Construction of intermolecular σ-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion.
Delano, 4th, Francis; Benner, Florian; Jang, Seoyun; Greer, Samuel M.; Demir, Selvan; Chemical science 15 (2024) 13389–13404; doi:10.1039/d4sc03786c

data_1572199
_publ_section_title
;
 Construction of intermolecular &#x3c3;-hole interactions in rare earth
 metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              13389
_journal_page_last               13404
_journal_paper_doi               10.1039/d4sc03786c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C26 H38 N Y'
_chemical_formula_sum            'C26 H38 N Y'
_chemical_formula_weight         454.504
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4832(6)
_cell_angle_gamma                90
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_cell_length_b                   15.24462(11)
_cell_length_c                   16.36886(11)
_cell_measurement_reflns_used    11781
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.7070
_cell_measurement_theta_min      2.7040
_cell_volume                     2305.89(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
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_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9813
_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    -76.00 -29.00   0.50    0.05    --  -47.10  93.00 164.00   94
  2  \w     -8.00  70.00   0.50    0.05    --   47.10 -93.00  52.00  156
  3  \w    -73.00 -48.00   0.50    0.05    --  -91.75  93.00 164.00   50
  4  \w   -148.00 -98.00   0.50    0.05    --  -91.75 -93.00  52.00  100
  5  \w    106.00 169.00   0.50    0.05    --  113.25  93.00 164.00  126
  6  \w     66.00  96.00   0.50    0.05    --  113.25 -93.00  52.00   60
  7  \w   -120.00 -56.00   0.50    0.05    --  -47.10 -37.00 -30.00  128
  8  \w    -39.00   3.00   0.50    0.05    --  -47.10  19.00 -60.00   84
  9  \w    -37.00  27.00   0.50    0.05    --  -47.10  19.00-120.00  128
 10  \w    -48.00 -23.00   0.50    0.05    --  -91.75  45.00  30.00   50
 11  \w    -53.00 -25.00   0.50    0.05    --  -91.75  45.00   0.00   56
 12  \w    -49.00 -23.00   0.50    0.05    --  -91.75  45.00 -60.00   52
 13  \w     53.00  78.00   0.50    0.05    --  113.25 -77.00-150.00   50
 14  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00 120.00   54
 15  \w     42.00  68.00   0.50    0.05    --  113.25 -61.00-180.00   52
 16  \w     43.00  92.00   0.50    0.05    --  113.25 -77.00 -90.00   98
 17  \w     77.00 103.00   0.50    0.05    --  113.25-125.00 150.00   52
 18  \w    132.00 175.00   0.50    0.05    --  113.25  77.00-150.00   86
 19  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00  30.00   50
 20  \w     46.00  92.00   0.50    0.05    --  113.25 -77.00 120.00   92
 21  \w     42.00  68.00   0.50    0.05    --  113.25 -61.00 -60.00   52
 22  \w     43.00  81.00   0.50    0.05    --  113.25 -94.00  90.00   76
 23  \w     97.00 168.00   0.50    0.05    --  113.25 125.00 -60.00  142
 24  \w    147.00 176.00   0.50    0.05    --  113.25  45.00 120.00   58
 25  \w    114.00 172.00   0.50    0.05    --  113.25  30.00-120.00  116
 26  \w    110.00 143.00   0.50    0.05    --  113.25  45.00 120.00   66
 27  \w     42.00  89.00   0.50    0.05    --  113.25 -77.00  90.00   94
 28  \w    128.00 162.00   0.50    0.05    --  113.25  15.00  60.00   68
 29  \w     43.00  69.00   0.50    0.05    --  113.25 -61.00 -90.00   52
 30  \w     44.00  69.00   0.50    0.05    --  113.25 -77.00-120.00   50
 31  \w     45.00  71.00   0.50    0.05    --  113.25 -77.00  60.00   52
 32  \w     43.00  68.00   0.50    0.05    --  113.25 -61.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9813
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19243
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9813
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         80.22
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    3.651
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             961.245
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.4833
_refine_diff_density_min         -0.3568
_refine_diff_density_rms         0.0663
_refine_ls_d_res_high            0.7823
_refine_ls_d_res_low             11.0987
_refine_ls_extinction_coef       0.00066(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0251
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.1280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4559
_reflns_number_total             4941
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc03786c2.cif
_cod_data_source_block           Cpstar2YDMP
_cod_depositor_comments
'Adding full bibliography for 1572175--1572199.cif.'
_cod_database_code               1572199
_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.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C6(H6a,H6b,H6c), C25(H25a,H25b,H25c), C14(H14a,H14b,
 H14c), C26(H26a,H26b,H26c), C13(H13a,H13b,H13c), C7(H7a,H7b,H7c), C15(H15a,
 H15b,H15c), C16(H16a,H16b,H16c), C27(H27a,H27b,H27c), C24(H24a,H24b,H24c),
 C17(H17a,H17b,H17c)
;
_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
;