Surface functionalized chalcogenides for highly selective removal of Hg2+
Jie, Hao-Chen; Lan, Zhi-Qing; Li, Ke-Feng; Ye, Xiao-Liang; Duan, Shui-Lin; Fu, Zhi-Hua; Wang, Guan-E; Xu, Gang; CrystEngComm 26 (2024) 6255–6259; doi:10.1039/D4CE00923A

data_7249483
_publ_section_title
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 Surface functionalized chalcogenides for highly selective removal of Hg2+
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_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              6255
_journal_page_last               6259
_journal_paper_doi               10.1039/D4CE00923A
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H8 Cu2 N6 S8.982, 4.5[CH3CN]'
_chemical_formula_sum            'C21 H21.5 Cu2 N10.5 S8.98'
_chemical_formula_weight         836.03
_chemical_name_systematic        CuPMTT
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-14
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2024-10-14 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.95(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.430(2)
_cell_length_b                   10.720(2)
_cell_length_c                   27.570(6)
_cell_measurement_reflns_used    13528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.692
_cell_measurement_theta_min      0.029
_cell_volume                     3345.7(11)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4161
_diffrn_reflns_av_unetI/netI     0.2079
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            109120
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.492
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  1.692
_exptl_absorpt_correction_T_min  0.029
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             1691
_exptl_crystal_preparation       'Three-dimensional electron diffraction'
_exptl_crystal_recrystallization_method 'Flaky stacking'
_exptl_crystal_size_max          0.018
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         11795
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1815
_refine_ls_R_factor_gt           0.1424
_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^)+(0.1915P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3384
_refine_ls_wR_factor_ref         0.3648
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                6211
_reflns_number_total             11795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00923a2.cif
_cod_data_source_block           3_a
_cod_depositor_comments          'Adding full bibliography for 7249483.cif.'
_cod_original_cell_volume        3345.7(12)
_cod_original_formula_sum        'C21 H21.50 Cu2 N10.50 S8.98'
_cod_database_code               7249483
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(6)
 0.47(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 S00C-C01C \\sim S3-C01C
 with sigma of 0.02
 S008-C10 \\sim S2-C10
 with sigma of 0.02
 S008-Cu1B \\sim S2-Cu1B
 with sigma of 0.02
 Cu2-S009 \\sim Cu2-S7
 with sigma of 0.02
 S009-C00I \\sim S7-C00I
 with sigma of 0.02
4. Rigid bond restraints
 S008
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 S009
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C011
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N014) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N01N) \\sim Ueq, Uanis(C010) \\sim Ueq, Uanis(C01F) \\sim Ueq,
Uanis(C01Q) \\sim Ueq, Uanis(C00Z) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N32) \\sim Ueq, Uanis(C01B) \\sim Ueq, Uanis(N01D) \\sim Ueq, Uanis(C10)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C01B) \\sim Ueq, Uanis(N01D) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C011)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(S1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01O) \\sim Ueq, Uanis(C00O) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C01I) \\sim Ueq, Uanis(C00G) \\sim Ueq, Uanis(C019) \\sim Ueq,
Uanis(C00I) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S008) \\sim Ueq, Uanis(S00C) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(N00A) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(N00Q) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N32) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N01A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00P) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00W) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C00P) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C00K) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C00P) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C015)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N018) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S008) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(S00C) \\sim Ueq, Uanis(S5) \\sim Ueq: with sigma of 5 and sigma for
terminal atoms of 10
Uanis(S3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S0) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cu3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S009) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S00L) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N012) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00K) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C011) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S6) \\sim Ueq, Uanis(S5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 Sof(S7)=1-FVAR(1)
 Sof(S009)=FVAR(1)
 Fixed Sof: S008(0.5) S00C(0.5) S3(0.5) S2(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C2(H2), N01D(H01D), N00A(H00A), N1(H1), N01N(H01N), C015(H015),
 N012(H012), N00Y(H00Y), N32(H32), C31(H31), N018(H018), C01F(H01F), N014(H014),
  N40(H40), C00W(H00W)
7.b Fitted hexagon refined as free rotating group:
 C00I(C2,C01B,N01D,C10,N00A), C00O(N01N,C6,C015,C011,N012), C00P(N00Y,C19,N32,
 C01Q,C31), N014(C01O,N40,C00F,C00W,C01I)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 396 electrons were 
found in a volume of 1423\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
9[CH3CN] per formula unit 
which account for 360 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64398
_shelx_hkl_checksum              55101
_shelx_fab_checksum              47956
_olex2_exptl_crystal_mounting_method
;
Three position electron diffraction
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_olex2_submission_original_sample_id C12H28Cu2N6O10S9
_olex2_submission_special_instructions 'No special instructions were received'