shelx_fab_checksum              46205
_olex2_submission_special_instructions 'No special instructions were received'