Thioether-Based Recyclable Metal Organic Frameworks for Selective and Efficient Removal of Hg2+ from Water
Li, Kan; Li, Jing-jing; Zhao, Ni; Xie, Ting-ting; Di, Bin; Xu, Li-li; Dalton Transactions  (2019) –; doi:10.1039/C9DT03714D

data_7701966
_publ_section_title
;
 Thioether-Based Recyclable Metal Organic Frameworks for Selective and
 Efficient Removal of Hg2+ from Water
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03714D
_journal_year                    2019
_chemical_formula_moiety
'2(C48 H42 Cu4 I6 N6 O4 S6), 4(C4 H9 N O), 4(H2 O), 2(C2 H8 N)'
_chemical_formula_sum            'C116 H144 Cu8 I12 N18 O16 S12'
_chemical_formula_weight         4462.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.422(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   37.334(4)
_cell_length_b                   11.7895(12)
_cell_length_c                   19.3724(19)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.97
_cell_measurement_theta_min      2.54
_cell_volume                     7568.7(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77489
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33083
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.758
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.2009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1612 before and 0.1089 after correction.
The Ratio of minimum to maximum transmission is 0.2691.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       block
_exptl_crystal_F_000             4308
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.492
_refine_diff_density_min         -2.837
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.1032
_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^)+(0.0551P)^2^+822.5405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6174
_reflns_number_total             6535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03714d2.cif
_cod_data_source_block           s_cui1_0m
_cod_database_code               7701966
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C29-N5
 1.46 with sigma of 0.01
 N5-C30
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O3) = Uanis(I1) = Uanis(O2)
Uanis(O4) = Uanis(I3)
Uanis(I2) = Uanis(O1)
Uanis(C30) = Uanis(C29) = Uanis(N5)
Uanis(Cu2) = Uanis(Cu3)
4. Others
 Sof(Cu3)=1-FVAR(1)
 Sof(Cu2)=FVAR(1)
 Fixed Sof: O6(0.75) H6C(0.75) H6D(0.75) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) N5(0.5) H5A(0.5) H5B(0.5)
 O7(0.25) H7A(0.25) H7B(0.25) O2(0.5) O3(0.5) O1(0.5) O4(0.5)
 Fixed X: Cu3(0.39756)
 Fixed Y: Cu3(0.563601)
 Fixed Z: Cu3(0.89401)
5.a Riding coordinates:
 O6(H6C,H6D), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), O7(H7A,H7B), C27(H27A,H27B,H27C)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C6(H6A,H6B), C19(H19A,H19B), N5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C20(H20), C8(H8), C23(H23), C21(H21), C12(H12), C2(H2), C5(H5),
 C22(H22), C1(H1), C4(H4), C18(H18), C16(H16), C17(H17), C15(H15)
;
_shelx_res_checksum              89376
_olex2_submission_special_instructions 'No special instructions were received'