Enhancing redox functionality in dinuclear europium complexes.
Suryadevara, Nithin; Bagio, Stanley; Hay, Moya A.; Gable, Robert W.; Boskovic, Colette; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9208–9218; doi:10.1039/d5dt00302d

data_7718613
_publ_section_title
;
 Enhancing redox functionality in dinuclear europium complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9208
_journal_page_last               9218
_journal_paper_doi               10.1039/d5dt00302d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C22 H21 Eu I2 N6), C2 H3 N, 1.5[C2H3N]'
_chemical_formula_sum            'C49 H49.5 Eu2 I4 N14.5'
_chemical_formula_weight         1653.05
_chemical_name_systematic        NS1-74B
_chemical_properties_physical    Air-sensitive,Moisture-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
_audit_creation_date             2024-07-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-01-29 deposited with the CCDC.	2025-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.433(3)
_cell_angle_beta                 93.699(3)
_cell_angle_gamma                100.407(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7226(4)
_cell_length_b                   15.0787(5)
_cell_length_c                   16.9543(6)
_cell_measurement_reflns_used    12945
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.5230
_cell_measurement_theta_min      3.0770
_cell_volume                     2835.60(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.938
_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    102.00 159.00   0.50    0.05    --  105.30  78.00 -82.00  114
  2  \w     93.00 177.00   0.50    0.05    --  105.30  45.00   0.00  168
  3  \w    115.00 176.00   0.50    0.05    --  105.30  45.00  60.00  122
  4  \w     35.00 105.00   0.50    0.05    --  105.30 -94.00 120.00  140
  5  \w     34.00 105.00   0.50    0.05    --  105.30 -94.00  60.00  142
  6  \w     35.00 104.00   0.50    0.05    --  105.30 -94.00  30.00  138
  7  \w     33.00 104.00   0.50    0.05    --  105.30 -94.00 -30.00  142
  8  \w     33.00 103.00   0.50    0.05    --  105.30 -94.00 -60.00  140
  9  \w     43.00 105.00   0.50    0.05    --  105.30 -94.00-120.00  124
 10  \w    -20.00  30.00   0.50    0.05    --   47.51 -19.00-120.00  100
 11  \w     33.00  98.00   0.50    0.05    --  105.30 -78.00 152.00  130
 12  \w    -20.00  56.00   0.50    0.05    --   47.51 -78.00 152.00  152
 13  \w    -24.00  30.00   0.50    0.05    --   47.51 -19.00 150.00  108
 14  \w    -63.00  21.00   0.50    0.05    --  -47.51  78.00 -82.00  168
 15  \w    -48.00 -19.00   0.50    0.05    --  -91.75  78.00 -82.00   58
 16  \w    -30.00  28.00   0.50    0.05    --  -47.51  19.00-150.00  116
 17  \w    -89.00 -63.00   0.50    0.05    --  -91.75  78.00 -82.00   52
 18  \w    -62.00  21.00   0.50    0.05    --  -47.51  57.00 150.00  166
 19  \w    -71.00 -23.00   0.50    0.05    --  -91.75  61.00 120.00   96
 20  \w    -46.00 -20.00   0.50    0.05    --  -91.75  45.00 120.00   52
 21  \w   -145.00 -80.00   0.50    0.05    --  -91.75 -78.00 152.00  130
 22  \w   -163.00 -91.00   0.50    0.05    --  -91.75 -45.00-120.00  144
 23  \w   -163.00 -85.00   0.50    0.05    --  -91.75 -45.00-180.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0064621000
_diffrn_orient_matrix_UB_12      -0.0553737000
_diffrn_orient_matrix_UB_13      0.0652087000
_diffrn_orient_matrix_UB_21      0.1152412000
_diffrn_orient_matrix_UB_22      0.0630221000
_diffrn_orient_matrix_UB_23      0.0463985000
_diffrn_orient_matrix_UB_31      -0.0690660000
_diffrn_orient_matrix_UB_32      0.0676222000
_diffrn_orient_matrix_UB_33      0.0501640000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29357
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.389
_diffrn_reflns_theta_min         2.709
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    33.132
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.051
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_description       block
_exptl_crystal_F_000             1566
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         11154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0749P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9568
_reflns_number_total             11154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00302d2.cif
_cod_data_source_block           ns1-74b-accn_dipe_crystal2
_cod_depositor_comments
'Adding full bibliography for 7718613--7718615.cif.'
_cod_original_cell_volume        2835.60(17)
_cod_original_formula_sum        'C49 H49.50 Eu2 I4 N14.50'
_cod_database_code               7718613
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C48H48Eu2I4N14
_chemical_oxdiff_usercomment     'orange crystal at 100K'
_shelx_estimated_absorpt_t_max   0.241
_shelx_estimated_absorpt_t_min   0.049
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C13(H13A,H13B), C1(H1A,H1B), C7(H7A,H7B), C29(H29A,H29B),
 C35(H35A,H35B)
1.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C19(H19), C21(H21), C28(H28), C10(H10), C41(H41), C15(H15),
 C27(H27), C20(H20), C9(H9), C26(H26), C43(H43), C34(H34), C12(H12), C25(H25),
 C37(H37), C5(H5), C40(H40), C31(H31), C42(H42), C18(H18), C6(H6), C4(H4),
 C38(H38), C39(H39), C33(H33), C32(H32), C3(H3), C17(H17), C16(H16)
1.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23025
_shelx_hkl_checksum              8071
_shelx_fab_checksum              36554
_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 1.518
_oxdiff_exptl_absorpt_empirical_full_min 0.623