Highly selective luminescence sensing for the detection of nitrobenzene and Fe3+ by new Cd(ii)-based MOFs
Yan, Yang-Tian; Liu, Jiao; Yang, Guo-Ping; Zhang, Fang; Fan, Ya-Ke; Zhang, Wen-Yan; Wang, Yao-Yu; CrystEngComm 20 (2018) 477–; doi:10.1039/C7CE01920C

data_7229873
_publ_section_title
;
 Highly selective luminescence sensing for the detection of nitrobenzene
 and Fe3+ by new Cd(ii)-based MOFs
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              477
_journal_paper_doi               10.1039/C7CE01920C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C92 H72 Cd4 O52, 2.5(H2 O)'
_chemical_formula_sum            'C92 H77 Cd4 O54.5'
_chemical_formula_weight         2504.17
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-08-14 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.048(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0000(12)
_cell_length_b                   23.672(2)
_cell_length_c                   26.421(2)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.302
_cell_measurement_theta_min      2.324
_cell_volume                     8750.5(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            44356
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.155
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0792 before and 0.0513 after correction. The Ratio of minimum to maximum transmission is 0.8104. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5028
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1392
_refine_ls_number_reflns         15908
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+18.0245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13502
_reflns_number_total             15908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01920c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7229873--7229875.cif.'
_cod_original_formula_sum        'C92 H77 Cd4 O54.50'
_cod_database_code               7229873
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H44A-O44 = O44-H44B
 0.85 with sigma of 0.02
 H45A-O45 = O45-H45B
 0.85 with sigma of 0.02
 H50A-O50 = O50-H50B
 0.85 with sigma of 0.02
 H55A-O55 = O55-H55B
 0.85 with sigma of 0.02
 H54B-O54 = O54-H54A
 0.85 with sigma of 0.02
 H23A-O23 = O23-H23B
 0.85 with sigma of 0.02
 H24A-O24 = O24-H24B
 0.85 with sigma of 0.02
 H22B-O22 = O22-H22A
 0.85 with sigma of 0.02
 H43A-O43 = O43-H43B
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22)
\\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq,
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O29)
\\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq,
Uanis(O33) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O36)
\\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O39) \\sim Ueq,
Uanis(O40) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O43)
\\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O46) \\sim Ueq,
Uanis(O47) \\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(O50)
\\sim Ueq, Uanis(O51) \\sim Ueq, Uanis(O52) \\sim Ueq, Uanis(O52A) \\sim Ueq,
Uanis(O53) \\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O54) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
4. Rigid body (RIGU) restrains
 O12, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O52A)=Sof(H52C)=Sof(H52D)=1-FVAR(1)
 Sof(O52)=Sof(H52A)=Sof(H52B)=FVAR(1)
 Fixed Sof: H53A(0.5) H53B(0.5)
6.a Riding coordinates:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O22(H22A,H22B), O23(H23A,
 H23B), O24(H24A,H24B), O43(H43A,H43B), O44(H44A,H44B), O45(H45A,H45B),
 O50(H50A,H50B), O51(H51A,H51B), O52(H52A,H52B), O53(H53A,H53B)
6.b Rotating group:
 O52A(H52C,H52D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5A), C8(H8), C11(H11A), C12(H12), C14(H14), C15(H15), C17(H17), C24(H24),
 C27(H27), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C39(H39), C42(H42),
  C43(H43), C46(H46A), C49(H49), C52(H52), C54(H54), C56(H56), C62(H62),
 C65(H65), C67(H67), C69(H69), C73(H73), C74(H74), C76(H76), C79(H79), C82(H82),
  C83(H83), C84(H84), C86(H86), C89(H89), C92(H92)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5), O9(H9), O11(H11), O18(H18), O25(H25), O29(H29), O35(H35),
 O40(H40), O41(H41), O46(H46), O48(H48)
;
_shelx_res_checksum              30017
_olex2_submission_special_instructions 'No special instructions were received'