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_1572191
_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 Dy N'
_chemical_formula_sum            'C26 H38 Dy N'
_chemical_formula_weight         527.07
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.34360(10)
_cell_length_b                   15.2429(2)
_cell_length_c                   16.38150(10)
_cell_measurement_reflns_used    13664
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      79.7040
_cell_measurement_theta_min      2.9020
_cell_volume                     2307.42(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -19.00  74.00   0.50    0.07    --   47.10 -87.00-139.00  186
  2  \w   -163.00 -81.00   0.50    0.27    --  -91.75 -87.00-139.00  164
  3  \w    -78.00 -19.00   0.50    0.27    --  -91.75  87.00 -22.00  118
  4  \w    103.00 178.00   0.50    0.27    --  113.25  87.00 -22.00  150
  5  \w     42.00 104.00   0.50    0.27    --  113.25 -87.00-139.00  124
  6  \w    -47.00  26.00   0.50    0.07    --  -47.10  37.00  90.00  146
  7  \w    -39.00  28.00   0.50    0.07    --  -47.10  19.00 -30.00  134
  8  \w    -74.00  26.00   0.50    0.07    --  -47.10  87.00 -22.00  200
  9  \w     36.00  93.00   0.50    0.07    --   47.10-125.00  60.00  114
 10  \w    -53.00 -20.00   0.50    0.27    --  -91.75  45.00 120.00   66
 11  \w    101.00 178.00   0.50    0.27    --  113.25  30.00 -90.00  154
 12  \w     42.00  69.00   0.50    0.27    --  113.25 -61.00 -90.00   54
 13  \w     42.00  94.00   0.50    0.27    --  113.25 -77.00 120.00  104
 14  \w     42.00  94.00   0.50    0.27    --  113.25 -77.00 -90.00  104
 15  \w     42.00  69.00   0.50    0.27    --  113.25 -61.00  90.00   54
 16  \w     42.00  69.00   0.50    0.27    --  113.25 -61.00-150.00   54
 17  \w     44.00 108.00   0.50    0.27    --  113.25-125.00  90.00  128
 18  \w     42.00  69.00   0.50    0.27    --  113.25 -61.00 -60.00   54
 19  \w     42.00  94.00   0.50    0.27    --  113.25 -77.00 -60.00  104
 20  \w    106.00 178.00   0.50    0.27    --  113.25  61.00 150.00  144
 21  \w     42.00  94.00   0.50    0.27    --  113.25 -77.00-120.00  104
 22  \w     42.00  69.00   0.50    0.27    --  113.25 -61.00 150.00   54
 23  \w    101.00 178.00   0.50    0.27    --  113.25  30.00 120.00  154
 24  \w    110.00 178.00   0.50    0.27    --  113.25  77.00  30.00  136
 25  \w     42.00  69.00   0.50    0.27    --  113.25 -61.00 -30.00   54
 26  \w     42.00  94.00   0.50    0.27    --  113.25 -77.00   0.00  104
 27  \w    110.00 178.00   0.50    0.27    --  113.25  77.00-180.00  136
 28  \w     47.00  99.00   0.50    0.27    --  113.25 -94.00  90.00  104
 29  \w     42.00  74.00   0.50    0.27    --  113.25 -77.00  60.00   64
;
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.274
_diffrn_reflns_theta_min         3.982
_exptl_absorpt_coefficient_mu    17.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.100a (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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0551P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4473
_reflns_number_total             4967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03786c2.cif
_cod_data_source_block           Cpstar2DyDMP
_cod_depositor_comments
'Adding full bibliography for 1572175--1572199.cif.'
_cod_database_code               1572191
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.198
_shelx_estimated_absorpt_t_min   0.084
_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:
 C3(H3), C2(H2)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C15(H15A,H15B,
 H15C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C16(H16A,
 H16B,H16C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C)
;
_shelx_res_checksum              2615
_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
- Detector area scaling
;