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_7716354
_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_absolute_configuration rmad
_chemical_formula_moiety         'C42 H54 B2 Fe N10'
_chemical_formula_sum            'C42 H54 B2 Fe N10'
_chemical_formula_weight         776.42
_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                84.431(5)
_cell_angle_beta                 71.236(3)
_cell_angle_gamma                66.087(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6416(15)
_cell_length_b                   13.0001(15)
_cell_length_c                   16.3745(19)
_cell_measurement_reflns_used    9154
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5305
_cell_measurement_theta_min      2.628
_cell_volume                     2143.4(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81837
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.548
_diffrn_reflns_theta_min         2.629
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 12659 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         28472
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                27191
_reflns_number_total             28472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01422g3.cif
_cod_data_source_block           jd_7_47_hex_freeze_0m_b
_cod_depositor_comments
'Adding full bibliography for 7716352--7716355.cif.'
_cod_database_code               7716354
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.866
_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 Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C13(H13), C14(H14), C15(H15), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41),
  C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C),
 C42(H42A,H42B,H42C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90582
_shelx_hkl_checksum              46630
_shelx_fab_checksum              9067
_olex2_submission_special_instructions 'No special instructions were received'