2,5-Furandicarboxylic acid as a linker for lanthanide coordination polymers: the role of heteroaromatic π‒π stacking and hydrogen bonding
Kumar, Manesh; Sheikh, Haq Nawaz; Fraconetti, Antonio; Zaręba, Jan K.; Sahoo, Subash Chandra; Frontera, Antonio; New Journal of Chemistry 43 (2019) 2179–; doi:10.1039/C8NJ05701J

data_7058076
_publ_section_title
;
 2,5-Furandicarboxylic acid as a linker for lanthanide coordination
 polymers: the role of heteroaromatic \p--\p stacking and hydrogen bonding
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2179
_journal_paper_doi               10.1039/C8NJ05701J
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C21 H19 Eu2 N O19, C3 H7 N O, 2.25(H2 O)'
_chemical_formula_sum            'C24 H30.5 Eu2 N2 O22.25'
_chemical_formula_weight         1006.92
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-14
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2018-12-14 deposited with the CCDC.
2019-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3278(2)
_cell_length_b                   21.1127(3)
_cell_length_c                   15.6552(2)
_cell_measurement_reflns_used    24538
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.3900
_cell_measurement_theta_min      3.2950
_cell_volume                     3406.00(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.929
_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    -68.00  -3.00   0.50    8.00    --   -9.95 -55.00 -92.00  130
  2  \w      1.00  53.00   0.50    8.00    --   -9.95  55.00  50.00  104
  3  \w    -53.00 -23.00   0.50    8.00    --   10.22 -55.00 -92.00   60
  4  \w     20.00  70.00   0.50    8.00    --   10.22  55.00  50.00  100
  5  \w    -58.00 -32.00   0.50    8.00    --   -9.95 125.00   0.00   52
  6  \w    -45.00 -19.00   0.50    8.00    --   -9.95 125.00 150.00   52
  7  \w    -58.00  -4.00   0.50    8.00    --   -9.95 125.00  30.00  108
  8  \w    -49.00  20.00   0.50    8.00    --   10.22 -38.00 -30.00  138
  9  \w    -38.00  26.00   0.50    8.00    --   10.22 -57.00 150.00  128
 10  \w      4.00  59.00   0.50    8.00    --   10.22-125.00 -60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30388
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.416
_diffrn_reflns_theta_min         3.245
_exptl_absorpt_coefficient_mu    3.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       block
_exptl_crystal_F_000             1970
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.826
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7219
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+11.1327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6721
_reflns_number_total             7219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05701j2.cif
_cod_data_source_block           kasm-f3
_cod_depositor_comments
'Adding full bibliography for 7058075--7058079.cif.'
_cod_original_formula_sum        'C24 H30.50 Eu2 N2 O22.25'
_cod_database_code               7058076
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H22B-H23G
 2.3 with sigma of 0.02
 C23-H23C \\sim H23B-H23A
 with sigma of 0.02
3. Rigid bond restraints
 H24A, C24, H24B, H24C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Others
 Fixed Sof: C22A(0.35) H22A(0.35) C23(0.35) H23A(0.35) H23B(0.35) H23C(0.35)
 C24(0.35) H24A(0.35) H24B(0.35) H24C(0.35) C22(0.65) H22(0.65) C23A(0.65)
 H23D(0.65) H23E(0.65) H23F(0.65) C24A(0.65) H24D(0.65) H24E(0.65) H24F(0.65)
 O23(0.25) H23G(0.25) H23H(0.25)
6.a Riding coordinates:
 O22(H22B,H22C), O23(H23G,H23H)
6.b Free rotating group:
 O21(H21D,H21E)
6.c Rotating group:
 O17(H17A,H17B), O16(H16A,H16B), O18(H18A,H18B)
6.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C3(H3), C9(H9), C15(H15), C16(H16), C19(H19), C22A(H22A),
 C22(H22)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
;
_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
;