A series of 3D lanthanide coordination polymers decorated with a rigid 3,5-pyridinedicarboxylic acid linker: syntheses, structural diversity, DFT study, Hirshfeld surface analysis, luminescence and magnetic properties
Kumar, Manesh; Kariem, Mukaddus; Sheikh, Haq Nawaz; Frontera, Antonio; Seth, Saikat Kumar; Jassal, Amanpreet Kaur; Dalton Transactions  (2018) –; doi:10.1039/C8DT02429D

data_7047287
_publ_section_title
;
 A series of 3D lanthanide coordination polymers decorated with a rigid
 3,5-pyridinedicarboxylic acid linker: syntheses, structural diversity,
 DFT study, Hirshfeld surface analysis, luminescence and magnetic
 properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT02429D
_journal_year                    2018
_chemical_formula_moiety         'C23 H18 Eu2 N3 O16, 2(H2 O), C3 H7 N O'
_chemical_formula_sum            'C26 H29 Eu2 N4 O19'
_chemical_formula_weight         1005.45
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2000y0
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 129.27(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.082(3)
_cell_length_b                   20.2060(11)
_cell_length_c                   20.535(4)
_cell_measurement_reflns_used    4648
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0820
_cell_measurement_theta_min      2.2800
_cell_volume                     3239(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9987
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_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    -10.00 103.00   1.00   10.70    --   26.92  77.00 -60.00  113
  2  \w    -49.00  59.00   1.00   10.70    --   26.92 -57.00  90.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0618857000
_diffrn_orient_matrix_UB_12      0.0081334000
_diffrn_orient_matrix_UB_13      0.0431688000
_diffrn_orient_matrix_UB_21      -0.0106410000
_diffrn_orient_matrix_UB_22      0.0340752000
_diffrn_orient_matrix_UB_23      -0.0107081000
_diffrn_orient_matrix_UB_31      -0.0654832000
_diffrn_orient_matrix_UB_32      0.0022928000
_diffrn_orient_matrix_UB_33      0.0035476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10796
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.0657
_exptl_crystal_size_min          0.0492
_refine_diff_density_max         5.143
_refine_diff_density_min         -7.347
_refine_diff_density_rms         0.595
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         7015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2540
_refine_ls_wR_factor_ref         0.2922
_reflns_number_gt                5412
_reflns_number_total             7015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02429d2.cif
_cod_data_source_block           g1_lt_mo
_cod_original_cell_volume        3238.3(11)
_cod_database_code               7047287
_chemical_oxdiff_formula         'C100 H100 Eu8 N16 O80 '
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2.a Free rotating group:
 O1AA(H1AA,H1AB), O2AA(H2AA,H2AB)
2.b Rotating group:
 O20(H20A,H20B), O28(H28A,H28B), O32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C75(H75), C20(H20), C65(H65), C83(H83), C107(H107), C111(H111), C5AA(H5AA),
 C10(H10), C5(H5), C6(H6), C4AA(H4AA)
2.d X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.728