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_1572194
_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         'C24 H30 I4 N Y, C H2 Cl2'
_chemical_formula_sum            'C25 H32 Cl2 I4 N Y'
_chemical_formula_weight         1013.92
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.465(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.30610(10)
_cell_length_b                   14.2414(2)
_cell_length_c                   21.2495(4)
_cell_measurement_reflns_used    10856
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      79.4960
_cell_measurement_theta_min      3.7570
_cell_volume                     3056.63(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.894
_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    -58.00 -33.00   0.50    0.46    --  -91.75  52.00 -11.00   50
  2  \w    -61.00 -16.00   0.50    0.11    --  -47.33 125.00 120.00   90
  3  \w    -60.00  25.00   0.50    0.11    --  -47.33  52.00 -11.00  170
  4  \w    -52.00 -22.00   0.50    0.46    --  -91.75  45.00 -60.00   60
  5  \w   -119.00 -35.00   0.50    0.11    --  -47.33 -52.00-156.00  168
  6  \w   -143.00-117.00   0.50    0.46    --  -91.75 -52.00-156.00   52
  7  \w   -157.00-112.00   0.50    0.46    --  -91.75 -77.00 -30.00   90
  8  \w     46.00  92.00   0.50    0.46    --  113.25 -77.00 150.00   92
  9  \w     46.00  93.00   0.50    0.46    --  113.25 -77.00  90.00   94
 10  \w     42.00  92.00   0.50    0.46    --  113.25 -77.00 120.00  100
 11  \w     43.00  72.00   0.50    0.46    --  113.25 -77.00 -90.00   58
 12  \w     42.00  67.00   0.50    0.46    --  113.25 -77.00-150.00   50
 13  \w     43.00  82.00   0.50    0.46    --  113.25 -77.00-180.00   78
 14  \w     42.00  67.00   0.50    0.46    --  113.25 -61.00 -90.00   50
 15  \w     52.00  77.00   0.50    0.46    --  113.25 -77.00 -60.00   50
 16  \w     42.00  67.00   0.50    0.46    --  113.25 -61.00   0.00   50
 17  \w     42.00  67.00   0.50    0.46    --  113.25 -61.00  60.00   50
 18  \w     42.00  67.00   0.50    0.46    --  113.25 -61.00  90.00   50
 19  \w     42.00  69.00   0.50    0.46    --  113.25 -61.00 -60.00   54
 20  \w      7.00  44.00   0.50    0.11    --   47.33 -52.00-156.00   74
 21  \w     42.00  67.00   0.50    0.46    --  113.25 -61.00-180.00   50
 22  \w     79.00 104.00   0.50    0.46    --  113.25 -94.00-180.00   50
 23  \w     47.00  84.00   0.50    0.46    --  113.25 -94.00-120.00   74
 24  \w     62.00  89.00   0.50    0.11    --   47.33-125.00  60.00   54
 25  \w    121.00 148.00   0.50    0.46    --  113.25  77.00 -90.00   54
 26  \w    151.00 176.50   0.50    0.46    --  113.25  77.00 -90.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17339
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.276
_diffrn_reflns_theta_min         3.760
_exptl_absorpt_coefficient_mu    36.121
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.382
_refine_diff_density_min         -2.176
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5979
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5186
_reflns_number_total             5979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03786c2.cif
_cod_data_source_block           Cpstar2YTIP
_cod_depositor_comments
'Adding full bibliography for 1572175--1572199.cif.'
_cod_database_code               1572194
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.220
_shelx_estimated_absorpt_t_min   0.052
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl3A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
3. Others
 Fixed Sof: Cl3A(0.5) H26C(0.5) H26D(0.5) H26A(0.5) H26B(0.5) Cl2A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26C,H26D), C26(H26A,H26B)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C21(H21A,H21B,
 H21C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              9033
_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
;