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_1569243
_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         'C14.75 H23.55 Fe N0.95 P5'
_chemical_formula_sum            'C14.75 H23.55 Fe N0.95 P5'
_chemical_formula_weight         424.89
_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
_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                90
_cell_angle_beta                 109.044(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2369(3)
_cell_length_b                   9.0210(2)
_cell_length_c                   16.3159(5)
_cell_measurement_reflns_used    10253
_cell_measurement_temperature    123
_cell_measurement_theta_max      32.0890
_cell_measurement_theta_min      3.7750
_cell_volume                     1980.78(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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      123.0
_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 0.918
_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    -97.00   9.00   0.50   20.00    --  -19.91 -38.00-120.00  212
  2  \w    -97.00   9.00   0.50   20.00    --  -19.91 -38.00 -30.00  212
  3  \w     16.00  78.00   0.50   20.00    --   21.47-122.00 -10.00  124
  4  \w    -97.00 -24.00   0.50   20.00    --  -19.91 -38.00  90.00  146
;
_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      0.0096864000
_diffrn_orient_matrix_UB_12      0.0109966000
_diffrn_orient_matrix_UB_13      -0.0395302000
_diffrn_orient_matrix_UB_21      -0.0516996000
_diffrn_orient_matrix_UB_22      -0.0027452000
_diffrn_orient_matrix_UB_23      -0.0229966000
_diffrn_orient_matrix_UB_31      -0.0031523000
_diffrn_orient_matrix_UB_32      0.0778401000
_diffrn_orient_matrix_UB_33      0.0047912000
_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  0.0189
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19036
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.255
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.160
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             879
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         6439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0450P)^2^+0.9734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5702
_reflns_number_total             6439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01488f2.cif
_cod_data_source_block           mp_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 1569243--1569247.cif.'
_cod_database_code               1569243
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H24FeNP5
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_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: P1A(0.95) N1(0.95) C13(0.95) H13A(0.95) H13B(0.95) C15(0.95)
 C12(0.95) H12A(0.95) H12B(0.95) C11(0.95) H11A(0.95) H11B(0.95) H11C(0.95)
 C14(0.95) H14A(0.95) H14B(0.95) P1B(0.05)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              66022
_shelx_hkl_checksum              25301
_olex2_diffrn_ambient_temperature_device 123
_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 1.098
_oxdiff_exptl_absorpt_empirical_full_min 0.902