Efficient carbene transfer reactivity mediated by Fe(II) complexes supported by bulky alkoxides.
Kulathungage, Lakshani W.; Kurup, Sudheer S.; Browne, Edison A.; Spalink, Gabriel H.; Ward, Cassandra L.; Lord, Richard L.; Groysman, Stanislav; Chemical communications (Cambridge, England) 60 (2024) 7033–7036; doi:10.1039/d4cc02108h

data_7133190
_publ_section_title
;
 Efficient carbene transfer reactivity mediated by Fe(II) complexes
 supported by bulky alkoxides.
;
_journal_issue                   55
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7033
_journal_page_last               7036
_journal_paper_doi               10.1039/d4cc02108h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C52 H76 Fe N2 O2'
_chemical_formula_sum            'C52 H76 Fe N2 O2'
_chemical_formula_weight         816.99
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-25 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                91.840(3)
_cell_angle_beta                 90.463(3)
_cell_angle_gamma                91.367(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5346(8)
_cell_length_b                   13.1604(12)
_cell_length_c                   18.8315(15)
_cell_measurement_reflns_used    5006
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.290
_cell_measurement_theta_min      2.166
_cell_volume                     2361.0(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.8 mm pinhole collimator'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1412
_diffrn_reflns_av_unetI/netI     0.1265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27533
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.363
_diffrn_reflns_theta_min         1.918
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.745209
_exptl_absorpt_correction_T_min  0.574295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1144 before and 0.0945 after correction.
 
For component 2:
 wR2(int) was 0.1156 before and 0.0963 after correction.
 The Ratio of minimum to maximum transmission is 0.77.

Final HKLF 4 output contains 81250 reflections, Rint = 0.1412
 (17444 with I > 3sig(I), Rint = 0.0821)
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.245
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         27533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.435
_refine_ls_R_factor_all          0.2119
_refine_ls_R_factor_gt           0.1598
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3966
_refine_ls_wR_factor_ref         0.4283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17586
_reflns_number_total             27533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02108h3.cif
_cod_data_source_block           sg13
_cod_depositor_comments
'Adding full bibliography for 7133190--7133192.cif.'
_cod_database_code               7133190
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.531(3)
 0.469(3)
2. 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
3.a Ternary CH refined with riding coordinates:
 C20(H20), C7(H7), C10(H10), C5(H5), C17(H17), C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C16(H16A,H16B), C19(H19A,H19B), C9(H9A,H9B), C14(H14A,H14B),
 C21(H21A,H21B), C8(H8A,H8B), C4(H4A,H4B), C22(H22A,H22B), C11(H11A,H11B),
 C18(H18A,H18B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C51(H51), C50(H50), C33(H33), C37(H37), C36(H36), C52(H52), C35(H35),
 C34(H34), C49(H49), C48(H48)
3.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C31(H31A,H31B,H31C), C40(H40A,
 H40B,H40C), C44(H44A,H44B,H44C), C27(H27A,H27B,H27C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              76590
_shelx_hkl_checksum              70306
_olex2_submission_special_instructions 'No special instructions were received'