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_1572175
_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 Dy I4 N, C H2 Cl2'
_chemical_formula_sum            'C25 H32 Cl2 Dy I4 N'
_chemical_formula_weight         1087.51
_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             2023-07-10
_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                 101.444(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3100(2)
_cell_length_b                   14.2475(2)
_cell_length_c                   21.2431(4)
_cell_measurement_reflns_used    22638
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.8950
_cell_measurement_theta_min      2.8590
_cell_volume                     3058.40(10)
_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 2018/2 (Sheldrick, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.839
_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      4.00  29.00   0.50    1.50    --    6.58 -78.00 129.00   50
  2  \w    -39.00 -12.00   0.50    1.50    --   -7.98 -78.00 129.00   54
  3  \w    -28.00  19.00   0.50    1.50    --   -7.98  78.00-104.00   94
  4  \w      0.00  35.00   0.50    1.50    --    6.58 -99.00 120.00   70
  5  \w      6.00  39.00   0.50    1.50    --    6.58 -99.00-120.00   66
  6  \w    -11.00  15.00   0.50    1.50    --    6.58 -77.00  60.00   52
  7  \w      2.00  38.00   0.50    1.50    --    6.58  57.00 -90.00   72
  8  \w    -31.00   7.00   0.50    1.50    --   -7.98 -57.00  30.00   76
  9  \w    -23.00  15.00   0.50    1.50    --   -7.98  77.00 -60.00   76
 10  \w    -28.00   7.00   0.50    1.50    --   -7.98 -57.00  60.00   70
 11  \w    -15.00  15.00   0.50    1.50    --   -7.98 -77.00 -30.00   60
;
_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      0.0372990000
_diffrn_orient_matrix_UB_12      0.0410624000
_diffrn_orient_matrix_UB_13      0.0100428000
_diffrn_orient_matrix_UB_21      0.0050652000
_diffrn_orient_matrix_UB_22      0.0091144000
_diffrn_orient_matrix_UB_23      -0.0322487000
_diffrn_orient_matrix_UB_31      -0.0592429000
_diffrn_orient_matrix_UB_32      0.0266365000
_diffrn_orient_matrix_UB_33      -0.0044502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37524
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.718
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.671
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.218
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_description       plate
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.622
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         8694
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0382P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7485
_reflns_number_total             8694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03786c2.cif
_cod_data_source_block           Cpstar2DyTIP100K
_cod_depositor_comments
'Adding full bibliography for 1572175--1572199.cif.'
_cod_database_code               1572175
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H32Cl2DyI4N
_shelx_estimated_absorpt_t_max   0.525
_shelx_estimated_absorpt_t_min   0.202
_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
Cl1B \\sim Cl1A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
3. Others
 Fixed Sof: Cl1A(0.5) H26C(0.5) H26D(0.5) H26A(0.5) H26B(0.5) Cl1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26C,H26D), C26(H26A,H26B)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              64725
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.475
_oxdiff_exptl_absorpt_empirical_full_min 0.675