The ambiguous behaviour of diphosphines towards the quasilinear iron(i) complex [Fe(N(SiMe<sub>3</sub>)<sub>2</sub>)<sub>2</sub>]<sup>-</sup> - between inertness, P-C bond cleavage and C-C double bond isomerisation.
Werncke, Christian Gunnar; Müller, Igor; Chemical communications (Cambridge, England) 56 (2020) 2268–2271; doi:10.1039/c9cc08968c

data_7125835
_publ_section_title
;
 The ambiguous behaviour of diphosphines towards the quasilinear iron(i)
 complex [Fe(N(SiMe<sub>3</sub>)<sub>2</sub>)<sub>2</sub>]<sup>-</sup> -
 between inertness, P-C bond cleavage and C-C double bond isomerisation.
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2268
_journal_page_last               2271
_journal_paper_doi               10.1039/c9cc08968c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C36 H42 Fe N P2 Si2, C20 H40.48 K O8'
_chemical_formula_sum            'C56 H82.48 Fe K N O8 P2 Si2'
_chemical_formula_weight         1110.77
_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             2019-11-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-11-08 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                97.045(2)
_cell_angle_beta                 103.248(2)
_cell_angle_gamma                95.214(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1704(6)
_cell_length_b                   15.3361(7)
_cell_length_c                   15.4398(7)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.22
_cell_volume                     2989.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_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 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest D8'
_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  0.0451
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            93235
_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         26.807
_diffrn_reflns_theta_min         2.216
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1099 before and 0.0469 after correction. The Ratio of minimum to maximum transmission is 0.9347. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1185
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         12781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0273P)^2^+2.1936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10812
_reflns_number_total             12781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08968c2.cif
_cod_data_source_block           k18c6_feppbz_hmds
_cod_depositor_comments
'Adding full bibliography for 7125833--7125836.cif.'
_cod_database_code               7125835
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.819
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C0AA) = Uanis(C2AA)
Uanis(C1AA) = Uanis(C3AA)
3. Others
 Fixed Sof: H01Y(0.88) H(0.88) H5AA(0.12) HA(0.12) H01Z(0.88) HC(0.88)
 H6AA(0.12) HB(0.12) C01U(0.88) H01(0.88) HF(0.88) C01V(0.88) H0AA(0.88)
 HG(0.88) H1AA(0.88) HH(0.88) H7AA(0.12) HD(0.12) HK(0.88) H2AA(0.88) HE(0.12)
 H8AA(0.12) C01Y(0.88) H3AA(0.88) HN(0.88) C01Z(0.88) H4AA(0.88) HO(0.88)
 C1AA(0.12) H1AB(0.12) H1AC(0.12) H1AD(0.12) C3AA(0.12) H3AB(0.12) H3AC(0.12)
 H3AD(0.12) C0AA(0.12) H0AB(0.12) H0AC(0.12) H0AD(0.12) C2AA(0.12) H2AB(0.12)
 H2AC(0.12) H2AD(0.12)
4.a Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B), C014(H01C,H01D), C015(H01E,H01F), C016(H01G,H01H), C017(H01I,
 H01J), C019(H01K,H01L), C01A(H01M,H01N), C01E(H01O,H01P), C01I(H01Q,H01R),
 C01J(H01S,H01T), C01L(H01U,H01V), C01M(H01W,H01X), C01S(H01Y,H), C01S(H5AA,HA),
  C01T(H01Z,HC), C01T(H6AA,HB), C01U(H01,HF), C01V(H0AA,HG), C01W(H1AA,HH),
 C01W(H7AA,HD), C01X(HK,H2AA), C01X(HE,H8AA), C01Y(H3AA,HN), C01Z(H4AA,HO)
4.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C14(H14), C17(H17), C15(H15), C28(H28), C36(H36), C16(H16),
 C26(H26), C6(H6), C30(H30), C29(H29), C27(H27), C33(H33), C35(H35), C2(H2),
 C20(H20), C3(H3), C5(H5), C34(H34), C22(H22), C24(H24), C4(H4), C21(H21),
 C23(H23)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C),
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C1AA(H1AB,H1AC,H1AD), C3AA(H3AB,H3AC,
 H3AD), C0AA(H0AB,H0AC,H0AD), C2AA(H2AB,H2AC,H2AD)
;
_shelx_res_checksum              34630
_olex2_submission_special_instructions 'No special instructions were received'