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_7130526
_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         'C94 H88 Fe2 N10, C7 H16, 1.25[C6H14]'
_chemical_formula_sum            'C101 H104 Fe2 N10'
_chemical_formula_weight         1569.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.0060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2588(3)
_cell_length_b                   25.6179(5)
_cell_length_c                   23.7754(5)
_cell_measurement_reflns_used    48170
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.23
_cell_volume                     9288.1(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  ed41q
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17029
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_min         1.889
_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    0.362
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       prism
_exptl_crystal_F_000             3328
_exptl_crystal_id                ed41q
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-5 -4 -4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1060
_refine_ls_number_reflns         17029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0392P)^2^+7.2159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14375
_reflns_number_total             17029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03260k2.cif
_cod_data_source_block           ed41q
_cod_database_code               7130526
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Secondary CH2 refined with riding coordinates: 
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B) 
2.b Aromatic/amide H refined with riding coordinates: 
 C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C6A(H6A), 
 C6B(H6B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C12A(H12A), 
 C12B(H12B), C16A(H16A), C16B(H16B), C17A(H17A), C17B(H17B), C18A(H18A), 
 C18B(H18B), C19A(H19A), C19B(H19B), C24A(H24A), C24B(H24B), C27A(H27A), 
 C27B(H27B), C33A(H33A), C33B(H33B), C36A(H36A), C36B(H36B), C42A(H42A), 
 C42B(H42B), C45A(H45A), C45B(H45B) 
2.c Idealised Me refined as rotating group: 
 C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F), C26A(H26A,H26B,H26C), C26B(H26D, 
 H26E,H26F), C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C32A(H32A,H32B,H32C), 
 C32B(H32D,H32E,H32F), C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C38A(H38A, 
 H38B,H38C), C38B(H38D,H38E,H38F), C41A(H41A,H41B,H41C), C41B(H41D,H41E,H41F), 
 C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F), C48(H48A,H48B,H48C), C54(H54A,H54B,
 H54C) 
;
_smtbx_masks_special_details
; 
A solvent mask was calculated and 256 electrons were found in a 
volume of 1616\%A^3^ in void per asymmetric unit. This is consistent 
with the presence of 1.25 hexane solvate molecules per asymmetric 
unit which account for 250 electrons per unit cell. 
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'