Towards frustration in Eu(II) Archimedean tessellations.
Chen, Hua; Manvell, Anna S.; Kubus, Mariusz; Dunstan, Maja A.; Lorusso, Giulia; Gracia, David; Jørgensen, Mike S B; Kegnæs, Søren; Wilhelm, Fabrice; Rogalev, Andrei; Evangelisti, Marco; Pedersen, Kasper S.; Chemical communications (Cambridge, England) 59 (2023) 1609–1612; doi:10.1039/d2cc06224k

data_7131107
_publ_section_title
;
 Towards frustration in Eu(II) Archimedean tessellations.
;
_journal_issue                   12
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1609
_journal_page_last               1612
_journal_paper_doi               10.1039/d2cc06224k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C25 H20 Eu I2 N5, C2 H3 N'
_chemical_formula_sum            'C27 H23 Eu I2 N6'
_chemical_formula_weight         837.27
_chemical_name_systematic
catena-[pentakis(mu-4,4'-bipyridine)-tetrakis-iodido-bis-europium(II))]
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2022-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                88.744(3)
_cell_angle_beta                 82.778(3)
_cell_angle_gamma                79.924(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0699(3)
_cell_length_b                   10.0551(4)
_cell_length_c                   19.0931(8)
_cell_measurement_reflns_used    15548
_cell_measurement_temperature    120.00(12)
_cell_measurement_theta_max      29.5800
_cell_measurement_theta_min      3.9020
_cell_volume                     1700.81(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_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    -13.00  85.00   1.00   41.16    --   11.03  37.00   0.00   98
  2  \w    -17.00  84.00   1.00   41.16    --   11.03  57.00  90.00  101
  3  \w     39.00 100.00   1.00   41.16    --   11.03 178.00 -60.00   61
  4  \w    -15.00  52.00   1.00   41.16    --   11.03 -99.00-150.00   67
  5  \w    -62.00  39.00   1.00   41.16    --   11.03 -57.00 -60.00  101
  6  \w    -42.00  21.00   1.00   41.16    --  -11.73 -77.00  60.00   63
  7  \w    -17.00  84.00   1.00   41.16    --   11.03  57.00-120.00  101
  8  \w    -36.00  63.00   1.00   41.16    --  -11.73  37.00  60.00   99
  9  \w    -42.00  21.00   1.00   41.16    --  -11.73 -77.00 150.00   63
 10  \w    -44.00  21.00   1.00   41.16    --  -11.73  77.00  60.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0752111000
_diffrn_orient_matrix_UB_12      -0.0185070000
_diffrn_orient_matrix_UB_13      0.0079193000
_diffrn_orient_matrix_UB_21      -0.0086062000
_diffrn_orient_matrix_UB_22      0.0597178000
_diffrn_orient_matrix_UB_23      0.0203025000
_diffrn_orient_matrix_UB_31      -0.0260089000
_diffrn_orient_matrix_UB_32      -0.0349934000
_diffrn_orient_matrix_UB_33      0.0304524000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37841
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.678
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_preparation
'The crystal was transferred directly from solution to polybutene oil and mounted on a nylon loop.,Magnetic properties'
_exptl_crystal_recrystallization_method
'An acetonitrile solution of EuI2 was layered with an acetonitrile solution of 4,4-bipyridine at -20C for 14 days.'
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.589
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         8644
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0246P)^2^+10.3959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6967
_reflns_number_total             8644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06224k2.cif
_cod_data_source_block           eui2bipy
_cod_depositor_comments
'Adding full bibliography for 7131107--7131108.cif.'
_cod_database_code               7131107
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C27H23EuI2N6
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.480
_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
2. Rigid bond restraints
 N5, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N5 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C24(H24),
  C25(H25), C21(H21), C22(H22)
4.b Fitted hexagon refined as free rotating group:
 C24(C25,N5,C21,C22,C23)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.352
_oxdiff_exptl_absorpt_empirical_full_min 0.785