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_7047288
_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_absolute_configuration ad
_chemical_formula_moiety         'C21 H13 Gd2 N3 O14, 1.33(H2 O)'
_chemical_formula_sum            'C21 H15.67 Gd2 N3 O15.33'
_chemical_formula_weight         869.87
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc200103
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   19.5746(2)
_cell_length_b                   19.5746(2)
_cell_length_c                   21.7740(3)
_cell_measurement_reflns_used    3965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1330
_cell_measurement_theta_min      2.2170
_cell_volume                     7225.28(14)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.895
_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    -24.00  97.00   1.00   66.00    --   26.84  19.00 -90.00  121
;
_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      -0.0125001000
_diffrn_orient_matrix_UB_12      -0.0377262000
_diffrn_orient_matrix_UB_13      0.0128484000
_diffrn_orient_matrix_UB_21      0.0234911000
_diffrn_orient_matrix_UB_22      0.0180993000
_diffrn_orient_matrix_UB_23      0.0263664000
_diffrn_orient_matrix_UB_31      -0.0322606000
_diffrn_orient_matrix_UB_32      0.0006620000
_diffrn_orient_matrix_UB_33      0.0142115000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4567
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71351
_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    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trigonal
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.351
_refine_diff_density_min         -2.554
_refine_diff_density_rms         0.250
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         3893
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          4.556
_refine_ls_shift/su_mean         0.155
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+104.8366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                3877
_reflns_number_total             3893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02429d2.cif
_cod_data_source_block           m3_rt_mo
_cod_original_cell_volume        7225.27(15)
_cod_database_code               7047288
_chemical_oxdiff_formula         'C189 H126 Gd18 N27 O141'
_reflns_odcompleteness_completeness 98.70
_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. Others
 Fixed Sof: H1A(0.33333) H1B(0.33333)
3.a Free rotating group:
 O1(H1A,H1B), O0AA(H0AA,H0AB)
3.b Rotating group:
 O39(H39A,H39B), O40(H40A,H40B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C20(H20), C8(H8), C16(H16), C18(H18), C4(H4), C32(H32), C28(H28),
 C30(H30)
;
_olex2_date_sample_data_collection 2016-12-12
_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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.812