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_7701965
_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         '0.5(C108 H108 Br8 Cu4 N12 O12 S12), C2 H3 N'
_chemical_formula_sum            'C56 H57 Br4 Cu2 N7 O6 S6'
_chemical_formula_weight         1563.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7837(7)
_cell_length_b                   22.9814(18)
_cell_length_c                   29.458(2)
_cell_measurement_reflns_used    7271
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.8100
_cell_measurement_theta_min      1.8510
_cell_volume                     6623.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -8.00  18.00   0.50    8.00    --    4.16  35.00 -83.00   52
  2  \w     48.00  78.00   0.50    8.00    --    4.16  35.00 -83.00   60
  3  \w     47.00  75.00   0.50    8.00    --    4.16  37.00-180.00   56
  4  \w     -8.00  26.00   0.50    8.00    --    4.16  37.00-180.00   68
  5  \w    -14.00  28.00   0.50    8.00    --   -1.74 -99.00 120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0307311000
_diffrn_orient_matrix_UB_12      -0.0260483000
_diffrn_orient_matrix_UB_13      0.0079011000
_diffrn_orient_matrix_UB_21      0.0103908000
_diffrn_orient_matrix_UB_22      -0.0090955000
_diffrn_orient_matrix_UB_23      -0.0227396000
_diffrn_orient_matrix_UB_31      0.0648498000
_diffrn_orient_matrix_UB_32      0.0138360000
_diffrn_orient_matrix_UB_33      -0.0000848000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.1644
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            33554
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.115
_diffrn_reflns_theta_min         1.772
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.589
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7836
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1793
_refine_ls_R_factor_gt           0.1191
_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^)+(0.0010P)^2^+369.5204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2743
_refine_ls_wR_factor_ref         0.2909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4353
_reflns_number_total             7836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03714d2.cif
_cod_data_source_block           lk-0610-100k
_cod_original_cell_volume        6623.3(9)
_cod_database_code               7701965
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Br01 \\sim Br: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Br01) \\sim Ueq, Uanis(Br) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Br01, Br
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(Br)=1-FVAR(1)
 Sof(Br01)=FVAR(1)
 Fixed Sof: C28(0.5) N4(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C6(H6A,H6B), C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C21(H21), C18(H18), C4(H4), C19(H19), C20(H20), C24(H24), C25(H25),
 C2(H2), C26(H26), C1(H1), C27(H27)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              43094
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.821