Cooperative Bond Activations by a Tucked-In Iron Complex
Zurakowski, Joseph A.; Drover, Marcus W.; Chemical Communications  (2023) –; doi:10.1039/D3CC03325B

data_7132018
_publ_section_title
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 Cooperative Bond Activations by a Tucked-In Iron Complex
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03325B
_journal_year                    2023
_chemical_formula_moiety         'C24 H20 B, C24 H47 Fe N2 P2'
_chemical_formula_sum            'C48 H67 B Fe N2 P2'
_chemical_formula_weight         800.63
_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             2022-10-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2023-05-31 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                96.196(4)
_cell_angle_beta                 93.280(4)
_cell_angle_gamma                105.849(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4118(10)
_cell_length_b                   14.7221(14)
_cell_length_c                   15.2322(16)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.90
_cell_volume                     2223.8(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            94612
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.470
_diffrn_reflns_theta_min         2.960
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         9147
_refine_ls_number_restraints     1352
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0589P)^2^+2.9038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7065
_reflns_number_total             9147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03325b3.cif
_cod_data_source_block           1
_cod_database_code               7132018
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
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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. Restrained distances
 C13A-P2A = C16A-P2A = C19A-P2A = C22A-P2A
 0.01 with sigma of 1.879
3. Uiso/Uaniso restraints and constraints
C25A \\sim C25B \\sim C26A \\sim C26B \\sim C27A \\sim C27B \\sim C28A \\sim
C28B \\sim C29A \\sim C29B \\sim C30A \\sim C30B: within 2A with sigma of 0.008
and sigma for terminal atoms of 0.016 within 2A
C11A \\sim C11B \\sim C12A \\sim C12B \\sim C13A \\sim C13B \\sim C14A \\sim
C14B \\sim C15A \\sim C15B \\sim C16A \\sim C16B \\sim C17A \\sim C17B: within
2A with sigma of 0.008 and sigma for terminal atoms of 0.016 within 2A
C18A \\sim C18B \\sim C19A \\sim C19B \\sim C20A \\sim C20B \\sim C21A \\sim
C21B \\sim C22A \\sim C22B \\sim C23A \\sim C23B \\sim C24A \\sim C24B: within
2A with sigma of 0.008 and sigma for terminal atoms of 0.016 within 2A
P2A \\sim P2B: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016 within 2A
Uanis(C25A) \\sim Ueq, Uanis(C25B) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C26B) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C27B) \\sim Ueq,
Uanis(C28A) \\sim Ueq, Uanis(C28B) \\sim Ueq, Uanis(C29A) \\sim Ueq,
Uanis(C29B) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C30B) \\sim Ueq: with sigma
of 0.008 and sigma for terminal atoms of 0.016
Uanis(C11A) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C12A) \\sim Ueq,
Uanis(C12B) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C13B) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C14B) \\sim Ueq, Uanis(C15A) \\sim Ueq,
Uanis(C15B) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq,
Uanis(C17A) \\sim Ueq, Uanis(C17B) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
Uanis(C18A) \\sim Ueq, Uanis(C18B) \\sim Ueq, Uanis(C19A) \\sim Ueq,
Uanis(C19B) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C20B) \\sim Ueq,
Uanis(C21A) \\sim Ueq, Uanis(C21B) \\sim Ueq, Uanis(C22A) \\sim Ueq,
Uanis(C22B) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C23B) \\sim Ueq,
Uanis(C24A) \\sim Ueq, Uanis(C24B) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
Uanis(P2A) \\sim Ueq, Uanis(P2B) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{P2A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A,
C23A, C24A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P2B, C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B, C21B, C22B,
C23B, C24B}
6. Others
 Sof(P2B)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=
 Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=
 Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=
 Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=
 Sof(H23D)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(P2A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=
 Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=
 Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(C25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=
 Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30B)=1-FVAR(2)
 Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C11A(H11A,H11B), C12A(H12A,H12B), C13A(H13A,H13B), C14A(H14A,H14B), C16A(H16A,
 H16B), C17A(H17A,H17B), C19A(H19A,H19B), C20A(H20A,H20B), C22A(H22A,H22B),
 C23A(H23A,H23B), C11B(H11C,H11D), C12B(H12C,H12D), C13B(H13C,H13D), C14B(H14C,
 H14D), C16B(H16C,H16D), C17B(H17C,H17D), C19B(H19C,H19D), C20B(H20C,H20D),
 C22B(H22C,H22D), C23B(H23C,H23D)
7.b Aromatic/amide H refined with riding coordinates:
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B), C30B(H30B), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48)
7.c Fitted hexagon refined as free rotating group:
 C25A(C26A,C27A,C28A,C29A,C30A), C25B(C26B,C27B,C28B,C29B,C30B)
7.d Idealised Me refined with riding coordinates:
 C15A(H15A,H15B,H15C), C18A(H18A,H18B,H18C), C21A(H21A,H21B,H21C), C24A(H24A,
 H24B,H24C), C15B(H15D,H15E,H15F), C18B(H18D,H18E,H18F), C21B(H21D,H21E,H21F),
 C24B(H24D,H24E,H24F)
7.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C)
;
_shelx_res_checksum              14888
_shelx_hkl_checksum              14566
_olex2_submission_special_instructions 'No special instructions were received'