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_1569247
_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         'C31 H54 Fe2 P10, 0.75[C6H14], 0.5[CH2Cl2]'
_chemical_formula_sum            'C40.5 H76 Cl Fe2 P10'
_chemical_formula_weight         1019.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-27
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5101(3)
_cell_length_b                   12.8109(2)
_cell_length_c                   24.2981(3)
_cell_measurement_reflns_used    18371
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      33.4500
_cell_measurement_theta_min      3.7920
_cell_volume                     4731.92(13)
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.927
_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   -107.00  10.00   0.25   20.00    --  -24.98 -77.00-180.00  468
  2  \w     57.00 118.00   0.25   20.00    --   26.85 178.00-150.00  244
  3  \w     -4.00 103.00   0.25   20.00    --   26.85  57.00  30.00  428
  4  \w     -5.00  29.00   0.25   20.00    --  -24.98  19.00 120.00  136
  5  \w    -22.00  53.00   0.25   20.00    --  -24.98  38.00 -60.00  300
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0344690000
_diffrn_orient_matrix_UB_12      -0.0339194000
_diffrn_orient_matrix_UB_13      -0.0125212000
_diffrn_orient_matrix_UB_21      -0.0210508000
_diffrn_orient_matrix_UB_22      0.0420367000
_diffrn_orient_matrix_UB_23      -0.0163951000
_diffrn_orient_matrix_UB_31      0.0232866000
_diffrn_orient_matrix_UB_32      -0.0122097000
_diffrn_orient_matrix_UB_33      -0.0215098000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            55081
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.549
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.48a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.575
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.288
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         18675
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0551P)^2^+2.8549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13489
_reflns_number_total             18675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01488f2.cif
_cod_data_source_block           abs_det_ana_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1569243--1569247.cif.'
_cod_original_formula_sum        'C40.50 H76 Cl Fe2 P10'
_cod_database_code               1569247
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         (C20H30Fe2P10C8H18C3H6C6h14)4
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.587
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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
C26B \\sim C27 \\sim C25B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
C21A \\sim C22A \\sim C23A \\sim C24A \\sim C21B \\sim C24B \\sim C22B \\sim
C23B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.7A
P4B \\sim P3B \\sim P3A \\sim P2A: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2.5A
3. Others
 Sof(Fe2B)=1-FVAR(1)
 Sof(Fe2A)=FVAR(1)
 Fixed Sof: Fe1A(0.92) P1A(0.92) P2A(0.92) P3A(0.92) P5A(0.92) P4A(0.92)
 H27A(0.92) H27B(0.92) H27C(0.08) H27D(0.08) C25A(0.92) H25A(0.92) H25B(0.92)
 C26A(0.92) H26A(0.92) H26B(0.92) C21A(0.92) C22A(0.92) H22A(0.92) H22B(0.92)
 H22C(0.92) C23A(0.92) H23A(0.92) H23B(0.92) H23C(0.92) C24A(0.92) H24A(0.92)
 H24B(0.92) H24C(0.92) P1B(0.08) P2B(0.08) C21B(0.08) C24B(0.08) H24D(0.08)
 H24E(0.08) H24F(0.08) C22B(0.08) H22D(0.08) H22E(0.08) H22F(0.08) C23B(0.08)
 H23D(0.08) H23E(0.08) H23F(0.08) P5B(0.08) P4B(0.08) P3B(0.08) Fe1B(0.08)
 C26B(0.08) H26C(0.08) H26D(0.08) C25B(0.08) H25C(0.08) H25D(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C25A(H25A,H25B), C26A(H26A,H26B), C26B(H26C,
 H26D), C25B(H25C,H25D)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C6(H6A,H6B,H6C),
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
  C30(H30A,H30B,H30C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C24A(H24A,
 H24B,H24C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C18(H18A,H18B,H18C),
 C31(H31A,H31B,H31C), C24B(H24D,H24E,H24F), C22B(H22D,H22E,H22F), C23B(H23D,
 H23E,H23F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91997
_shelx_hkl_checksum              38796
_shelx_fab_checksum              44194
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.709