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_1572196
_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 Gd I4 N, C H2 Cl2'
_chemical_formula_sum            'C25 H32 Cl2 Gd I4 N'
_chemical_formula_weight         1082.26
_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             2023-05-10
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3396(2)
_cell_length_b                   14.3064(3)
_cell_length_c                   21.2014(4)
_cell_measurement_reflns_used    21684
_cell_measurement_temperature    99.8(6)
_cell_measurement_theta_max      31.5720
_cell_measurement_theta_min      2.8430
_cell_volume                     3075.22(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(6)
_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 0.828
_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    -28.00  19.00   0.50    1.56    --   -7.98  78.00 174.00   94
  2  \w    -28.00  -2.00   0.50    1.56    --   -7.98 -78.00  49.00   52
  3  \w    -15.00  14.00   0.50    1.56    --   -7.98 -77.00   0.00   58
  4  \w    -38.00   7.00   0.50    1.56    --   -7.98 -57.00 -60.00   90
  5  \w    -16.00   9.00   0.50    1.56    --   -7.98 -77.00 -90.00   50
  6  \w    -14.00  11.00   0.50    1.56    --   -7.98 -77.00-150.00   50
  7  \w      1.00  39.00   0.50    1.56    --    6.58 -99.00-180.00   76
  8  \w    -16.00  24.00   0.50    1.56    --    6.58 -77.00 -30.00   80
  9  \w    -26.00  15.00   0.50    1.56    --    6.58 -78.00  49.00   82
 10  \w     -6.00  31.00   0.50    1.56    --    6.58  57.00-150.00   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      0.0066257000
_diffrn_orient_matrix_UB_12      0.0153735000
_diffrn_orient_matrix_UB_13      0.0322888000
_diffrn_orient_matrix_UB_21      0.0407485000
_diffrn_orient_matrix_UB_22      -0.0390476000
_diffrn_orient_matrix_UB_23      0.0105795000
_diffrn_orient_matrix_UB_31      0.0564934000
_diffrn_orient_matrix_UB_32      0.0263781000
_diffrn_orient_matrix_UB_33      -0.0031281000
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36647
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.690
_diffrn_reflns_theta_min         2.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.361
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.065
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (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    2.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.135
_refine_diff_density_min         -2.207
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         8616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0297P)^2^+5.4165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7408
_reflns_number_total             8616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03786c2.cif
_cod_data_source_block           Cpstar2GdTIP
_cod_depositor_comments
'Adding full bibliography for 1572175--1572199.cif.'
_cod_database_code               1572196
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H32Cl2GdI4N
_shelx_estimated_absorpt_t_max   0.630
_shelx_estimated_absorpt_t_min   0.196
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C14(H14A,
 H14B,H14C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              75907
_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 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.679