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_7130529
_publ_section_title
;
 \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         'C50 H53 Fe N4 P, C6 H18 O Si2'
_chemical_formula_sum            'C56 H71 Fe N4 O P Si2'
_chemical_formula_weight         959.16
_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             2022-06-04
_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                 92.99
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0209(2)
_cell_length_b                   24.1592(3)
_cell_length_c                   17.9381(2)
_cell_measurement_reflns_used    33518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.16
_cell_volume                     5202.41(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100'
_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  ed88s
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            83142
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.033
_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    0.409
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7079
_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    1.225
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2048
_exptl_crystal_id                ed88s
_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 -2 -7) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         12903
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0414P)^2^+3.0912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11217
_reflns_number_total             12903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03260k2.cif
_cod_data_source_block           ed88s
_cod_database_code               7130529
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.910
_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. Uiso/Uaniso restraints and constraints 
C51A \\sim C51: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 
0.08 within 1.7A 
C56 \\sim C56A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 
0.08 within 1.7A 
3. Others 
 Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1) 
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1) 
 Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=1-FVAR(2) 
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(2) 
4.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) 
4.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), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), 
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B, 
 H55C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C), C51A(H51D,H51E,H51F), 
 C56A(H56D,H56E,H56F) 
;
_olex2_submission_special_instructions 'No special instructions were received'