A novel copper(i) metal‒organic framework as a highly efficient and ultrasensitive electrochemical platform for detection of Hg(ii) ions in aqueous solution
Wang, Xiao-Qing; Tang, Jing; Ma, Xuehui; Wu, Dan; Yang, Jie; CrystEngComm 23 (2021) 3043–3051; doi:10.1039/D1CE00197C

data_7242415
_publ_section_title
;
 A novel copper(i) metal--organic framework as a highly efficient and
 ultrasensitive electrochemical platform for detection of Hg(ii) ions in
 aqueous solution
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              3043
_journal_page_last               3051
_journal_paper_doi               10.1039/D1CE00197C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '0.13(C176 H144 Cl24 Cu24 N80)'
_chemical_formula_sum            'C22 H18 Cl3 Cu3 N10'
_chemical_formula_weight         719.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-14 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.3530(13)
_cell_length_b                   30.106(3)
_cell_length_c                   26.328(2)
_cell_measurement_reflns_used    1611
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.065
_cell_measurement_theta_min      2.595
_cell_volume                     11376.6(18)
_computing_cell_refinement       'SAINT V6.36A (?, 2016)'
_computing_data_reduction        'SAINT V6.36A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13688
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_min         2.595
_exptl_absorpt_coefficient_mu    2.536
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       block
_exptl_crystal_F_000             5728
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.889
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1035
_reflns_number_total             2714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00197c2.cif
_cod_data_source_block           181112h
_cod_depositor_comments          'Adding full bibliography for 7242415.cif.'
_cod_original_cell_volume        11376.7(18)
_cod_database_code               7242415
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.537
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15-C13 = C14-N8 = C17-C16
 1.37 with sigma of 0.02
3. Rigid bond restraints
 C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim Cu1 \\sim Cl1: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cu4(0.25) Cl4(0.25) N8(0.5) C14(0.5) H14(0.5) C13(0.5) C15(0.5)
 H15(0.5) C17(0.5) H17(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C3(H3), C6(H6), C12(H12), C1(H1), C10(H10),
 C9(H9), C11(H11), C5(H5), C4(H4), C7(H7), C8(H8)
;
_shelx_res_checksum              19508
_shelx_hkl_checksum              4121
_shelx_fab_checksum              6355
_olex2_submission_special_instructions 'No special instructions were received'