Implementation of 2,2'-azobispyridine radical mono- and dianions in dinuclear rare earth metal complexes.
Delano, 4th, Francis; Demir, Selvan; Chemical communications (Cambridge, England) 60 (2024) 11702–11705; doi:10.1039/d4cc03222e

data_7133617
_publ_section_title
;
 Implementation of 2,2'-azobispyridine radical mono- and dianions in
 dinuclear rare earth metal complexes.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11702
_journal_page_last               11705
_journal_paper_doi               10.1039/d4cc03222e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C46 H60 N4 Y2'
_chemical_formula_sum            'C46 H60 N4 Y2'
_chemical_formula_weight         846.80
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-29 deposited with the CCDC.	2024-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9313(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.44889(8)
_cell_length_b                   17.36119(16)
_cell_length_c                   12.52981(12)
_cell_measurement_reflns_used    17151
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0510
_cell_measurement_theta_min      4.3270
_cell_volume                     2035.78(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_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    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9826
_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    117.00 147.00   0.50    0.69    --  107.11  37.00 -60.00   60
  2  \w    127.00 171.00   0.50    0.69    --  107.11  57.00-180.00   88
  3  \w    108.00 134.00   0.50    0.69    --  107.11  19.00 -90.00   52
  4  \w    151.00 177.00   0.50    0.69    --  107.11  57.00  60.00   52
  5  \w    146.00 177.00   0.50    0.69    --  107.11  37.00  90.00   62
  6  \w    133.00 159.00   0.50    0.69    --  107.11  57.00 150.00   52
  7  \w    115.00 141.00   0.50    0.69    --  107.11  37.00  90.00   52
  8  \w    153.00 178.00   0.50    0.69    --  107.11  19.00 -60.00   50
  9  \w    138.00 170.00   0.50    0.69    --  107.11  19.00 -90.00   64
 10  \w     97.00 144.00   0.50    0.69    --  107.11  19.00 -60.00   94
 11  \w     97.00 167.00   0.50    0.69    --  107.11  19.00-120.00  140
 12  \w    -43.00  25.00   0.50    0.17    --  -47.70  37.00 -90.00  136
 13  \w    -40.00 -13.00   0.50    0.69    --  -86.25  37.00-180.00   54
 14  \w    -36.00   6.00   0.50    0.17    --  -47.70  37.00 -30.00   84
 15  \w    107.00 149.00   0.50    0.69    --  107.11 125.00 -30.00   84
 16  \w    103.00 160.00   0.50    0.69    --  107.11  83.00 150.00  114
 17  \w     -8.00  25.00   0.50    0.17    --   47.70 -19.00  90.00   66
 18  \w    -27.00  23.00   0.50    0.17    --   47.70 -19.00  30.00  100
 19  \w    -27.00  11.00   0.50    0.17    --   47.70 -19.00 -30.00   76
 20  \w    -72.00  25.00   0.50    0.17    --  -47.70  83.00 150.00  194
 21  \w    -63.00 -38.00   0.50    0.69    --  -86.25  83.00 150.00   50
 22  \w    -81.00 -39.00   0.50    0.17    --  -47.70 125.00  60.00   84
 23  \w     78.00 103.00   0.50    0.69    --  107.11 -77.00 -60.00   50
 24  \w     40.00  65.00   0.50    0.69    --  107.11 -57.00-150.00   50
 25  \w     38.00  64.00   0.50    0.69    --  107.11 -57.00-120.00   52
 26  \w     38.00  64.00   0.50    0.69    --  107.11 -77.00 -60.00   52
 27  \w     35.00  64.00   0.50    0.69    --  107.11 -57.00   0.00   58
 28  \w     36.00  61.00   0.50    0.69    --  107.11 -57.00  30.00   50
 29  \w     36.00  65.00   0.50    0.69    --  107.11 -57.00  60.00   58
 30  \w     35.00  64.00   0.50    0.69    --  107.11 -57.00  90.00   58
 31  \w     63.00  89.00   0.50    0.69    --  107.11 -83.00  29.00   52
 32  \w     72.00 104.00   0.50    0.69    --  107.11 -99.00  30.00   64
 33  \w     38.00 103.00   0.50    0.69    --  107.11 -99.00 150.00  130
 34  \w     73.00 104.00   0.50    0.69    --  107.11 -99.00  90.00   62
 35  \w     35.00  60.00   0.50    0.69    --  107.11 -99.00  30.00   50
 36  \w     39.00  65.00   0.50    0.69    --  107.11 -99.00  90.00   52
 37  \w     48.00  95.00   0.50    0.69    --  107.11 -99.00 -30.00   94
 38  \w     40.00  75.00   0.50    0.69    --  107.11-125.00-120.00   70
 39  \w     80.00 105.00   0.50    0.69    --  107.11-125.00-120.00   50
 40  \w     74.00 103.00   0.50    0.69    --  107.11 -99.00-180.00   58
 41  \w     37.00  65.00   0.50    0.69    --  107.11-125.00-150.00   56
 42  \w    103.00 129.00   0.50    0.69    --  107.11 -83.00  29.00   52
 43  \w     29.00  60.00   0.50    0.17    --   47.70 -83.00  29.00   62
 44  \w    -18.00  21.00   0.50    0.17    --   47.70 -83.00  29.00   78
 45  \w   -104.00 -35.00   0.50    0.17    --  -47.70 -19.00 -60.00  138
 46  \w   -157.00-131.00   0.50    0.69    --  -86.25 -37.00-120.00   52
 47  \w   -141.00-116.00   0.50    0.69    --  -86.25 -37.00 -60.00   50
 48  \w   -148.00-120.00   0.50    0.69    --  -86.25 -37.00 -30.00   56
 49  \w   -159.00-116.00   0.50    0.69    --  -86.25 -37.00  30.00   86
 50  \w   -159.00-123.00   0.50    0.69    --  -86.25 -37.00  90.00   72
 51  \w   -156.00-119.00   0.50    0.69    --  -86.25 -83.00  29.00   74
;
_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      0.1637335000
_diffrn_orient_matrix_UB_12      0.0003350000
_diffrn_orient_matrix_UB_13      0.0043330000
_diffrn_orient_matrix_UB_21      -0.0076011000
_diffrn_orient_matrix_UB_22      -0.0778641000
_diffrn_orient_matrix_UB_23      -0.0594679000
_diffrn_orient_matrix_UB_31      -0.0152532000
_diffrn_orient_matrix_UB_32      0.0425574000
_diffrn_orient_matrix_UB_33      -0.1088834000
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26108
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.307
_diffrn_reflns_theta_min         4.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.074
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+3.0192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4089
_reflns_number_total             4239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03222e2.cif
_cod_data_source_block           Cptet4Y2abpy
_cod_depositor_comments
'Adding full bibliography for 7133617--7133618.cif.'
_cod_database_code               7133617
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H47N4Y2
_diffrn_oxdiff_digest_frames
;
01af40c0377ada60ae0e0170171f33c39c036943b76
;
_diffrn_oxdiff_digest_hkl
;
01c7a27c04d04d38c49785bdc10b392554fd2a
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C3(H3), C5(H5), C2(H2), C4(H4)
1.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C11(H11A,H11B,
 H11C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C20(H20A,
 H20B,H20C)
;
_shelx_res_checksum              63518
_shelx_hkl_checksum              31184
_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 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.783