Disparate reactivity of a chiral iron(II) tetracarbene complex with organic azides.
Russell, Jerred J.; DeJesus, Joseph F.; Smith, Brett A.; Nalaoh, Phattananawee; Vogiatzis, Konstantinos D.; Jenkins, David M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10819–10823; doi:10.1039/d4dt01422g

data_7716355
_publ_section_title
;
 Disparate reactivity of a chiral iron(II) tetracarbene complex with
 organic azides.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10819
_journal_page_last               10823
_journal_paper_doi               10.1039/d4dt01422g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C36 H58 B2 Fe N10)'
_chemical_formula_sum            'C72 H116 B4 Fe2 N20'
_chemical_formula_weight         1416.78
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-09 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                105.924(8)
_cell_angle_beta                 97.804(8)
_cell_angle_gamma                98.957(8)
_cell_formula_units_Z            1
_cell_length_a                   11.847(3)
_cell_length_b                   12.104(3)
_cell_length_c                   16.289(5)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.50
_cell_volume                     2179.2(10)
_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, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            89349
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.247
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1242 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.8492.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.044(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         17677
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.9061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                16300
_reflns_number_total             17677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01422g3.cif
_cod_data_source_block           mo_jenkins_jerred_jr0221_0m
_cod_depositor_comments
'Adding full bibliography for 7716352--7716355.cif.'
_cod_original_cell_volume        2179.3(10)
_cod_database_code               7716355
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.956(12)
 0.044(12)
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:
 C1(H1), C6(H6), C28(H28), C29(H29), C38(H38), C43(H43), C60(H60), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
  C65(H65A,H65B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C19(H19), C20(H20),
 C44(H44), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C56(H56), C57(H57)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C54(H54A,H54B,H54C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              62625
_shelx_hkl_checksum              41938
_shelx_fab_checksum              83212
_olex2_submission_special_instructions 'No special instructions were received'