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_1569244
_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         '2(C8.5 H15 Br0.5 Fe0.5 P2.5)'
_chemical_formula_sum            'C17 H30 Br Fe P5'
_chemical_formula_weight         525.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-19
_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                90
_cell_angle_beta                 105.764(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2089(5)
_cell_length_b                   11.4407(4)
_cell_length_c                   18.1308(8)
_cell_measurement_reflns_used    5064
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      31.5100
_cell_measurement_theta_min      3.8660
_cell_volume                     2237.60(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_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)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.896
_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    -92.00  -2.00   0.25   50.00    --  -19.91 -38.00-180.00  360
  2  \w    -83.00 -57.00   0.25   50.00    --  -19.91 133.00 143.00  104
  3  \w    -90.00  -3.00   0.25   50.00    --  -19.91 -38.00  90.00  348
;
_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      0.0539627000
_diffrn_orient_matrix_UB_12      0.0025364000
_diffrn_orient_matrix_UB_13      -0.0132671000
_diffrn_orient_matrix_UB_21      0.0375221000
_diffrn_orient_matrix_UB_22      -0.0001476000
_diffrn_orient_matrix_UB_23      0.0383969000
_diffrn_orient_matrix_UB_31      0.0020869000
_diffrn_orient_matrix_UB_32      -0.0619551000
_diffrn_orient_matrix_UB_33      -0.0006606000
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13109
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.281
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6052
_reflns_number_total             7434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01488f2.cif
_cod_data_source_block           resp5_tbu_dibr_mp_abs_ana
_cod_depositor_comments
'Adding full bibliography for 1569243--1569247.cif.'
_cod_database_code               1569244
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H30BrFeP5
_chemical_oxdiff_usercomment     'green needle'
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.516
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H10A(0.5) H10B(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) H18A(0.5) H18C(0.5) H12A(0.5) H12B(0.5) H11A(0.5) H11B(0.5)
 H22A(0.5) H22B(0.5) H24A(0.5) H24B(0.5) H23A(0.5) H23B(0.5) H9A(0.5) H9C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B), C22(H22A,H22B), C24(H24A,
 H24B), C23(H23A,H23B)
3.b Me refined with everything fixed:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C),
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              79862
_shelx_hkl_checksum              29053
_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 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.788