A rare (3,12)-connected zirconium metal‒organic framework with efficient iodine adsorption capacity and pH sensing
Guo, Bingbing; Li, Fugang; Wang, Chiming; Zhang, Liangliang; Sun, Daofeng; Journal of Materials Chemistry A 7 (2019) 13173–; doi:10.1039/C9TA03126J

data_7237663
_publ_section_title
;
 A rare (3,12)-connected zirconium metal--organic framework with efficient
 iodine adsorption capacity and pH sensing
;
_journal_issue                   21
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              13173
_journal_paper_doi               10.1039/C9TA03126J
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         '0.08(C576 H336 N48 O192 Zr36)'
_chemical_formula_sum            'C48 H28 N4 O16 Zr3'
_chemical_formula_weight         1190.40
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-04-11 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   32.9862(2)
_cell_length_b                   32.9862(2)
_cell_length_c                   32.9862(2)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.1090
_cell_measurement_theta_min      3.7870
_cell_volume                     35891.9(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            40712
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         3.790
_diffrn_source                   CuK\a
_exptl_absorpt_coefficient_mu    2.367
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.661
_exptl_crystal_description       triangular
_exptl_crystal_F_000             7104
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.000015(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5604
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1380P)^2^+118.6884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3727
_reflns_number_total             5604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ta03126j2.cif
_cod_data_source_block           upc-158
_cod_original_cell_volume        35892.0(7)
_cod_database_code               7237663
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C11-C13 = C15-C8 = C9-C10
 1.39 with sigma of 0.02
3. Restrained angles
 C11-C13-C15
 fixed at 120 with sigma of 0.02
 C13-C15-C8
 fixed at 120 with sigma of 0.02
 C15-C8-C9
 fixed at 120 with sigma of 0.02
 C8-C9-C10
 fixed at 120 with sigma of 0.02
 C9-C10-C11
 fixed at 120 with sigma of 0.02
4. Restrained planarity
 C8, C9, C10, C11, C15
 with sigma of 0.1
 C8, C9, C10, C11, C13, C15
 with sigma of 0.1
5. Rigid bond restraints
 C11, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim N1 \\sim C1 \\sim C2 \\sim C3
\\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim
C12 \\sim C15: within 3.7A with sigma of 0.005 and sigma for terminal atoms of
0.001
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C15: within 3.7A with sigma of
0.005 and sigma for terminal atoms of 0.001
Uanis(C16) = Uanis(C14)
7. Others
 Sof(C14)=Sof(H14)=1-FVAR(1)
 Sof(C13)=Sof(H13)=FVAR(1)
 Sof(C16)=Sof(H16)=1-FVAR(2)
 Sof(C15)=Sof(H15)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
 C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'