Controlled introduction of functional groups at one P atom in [Cp*Fe(<i>η</i><sup>5</sup>-P<sub>5</sub>)] and release of functionalised phosphines.
Reichl, Stephan; Riedlberger, Felix; Piesch, Martin; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical science 14 (2023) 7285–7290; doi:10.1039/d3sc01488f

data_1569246
_publ_section_title
;
 Controlled introduction of functional groups at one P atom in
 [Cp*Fe(<i>&#x3b7;</i><sup>5</sup>-P<sub>5</sub>)] and release of
 functionalised phosphines.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7285
_journal_page_last               7290
_journal_paper_doi               10.1039/d3sc01488f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '1(C29 H40 Fe P6)'
_chemical_formula_sum            'C29 H40 Fe P6'
_chemical_formula_weight         630.28
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-30
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                85.336(3)
_cell_angle_beta                 85.053(4)
_cell_angle_gamma                88.352(4)
_cell_formula_units_Z            4
_cell_length_a                   11.7026(6)
_cell_length_b                   14.3826(5)
_cell_length_c                   18.9471(7)
_cell_measurement_reflns_used    15905
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.5560
_cell_measurement_theta_min      3.7070
_cell_volume                     3165.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.48a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     21.00 115.00   1.00    5.00    --   45.15  57.00 -90.00   94
  2  \w    -24.00  69.00   1.00    5.00    --   45.15 -57.00 120.00   93
  3  \w    -21.00  75.00   1.00    5.00    --   45.15 -77.00   0.00   96
  4  \w     35.00  72.00   1.00   20.00    --  103.33 -45.00 -90.00   37
  5  \w     35.00  72.00   1.00   20.00    --  103.33 -45.00  30.00   37
  6  \w     81.00 175.00   1.00   20.00    --  103.33  33.00 147.82   94
  7  \w     31.00  57.00   1.00   20.00    --  103.33 -30.00 -30.00   26
  8  \w     32.00 112.00   1.00   20.00    --  103.33-125.00-150.00   80
  9  \w     22.00 107.00   1.00   20.00    --  103.33 -94.00   0.00   85
 10  \w     35.00  72.00   1.00   20.00    --  103.33 -45.00 150.00   37
 11  \w     97.00 175.00   1.00   20.00    --  103.33 125.00   0.00   78
 12  \w     32.00 112.00   1.00   20.00    --  103.33-125.00 -30.00   80
 13  \w     67.00 178.00   1.00   20.00    --  103.33  15.00  90.00  111
 14  \w     32.00 127.00   1.00   20.00    --  103.33 -77.00  30.00   95
 15  \w     16.00 115.00   1.00    5.00    --   45.15  72.00 152.66   99
 16  \w     15.00  42.00   1.00    5.00    --   45.15  76.00  85.20   27
 17  \w     15.00  42.00   1.00    5.00    --   45.15  78.00  38.60   27
 18  \w     78.00 173.00   1.00   20.00    --  103.33  61.00-180.00   95
 19  \w     80.00 172.00   1.00   20.00    --  103.33  45.00-120.00   92
 20  \w     80.00 172.00   1.00   20.00    --  103.33  45.00   0.00   92
 21  \w     80.00 176.00   1.00   20.00    --  103.33  30.00 -30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32841
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.574
_diffrn_reflns_theta_min         3.726
_exptl_absorpt_coefficient_mu    6.812
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.48a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         12335
_refine_ls_number_restraints     753
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0302P)^2^+13.5488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9948
_reflns_number_total             12335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01488f2.cif
_cod_data_source_block           tpabs_erroroff_gaus
_cod_depositor_comments
'Adding full bibliography for 1569243--1569247.cif.'
_cod_database_code               1569246
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.428
_shelx_estimated_absorpt_t_min   0.234
_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. Restrained distances
 C38B-C37B \\sim C36B-C37B \\sim C38B-C34B \\sim C35B-C34B \\sim C36B-C35B
 with sigma of 0.02
 C22B-C23B \\sim C23B-C18B \\sim C18B-C19B \\sim C19B-C20B \\sim C20B-C21B
\\sim C21B-C22B
 with sigma of 0.02
 P12A-C46A \\sim P12B-C46B
 with sigma of 0.02
 C58B-C53B \\sim C57B-C58B \\sim C57B-C56B \\sim C55B-C56B \\sim C54B-C55B
\\sim C53B-C54B
 with sigma of 0.04
 C15B-C16B \\sim C17B-C16B
 with sigma of 0.02
 P7-C44A \\sim P7-C44B
 with sigma of 0.02
 C7B-C8B \\sim C9B-C8B \\sim C7B-C6B \\sim C5B-C6B \\sim C6A-C5A \\sim C5B-C9B
\\sim C9A-C5A \\sim C9A-C8A
 \\sim C8A-C7A \\sim C6A-C7A
 with sigma of 0.02
 P10B-P11B \\sim P11A-P10A \\sim P9A-P10A \\sim P10B-P9B \\sim P9A-P8A \\sim
P8B-P9B
 with sigma of 0.02
 P11B-P7 \\sim P11A-P7 \\sim P8B-P7 \\sim P8A-P7
 with sigma of 0.02
 C40B-C36B \\sim C40B-C34B
 with sigma of 0.02
 C17B-C16B \\sim C17A-C16A \\sim C16A-C15A \\sim C15B-C16B
 with sigma of 0.02
 P6A-C17A \\sim P6B-C17B
 with sigma of 0.02
 P3A-P2 \\sim P3B-P2 \\sim P5B-P4B \\sim P4A-P5A \\sim P3B-P4B \\sim P3A-P4A
 with sigma of 0.02
 P1-P5B \\sim P1-P5A
 with sigma of 0.02
 C52B-C47B \\sim C52A-C47A \\sim C52B-C51B \\sim C52A-C51A \\sim C51B-C50B
\\sim C51A-C50A \\sim C50B-
 C49B \\sim C50A-C49A \\sim C49B-C48B \\sim C48A-C47A \\sim C48B-C47B \\sim
C49A-C48A
 with sigma of 0.02
 C25B-C24B \\sim C29B-C24B \\sim C29B-C28B \\sim C28B-C27B \\sim C27B-C26B
\\sim C26B-C25B \\sim C26A-
 C25A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C47B \\sim C52B \\sim C51B \\sim C50B \\sim C49B \\sim C48B \\sim C53B \\sim
C58B \\sim C57B \\sim C56B \\sim C55B \\sim C54B \\sim C53A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C15A \\sim C15B \\sim C16B \\sim C16A \\sim C17B \\sim C17A \\sim P6B \\sim P6A
\\sim C24B \\sim C29B \\sim C27B \\sim C26B \\sim C25B \\sim C28B \\sim C18B
\\sim C19B \\sim C20B \\sim C21B \\sim C22B \\sim C23B: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 1.7A
C46B \\sim C45B \\sim C44B \\sim C46A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C10B \\sim C5B \\sim C9B \\sim C14B \\sim C8B \\sim C13B \\sim C12B \\sim C7B
\\sim C6B \\sim C11B \\sim C6A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
P11A \\sim P11B \\sim P10A \\sim P10B \\sim P9A \\sim P9B \\sim P8B \\sim P8A:
within 2.5A with sigma of 0.02 and sigma for terminal atoms of 0.02 within 2.5A
C40B \\sim C35B \\sim C36B \\sim C41B \\sim C37B \\sim C42B \\sim C38B \\sim
C43B \\sim C34B \\sim C39B \\sim C36A: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.005 within 1.7A
P3B \\sim P3A \\sim P4B \\sim P4A \\sim P5B \\sim P5A: within 2.5A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
4. Others
 Fixed Sof: P8A(0.76) P12A(0.85) P10A(0.76) P5A(0.65) P9A(0.76) P6A(0.77)
 P4A(0.65) C38A(0.85) C58A(0.85) H58A(0.85) C48A(0.85) H48A(0.85) C29A(0.77)
 H29A(0.77) C35A(0.85) C49A(0.85) H49A(0.85) C34A(0.85) C23A(0.77) H23A(0.77)
 C47A(0.85) C7A(0.85) C36A(0.85) C53A(0.85) C28A(0.77) H28A(0.77) C15A(0.77)
 H15A(0.77) H15B(0.77) C5A(0.85) C27A(0.77) H27A(0.77) C6A(0.85) C37A(0.85)
 C8A(0.85) C25A(0.77) H25A(0.77) C9A(0.85) C44A(0.85) H44A(0.85) H44B(0.85)
 C26A(0.77) H26A(0.77) C24A(0.77) C52A(0.85) H52A(0.85) C57A(0.85) H57A(0.85)
 C18A(0.77) C45A(0.85) H45A(0.85) H45B(0.85) C43A(0.85) H43A(0.85) H43B(0.85)
 H43C(0.85) C16A(0.77) H16A(0.77) H16B(0.77) C19A(0.77) H19A(0.77) C56A(0.85)
 H56A(0.85) C20A(0.77) H20A(0.77) C46A(0.85) H46A(0.85) H46B(0.85) C50A(0.85)
 H50A(0.85) C40A(0.85) H40A(0.85) H40B(0.85) H40C(0.85) C54A(0.85) H54A(0.85)
 C17A(0.77) H17A(0.77) H17B(0.77) C39A(0.85) H39A(0.85) H39B(0.85) H39C(0.85)
 C22A(0.77) H22A(0.77) C51A(0.85) H51A(0.85) C55A(0.85) H55A(0.85) C12A(0.85)
 H12A(0.85) H12B(0.85) H12C(0.85) C42A(0.85) H42A(0.85) H42B(0.85) H42C(0.85)
 C10A(0.85) H10A(0.85) H10B(0.85) H10C(0.85) C21A(0.77) H21A(0.77) C11A(0.85)
 H11A(0.85) H11B(0.85) H11C(0.85) C13A(0.85) H13A(0.85) H13B(0.85) H13C(0.85)
 C14A(0.85) H14A(0.85) H14B(0.85) H14C(0.85) P3A(0.65) P6B(0.23) P12B(0.15)
 C6B(0.15) C9B(0.15) C5B(0.15) C7B(0.15) C8B(0.15) C11B(0.15) H11D(0.15)
 H11E(0.15) H11F(0.15) C14B(0.15) H14D(0.15) H14E(0.15) H14F(0.15) C10B(0.15)
 H10D(0.15) H10E(0.15) H10F(0.15) C12B(0.15) H12D(0.15) H12E(0.15) H12F(0.15)
 C13B(0.15) H13D(0.15) H13E(0.15) H13F(0.15) C41A(0.85) H41A(0.85) H41B(0.85)
 H41C(0.85) P11A(0.76) C17B(0.23) H17C(0.23) H17D(0.23) C16B(0.23) H16C(0.23)
 H16D(0.23) C15B(0.23) H15C(0.23) H15D(0.23) C45B(0.15) H45C(0.15) H45D(0.15)
 C46B(0.15) H46C(0.15) H46D(0.15) C44B(0.15) H44C(0.15) H44D(0.15) C37B(0.15)
 C34B(0.15) C38B(0.15) C35B(0.15) C36B(0.15) C42B(0.15) H42D(0.15) H42E(0.15)
 H42F(0.15) C39B(0.15) H39D(0.15) H39E(0.15) H39F(0.15) C43B(0.15) H43D(0.15)
 H43E(0.15) H43F(0.15) C41B(0.15) H41D(0.15) H41E(0.15) H41F(0.15) C40B(0.15)
 H40D(0.15) H40E(0.15) H40F(0.15) C50B(0.15) H50B(0.15) C49B(0.15) H49B(0.15)
 C48B(0.15) H48B(0.15) C47B(0.15) C52B(0.15) H52B(0.15) C51B(0.15) H51B(0.15)
 C56B(0.15) H56B(0.15) C55B(0.15) H55B(0.15) C54B(0.15) H54B(0.15) C53B(0.15)
 C58B(0.15) H58B(0.15) C57B(0.15) H57B(0.15) C22B(0.23) H22B(0.23) C23B(0.23)
 H23B(0.23) C18B(0.23) C19B(0.23) H19B(0.23) C20B(0.23) H20B(0.23) C21B(0.23)
 H21B(0.23) C24B(0.23) C25B(0.23) H25B(0.23) C26B(0.23) H26B(0.23) C27B(0.23)
 H27B(0.23) C28B(0.23) H28B(0.23) C29B(0.23) H29B(0.23) P3B(0.35) P4B(0.35)
 P5B(0.35) P9B(0.24) P8B(0.24) P10B(0.24) P11B(0.24)
5.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C44A(H44A,H44B), C45A(H45A,H45B), C16A(H16A,H16B), C46A(H46A,
 H46B), C17A(H17A,H17B), C17B(H17C,H17D), C16B(H16C,H16D), C15B(H15C,H15D),
 C45B(H45C,H45D), C46B(H46C,H46D), C44B(H44C,H44D)
5.b Aromatic/amide H refined with riding coordinates:
 C58A(H58A), C48A(H48A), C29A(H29A), C49A(H49A), C23A(H23A), C28A(H28A),
 C27A(H27A), C25A(H25A), C26A(H26A), C52A(H52A), C57A(H57A), C19A(H19A),
 C56A(H56A), C20A(H20A), C50A(H50A), C54A(H54A), C22A(H22A), C51A(H51A),
 C55A(H55A), C21A(H21A), C50B(H50B), C49B(H49B), C48B(H48B), C52B(H52B),
 C51B(H51B), C56B(H56B), C55B(H55B), C54B(H54B), C58B(H58B), C57B(H57B),
 C22B(H22B), C23B(H23B), C19B(H19B), C20B(H20B), C21B(H21B), C25B(H25B),
 C26B(H26B), C27B(H27B), C28B(H28B), C29B(H29B)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C4(H4A,H4B,H4C), C43A(H43A,H43B,H43C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C40A(H40A,H40B,H40C), C2(H2A,H2B,H2C), C39A(H39A,
 H39B,H39C), C12A(H12A,H12B,H12C), C42A(H42A,H42B,H42C), C10A(H10A,H10B,H10C),
 C3(H3A,H3B,H3C), C11A(H11A,H11B,H11C), C13A(H13A,H13B,H13C), C14A(H14A,H14B,
 H14C), C11B(H11D,H11E,H11F), C14B(H14D,H14E,H14F), C10B(H10D,H10E,H10F),
 C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F), C41A(H41A,H41B,H41C), C42B(H42D,
 H42E,H42F), C39B(H39D,H39E,H39F), C43B(H43D,H43E,H43F), C41B(H41D,H41E,H41F),
 C40B(H40D,H40E,H40F)
;
_shelx_res_checksum              8123
_shelx_hkl_checksum              19443
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;