γ-Agostic interactions in (MesCCC)Fe–Mes(L) complexes
Najera, Daniel C.; Peñas-Defrutos, Marconi N.; García-Melchor, Max; Fout, Alison R.; Chemical Communications  (2022) –; doi:10.1039/D2CC03260K

data_7130525
_publ_section_title
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 \g-Agostic interactions in (MesCCC)Fe--Mes(L) complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03260K
_journal_year                    2022
_chemical_formula_moiety         'C52 H49 Fe N5, 2(C7H8)'
_chemical_formula_sum            'C66 H65 Fe N5'
_chemical_formula_weight         984.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-05
_audit_creation_method
; 
Olex2 1.5 
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) 
;
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.9527(6)
_cell_length_b                   22.9527(6)
_cell_length_c                   43.0513(17)
_cell_measurement_reflns_used    18460
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.27
_cell_volume                     22680.6(12)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX3 V2019.11-0 (Bruker, 2019)'
_computing_data_reduction
; 
SAINT V8.40B, XPREP v2014/2, (Bruker, 2019), SADABS V2016/2 
(Krause et al., 2015) 
;
_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, 2015a)'
_computing_structure_solution    'SHELXT-2018-2 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ed27r
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            10393
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.380
_diffrn_reflns_theta_min         2.011
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.9930
_exptl_absorpt_correction_T_min  0.8453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             8352
_exptl_crystal_id                ed27r
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 3 -4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0432P)^2^+42.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7737
_reflns_number_total             10393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03260k2.cif
_cod_data_source_block           ed27r
_cod_original_cell_volume        22680.6(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7130525
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.939
_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), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C16(H16), 
 C17(H17), C18(H18), C19(H19), C24(H24), C27(H27), C33(H33), C36(H36), C42(H42), 
  C45(H45), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52) 
2.b Idealised Me refined as rotating group: 
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C32(H32A,H32B, 
 H32C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C44(H44A, 
 H44B,H44C) 
;
_smtbx_masks_special_details
; 
A solvent mask was calculated and 1746 electrons were found in a 
volume of 6747\%A^3^ in void per asymmetric unit. This is consistent 
with the presence of 2 toluene solvate molecules per asymmetric 
unit which account for 1600 electrons per unit cell. 
;
_smtbx_masks_void_probe_radius   1.5
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'