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_7047284
_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         'C21 H15 N3 O15 Sm2, H2 O'
_chemical_formula_sum            'C21 H17 N3 O16 Sm2'
_chemical_formula_weight         868.08
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc200114
_audit_creation_date             2018-03-16
_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                 94.069(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5749(9)
_cell_length_b                   11.2005(6)
_cell_length_c                   14.8295(8)
_cell_measurement_reflns_used    4658
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0020
_cell_measurement_theta_min      1.8800
_cell_volume                     2414.8(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 15.9974
_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     55.00 111.00   1.00    7.50    --   26.84 178.00 -30.00   56
  2  \w     57.00 115.00   1.00    7.50    --   26.84 178.00-180.00   58
  3  \w    -31.00  73.00   1.00    7.50    --   26.84   0.00 150.00  104
;
_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      -0.0120727000
_diffrn_orient_matrix_UB_12      -0.0606874000
_diffrn_orient_matrix_UB_13      -0.0075331000
_diffrn_orient_matrix_UB_21      0.0453580000
_diffrn_orient_matrix_UB_22      -0.0121861000
_diffrn_orient_matrix_UB_23      -0.0117842000
_diffrn_orient_matrix_UB_31      0.0133173000
_diffrn_orient_matrix_UB_32      -0.0132113000
_diffrn_orient_matrix_UB_33      0.0458947000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7913
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52792
_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    2.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.454
_refine_diff_density_min         -2.695
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                4513
_reflns_number_total             5257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02429d2.cif
_cod_data_source_block           m5_rt_mo
_cod_database_code               7047284
_chemical_oxdiff_formula         'C336 H304 N80 O224 Sm32'
_reflns_odcompleteness_completeness 98.71
_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:
 O32(H32A,H32B)
2.b Rotating group:
 O25(H25A,H25B), O40(H40A,H40B), O48(H48A,H48B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C0AA(H0AA), C15(H15), C20(H20), C25(H25), C48(H48), C57(H57),
 C62(H62), C68(H68)
;
_olex2_date_sample_data_collection 2016-12-15
_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 1.879
_oxdiff_exptl_absorpt_empirical_full_min 0.720