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_7047286
_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         'C14 H10 Dy N2 O10, H2 O'
_chemical_formula_sum            'C14 H12 Dy N2 O11'
_chemical_formula_weight         546.76
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2000z1
_audit_creation_date             2018-03-15
_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                96.241(5)
_cell_angle_beta                 94.321(5)
_cell_angle_gamma                93.127(5)
_cell_formula_units_Z            2
_cell_length_a                   9.2117(6)
_cell_length_b                   9.5034(6)
_cell_length_c                   10.2696(6)
_cell_measurement_reflns_used    3631
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9640
_cell_measurement_theta_min      4.3430
_cell_volume                     889.37(10)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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      0.00  54.00   1.00    1.00    --   25.57 -57.00  60.00   54
  2  \w    -11.00 107.00   1.00    1.00    --   66.78 -77.00  60.00  118
  3  \w     90.00 128.00   1.00    1.00    --  108.00 -65.00   0.00   38
  4  \w    123.00 153.00   1.00    1.00    --  108.00 -89.00 -60.00   30
  5  \w    118.00 156.00   1.00    1.00    --  108.00 -89.00-120.00   38
  6  \w     70.00 131.00   1.00    1.00    --  108.00 -89.00   0.00   61
  7  \w     47.00 123.00   1.00    1.00    --  108.00-129.00 -95.86   76
  8  \w     32.00  67.00   1.00    1.00    --  108.00 -65.00   0.00   35
  9  \w     29.00  54.00   1.00    1.00    --  108.00 -89.00   0.00   25
 10  \w     23.00 104.00   1.00    1.00    --  108.00 -89.00 -60.00   81
 11  \w     26.00 104.00   1.00    1.00    --  108.00 -89.00-120.00   78
 12  \w     54.00 144.00   1.00    1.00    --  108.00  32.00-120.00   90
 13  \w    149.00 178.00   1.00    1.00    --  108.00  43.00 -90.00   29
 14  \w    120.00 169.00   1.00    1.00    --  108.00 104.00  30.00   49
 15  \w    124.00 151.00   1.00    1.00    --  108.00  54.00 120.00   27
 16  \w    100.00 145.00   1.00    1.00    --   66.78 111.00 150.00   45
 17  \w    109.00 144.00   1.00    1.00    --   66.78 154.00 112.00   35
 18  \w     92.00 142.00   1.00    1.00    --   66.78 178.00   0.00   50
 19  \w    103.00 178.00   1.00    1.00    --  108.00 138.00 -90.00   75
 20  \w    117.00 178.00   1.00    1.00    --  108.00  43.00-180.00   61
 21  \w    104.00 139.00   1.00    1.00    --   66.78 111.00 -30.00   35
 22  \w    102.00 175.00   1.00    1.00    --  108.00 104.00 -60.00   73
 23  \w     84.00 131.00   1.00    1.00    --  108.00  43.00 -90.00   47
 24  \w     66.00 149.00   1.00    1.00    --  108.00  43.00   0.00   83
 25  \w     78.00 104.00   1.00    1.00    --   66.78 154.00 112.00   26
 26  \w     70.00 107.00   1.00    1.00    --  108.00  54.00 120.00   37
 27  \w     69.00 173.00   1.00    1.00    --  108.00  43.00  90.00  104
 28  \w    -12.00 107.00   1.00    1.00    --   66.78 -45.00-150.00  119
 29  \w    -15.00 148.00   1.00    1.00    --   66.78 -15.00  30.00  163
 30  \w    -39.00  -3.00   1.00    1.00    --   25.57 -57.00  60.00   36
 31  \w    -44.00  59.00   1.00    1.00    --   25.57 -57.00 -60.00  103
 32  \w    -45.00  53.00   1.00    1.00    --   25.57 -77.00-150.00   98
;
_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      0.1635620000
_diffrn_orient_matrix_UB_12      0.0395197000
_diffrn_orient_matrix_UB_13      -0.0062521000
_diffrn_orient_matrix_UB_21      0.0166055000
_diffrn_orient_matrix_UB_22      0.0382507000
_diffrn_orient_matrix_UB_23      0.1502666000
_diffrn_orient_matrix_UB_31      0.0348418000
_diffrn_orient_matrix_UB_32      -0.1538658000
_diffrn_orient_matrix_UB_33      0.0175298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5221
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.35
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19447
_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    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.079
_refine_diff_density_max         8.343
_refine_diff_density_min         -9.150
_refine_diff_density_rms         0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.303
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.008
_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          0.2635
_refine_ls_wR_factor_ref         0.2656
_reflns_number_gt                3053
_reflns_number_total             3122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02429d2.cif
_cod_data_source_block           m2_rt_cu
_cod_original_cell_volume        889.37(9)
_cod_database_code               7047286
_chemical_oxdiff_formula         'C28 H26 Dy2 N4 O24'
_reflns_odcompleteness_completeness 98.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O15(H15A,H15B)
2.b Rotating group:
 O4(H4A,H4B), O3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C15(H15), C19(H19), C25(H25), C31(H31)
;
_olex2_date_sample_data_collection 2016-09-02
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.697
_oxdiff_exptl_absorpt_empirical_full_min 0.518