Synthesis of eight isostructural 2D lanthanide coordination polymers assembled by rigid furan-2,5-dicarboxylic acid and flexible adipic acid as linkers and exploration of luminescent Eu/Tb polymers as efficient and sensitive sensors for nitroaromatic compounds
Nisa, Zaib ul; Tashi, Lobzang; Sen, Charanjeet; Ashashi, Nargis Akhter; Sahoo, Subash Chandra; Sheikh, Haq Nawaz; New Journal of Chemistry 44 (2020) 8125–8137; doi:10.1039/D0NJ01018A

data_7059577
_publ_section_title
;
 Synthesis of eight isostructural 2D lanthanide coordination polymers
 assembled by rigid furan-2,5-dicarboxylic acid and flexible adipic acid
 as linkers and exploration of luminescent Eu/Tb polymers as efficient and
 sensitive sensors for nitroaromatic compounds
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8125
_journal_page_last               8137
_journal_paper_doi               10.1039/D0NJ01018A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C29 H21 N3 O9 Pb2, 0.5(C6 H15 N)'
_chemical_formula_sum            'C32 H28.5 N3.5 O9 Pb2'
_chemical_formula_weight         1020.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc23701f
_audit_creation_date             2019-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.181(2)
_cell_angle_beta                 97.698(2)
_cell_angle_gamma                94.222(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2850(3)
_cell_length_b                   13.3070(3)
_cell_length_c                   13.3260(3)
_cell_measurement_reflns_used    11400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5140
_cell_measurement_theta_min      1.9870
_cell_volume                     1756.90(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_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    -22.00  19.00   0.50   12.00    --   -6.40  77.00 -30.00   82
  2  \w     29.00  55.00   0.50   12.00    --   -6.40  77.00 -30.00   52
  3  \w     37.00  67.00   0.50   12.00    --   -6.40  77.00-120.00   60
  4  \w     26.00  58.00   0.50   12.00    --    7.80  77.00-150.00   64
  5  \w      3.00  61.00   0.50   12.00    --    7.80  77.00 -60.00  116
  6  \w    -18.00  12.00   0.50   12.00    --    7.80  77.00-150.00   60
  7  \w    -31.00  22.00   0.50   12.00    --   -6.40  77.00-120.00  106
  8  \w    -21.00  73.00   0.50   12.00    --    7.80  77.00  60.00  188
  9  \w      4.00  74.00   0.50   12.00    --    7.80  77.00 150.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195265000
_diffrn_orient_matrix_UB_12      -0.0495548000
_diffrn_orient_matrix_UB_13      -0.0193035000
_diffrn_orient_matrix_UB_21      0.0150404000
_diffrn_orient_matrix_UB_22      -0.0067474000
_diffrn_orient_matrix_UB_23      0.0515280000
_diffrn_orient_matrix_UB_31      -0.0654953000
_diffrn_orient_matrix_UB_32      -0.0224854000
_diffrn_orient_matrix_UB_33      -0.0029502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.988
_refine_diff_density_min         -2.172
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+10.7494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5999
_reflns_number_total             6999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01018a2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7059575--7059582.cif.

 Adding full bibliography for 7059575--7059582.cif.
;
_cod_original_formula_sum        'C32 H28.50 N3.50 O9 Pb2'
_cod_database_code               7059577
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Pb C O N H'
_shelx_estimated_absorpt_t_max   0.249
_shelx_estimated_absorpt_t_min   0.160
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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. Restrained distances
 N4-C30 = N4-C32 = N4-C34
 1.463 with sigma of 0.001
 N4-C31 = N4-C33 = N4-C35
 2.532 with sigma of 0.002
 C30-C32 = C32-C34 = C34-C30
 2.416 with sigma of 0.002
 C30-C31 = C32-C33 = C34-C35
 1.439 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) = Uanis(N4) = Uanis(C30) = Uanis(C32) = Uanis(C34) = Uanis(C31) =
Uanis(C33)
4. Others
 Fixed Sof: N4(0.5) C30(0.5) H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C16(H16), C12(H12), C20(H20), C13(H13), C5(H5), C11(H11),
 C18(H18), C25(H25), C23(H23), C24(H24), C26(H26), C10(H10), C27(H27)
5.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C31(H31A,H31B,
 H31C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              50149
_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 4.998
_oxdiff_exptl_absorpt_empirical_full_min 0.462