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_1569245
_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         'C28 H48 Fe2 P10'
_chemical_formula_sum            'C28 H48 Fe2 P10'
_chemical_formula_weight         806.06
_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             2020-02-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                63.684(5)
_cell_angle_beta                 89.773(4)
_cell_angle_gamma                81.732(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8375(4)
_cell_length_b                   14.5973(7)
_cell_length_c                   16.2499(8)
_cell_measurement_reflns_used    6442
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.2030
_cell_measurement_theta_min      5.0400
_cell_volume                     1855.28(18)
_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 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.969
_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    -82.00 -25.00   0.50    4.00    --  -40.22 125.00 -90.00  114
  2  \w    -90.00 -29.00   0.50    4.00    --  -40.22 127.00  93.00  122
  3  \w    -37.00  34.00   0.50    4.00    --   40.22 -38.00-180.00  142
  4  \w    -13.00  38.00   0.50    4.00    --   40.22 -38.00   0.00  102
  5  \w      4.00 131.00   0.50    4.00    --   40.22   0.00-180.00  254
  6  \w    111.00 167.00   0.50   16.00    --  104.78  45.00  30.00  112
  7  \w     27.00  78.00   0.50   16.00    --  104.78-111.00-150.00  102
  8  \w    124.00 177.00   0.50   16.00    --  104.78  45.00 -90.00  106
  9  \w     29.00  68.00   0.50   16.00    --  104.78 -91.00 161.72   78
 10  \w     41.00  69.00   0.50   16.00    --  104.78 -61.00 -90.00   56
 11  \w     73.00 139.00   0.50   16.00    --  104.78 -91.00 161.72  132
 12  \w     81.00 107.00   0.50   16.00    --  104.78  45.00  30.00   52
 13  \w     35.00  71.00   0.50   16.00    --  104.78 -61.00   0.00   72
 14  \w     20.00  79.00   0.50   16.00    --  104.78 -95.00 120.00  118
 15  \w    139.00 177.00   0.50   16.00    --  104.78  45.00 -60.00   76
 16  \w     78.00 120.00   0.50   16.00    --  104.78  45.00 -60.00   84
 17  \w     40.00  68.00   0.50   16.00    --  104.78 -83.00  73.54   56
 18  \w     88.00 115.00   0.50   16.00    --  104.78 -83.00  73.54   54
 19  \w     84.00 149.00   0.50   16.00    --  104.78  61.00  60.00  130
 20  \w     77.00 112.00   0.50   16.00    --  104.78  45.00 -90.00   70
 21  \w     40.00 127.00   0.50   16.00    --  104.78 -91.00  -2.71  174
 22  \w     19.00  80.00   0.50   16.00    --  104.78 -90.00-134.49  122
 23  \w     93.00 144.00   0.50   16.00    --  104.78 -90.00-134.49  102
 24  \w     71.00 164.00   0.50   16.00    --  104.78  30.00   0.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12816
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.725
_diffrn_reflns_theta_min         5.069
_exptl_absorpt_coefficient_mu    10.494
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.151
_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    1.443
_exptl_crystal_description       needle
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         7024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0536P)^2^+0.0620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6125
_reflns_number_total             7024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01488f2.cif
_cod_data_source_block           abs_det_ana
_cod_depositor_comments
'Adding full bibliography for 1569243--1569247.cif.'
_cod_original_cell_volume        1855.28(17)
_cod_database_code               1569245
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.452
_shelx_estimated_absorpt_t_min   0.077
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C15(H15A,H15B)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C9(H9A,H9B,H9C), C18(H18A,H18B,
 H18C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C),
 C24(H24A,H24B,H24C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C14(H14A,H14B,
 H14C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              9939
_shelx_hkl_checksum              57407
_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
;