Amine-substituent induced highly selective and rapid "turn-on" detection of carcinogenic 1,4-dioxane from purely aqueous and vapour phase with novel post-synthetically modified d<sup>10</sup>-MOFs.
Mondal, Udayan; Bej, Sourav; Hazra, Abhijit; Mandal, Sukdeb; Pal, Tapan K.; Banerjee, Priyabrata; Dalton transactions (Cambridge, England : 2003) 51 (2022) 2083–2093; doi:10.1039/d1dt03976h

data_7709267
_publ_section_title
;
 Amine-substituent induced highly selective and rapid "turn-on" detection
 of carcinogenic 1,4-dioxane from purely aqueous and vapour phase with
 novel post-synthetically modified d<sup>10</sup>-MOFs.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2083
_journal_page_last               2093
_journal_paper_doi               10.1039/d1dt03976h
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C36 H46 Cd3 N7 O16'
_chemical_formula_sum            'C36 H46 Cd3 N7 O16'
_chemical_formula_weight         1170.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-12-20
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-12-27 deposited with the CCDC.	2022-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3983(4)
_cell_length_b                   10.3191(3)
_cell_length_c                   16.2707(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.099
_cell_measurement_theta_min      2.00
_cell_volume                     2173.03(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'BRUKER SMART APEX-II CCD'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22224
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.645
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6285
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             1166
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3827
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0359P)^2^+5.5364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3366
_reflns_number_total             3827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03976h2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7709267.cif.'
_cod_database_code               7709267
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9B-C16B \\sim O9B-C16A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O9B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.002 within
2A
Uanis(C18B) \\sim Ueq, Uanis(N2B) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C17B)
\\sim Ueq, Uanis(O9B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C16A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15B) \\sim Ueq, Uanis(N3B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(N3B) \\sim Ueq, Uanis(C15B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C17A, C16A, N2A, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2B, C16B, C17B, C18B, O9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: N4(0.5) H4A(0.5) H4B(0.5) H3(0.5) H11(0.5) O8A(0.5) N1A(0.5)
 H1AA(0.5) H1AB(0.5) N2A(0.75) N3A(0.5) C13A(0.5) H13A(0.5) C14A(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C15A(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C16A(0.75)
 H16A(0.75) C17A(0.75) H17A(0.75) H17B(0.75) H17C(0.75) C18A(0.75) H18A(0.75)
 H18B(0.75) H18C(0.75) O8B(0.5) N1B(0.5) N2B(0.25) N3B(0.5) C13B(0.5) H13B(0.5)
 C14B(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15B(0.5) H15D(0.5) H15E(0.5)
 H15F(0.5) C16B(0.25) H16B(0.25) C17B(0.25) H17D(0.25) H17E(0.25) H17F(0.25)
 C18B(0.25) H18D(0.25) H18E(0.25) H18F(0.25)
6.a Rotating group:
 N4(H4A,H4B), N1A(H1AA,H1AB), N1B(H1BA,H1BB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C13A(H13A), C16A(H16A),
 C13B(H13B), C16B(H16B)
6.c Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C17A(H17A,H17B,H17C), C18A(H18A,
 H18B,H18C), C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C17B(H17D,H17E,H17F),
 C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              4843
_olex2_submission_special_instructions 'No special instructions were received'