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_7047283
_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         '0.25(C42 H30 N6 O30 Pr4), H2 O'
_chemical_formula_sum            'C10.5 H9.5 N1.5 O8.5 Pr'
_chemical_formula_weight         433.61
_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.cc2000wy
_audit_creation_date             2018-03-13
_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                75.375(7)
_cell_angle_beta                 83.809(7)
_cell_angle_gamma                69.205(7)
_cell_formula_units_Z            4
_cell_length_a                   8.8422(7)
_cell_length_b                   10.7274(8)
_cell_length_c                   18.8231(16)
_cell_measurement_reflns_used    5016
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8270
_cell_measurement_theta_min      2.1140
_cell_volume                     1614.7(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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9987
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_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    -52.00  66.00   1.00    6.50    --   26.84 -77.00 150.00  118
  2  \w    -52.00  66.00   1.00    6.50    --   26.84 -77.00 -90.00  118
  3  \w    -52.00  66.00   1.00    6.50    --   26.84 -77.00  30.00  118
;
_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      0.0054305000
_diffrn_orient_matrix_UB_12      0.0665255000
_diffrn_orient_matrix_UB_13      -0.0077628000
_diffrn_orient_matrix_UB_21      -0.0446776000
_diffrn_orient_matrix_UB_22      0.0183783000
_diffrn_orient_matrix_UB_23      -0.0324128000
_diffrn_orient_matrix_UB_31      -0.0730779000
_diffrn_orient_matrix_UB_32      0.0227965000
_diffrn_orient_matrix_UB_33      0.0201599000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9020
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.09
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89928
_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    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.348
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0901P)^2^+24.7250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1772
_reflns_number_gt                6074
_reflns_number_total             6968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02429d2.cif
_cod_data_source_block           1_rt_mo
_cod_original_formula_sum        'C10.50 H9.50 N1.50 O8.50 Pr'
_cod_database_code               7047283
_chemical_oxdiff_formula         'C52 H52 N8 O37 Pr4'
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 O1(H1A,H1B), O1AA(H1AB,H1AC)
2.b Rotating group:
 O3(H3A,H3B), O28(H28A,H28B), O30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C2AA(H2AA), C5(H5), C15(H15), C24(H24), C26(H26), C33(H33),
 C39(H39), C42(H42)
;
_olex2_date_sample_data_collection 2016-01-30
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.782