Amine-catalyzed substitution in CpFe(CO)<sub>2</sub>I by phosphine and bisphosphine ligands.
Kosińska, Aneta; Jamroz, Daria; Rybarczyk-Pirek, Agnieszka J; Wojtulewski, Sławomir; Palusiak, Marcin; Zakrzewski, Janusz; Rudolf, Bogna; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9732–9740; doi:10.1039/d4dt00416g

data_7716133
_publ_section_title
;
 Amine-catalyzed substitution in CpFe(CO)<sub>2</sub>I by phosphine and
 bisphosphine ligands.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9732
_journal_page_last               9740
_journal_paper_doi               10.1039/d4dt00416g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'I, C32 H29 Fe O P2'
_chemical_formula_sum            'C32 H29 Fe I O P2'
_chemical_formula_weight         674.24
_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             2023-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-14 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.778(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7064(2)
_cell_length_b                   14.0307(2)
_cell_length_c                   23.7668(5)
_cell_measurement_reflns_used    21567
_cell_measurement_temperature    100.1(9)
_cell_measurement_theta_max      76.3650
_cell_measurement_theta_min      3.7690
_cell_volume                     2836.98(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4052
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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     -1.00  38.00   1.00   10.48    --  -41.44  19.00-180.00   39
  2  \w      2.00  35.00   1.00   10.48    --  -41.44  19.00-150.00   33
  3  \w      5.00  39.00   1.00   10.48    --  -41.44  19.00 150.00   34
  4  \w     -3.00  40.00   1.00   10.48    --  -41.44  19.00 120.00   43
  5  \w     -4.00  33.00   1.00   10.48    --  -41.44  19.00  60.00   37
  6  \w     -5.00  38.00   1.00   10.48    --  -41.44  19.00 -90.00   43
  7  \w     29.00  67.00   1.00   10.48    --   41.44-125.00 150.00   38
  8  \w     27.00  60.00   1.00   10.48    --   41.44-125.00 -30.00   33
  9  \w     34.00  86.00   1.00   10.48    --   41.44-125.00-120.00   52
 10  \w      8.00  83.00   1.00   10.48    --   41.44 -99.00   0.00   75
 11  \w    145.00 171.00   1.00   41.91    --  113.00  77.00  90.00   26
 12  \w     84.00 109.00   1.00   41.91    --  113.00-111.00   0.00   25
 13  \w     40.00  71.00   1.00   41.91    --  113.00 -45.00  90.00   31
 14  \w    118.00 144.00   1.00   41.91    --  113.00  30.00 -90.00   26
 15  \w     41.00  71.00   1.00   41.91    --  113.00 -45.00  60.00   30
 16  \w    112.00 138.00   1.00   41.91    --  113.00  77.00  90.00   26
 17  \w    114.00 147.00   1.00   41.91    --  113.00 -79.00-117.27   33
 18  \w     53.00 109.00   1.00   41.91    --  113.00-111.00-120.00   56
 19  \w     39.00  71.00   1.00   41.91    --  113.00 -45.00-120.00   32
 20  \w    107.00 165.00   1.00   41.91    --  113.00  15.00  60.00   58
 21  \w     63.00 109.00   1.00   41.91    --  113.00-111.00  90.00   46
 22  \w     38.00  70.00   1.00   41.91    --  113.00 -45.00 120.00   32
 23  \w     77.00 109.00   1.00   41.91    --  113.00-111.00  30.00   32
 24  \w     36.00  61.00   1.00   41.91    --  113.00-111.00   0.00   25
 25  \w     56.00 100.00   1.00   41.91    --  113.00 -95.00-180.00   44
 26  \w    152.00 178.00   1.00   41.91    --  113.00  15.00 120.00   26
 27  \w    146.00 177.00   1.00   41.91    --  113.00  77.00 150.00   31
 28  \w     94.00 127.00   1.00   41.91    --  113.00  61.00 120.00   33
 29  \w     83.00 170.00   1.00   41.91    --  113.00  61.00  60.00   87
 30  \w     75.00 105.00   1.00   41.91    --  113.00-111.00 -30.00   30
 31  \w     54.00  81.00   1.00   41.91    --  113.00  15.00  60.00   27
 32  \w    122.00 147.00   1.00   41.91    --  113.00 -83.00  84.15   25
 33  \w     52.00  78.00   1.00   41.91    --  113.00  15.00-180.00   26
 34  \w     70.00 108.00   1.00   41.91    --  113.00-111.00 -90.00   38
 35  \w     35.00  65.00   1.00   41.91    --  113.00-111.00 -90.00   30
 36  \w    129.00 171.00   1.00   41.91    --  113.00  30.00-150.00   42
 37  \w     32.00  57.00   1.00   41.91    --  113.00 -95.00   0.00   25
 38  \w    119.00 172.00   1.00   41.91    --  113.00  15.00-180.00   53
 39  \w     66.00 108.00   1.00   41.91    --  113.00-111.00 150.00   42
 40  \w     70.00  96.00   1.00   41.91    --  113.00-111.00  60.00   26
 41  \w     51.00  76.00   1.00   41.91    --  113.00 -61.00 150.00   25
 42  \w     38.00  84.00   1.00   41.91    --  113.00 -95.00  30.00   46
 43  \w     57.00  85.00   1.00   41.91    --  113.00 -61.00-120.00   28
 44  \w     32.00  79.00   1.00   41.91    --  113.00 -95.00 -90.00   47
 45  \w    148.00 173.00   1.00   41.91    --  113.00 111.00 -90.00   25
 46  \w     35.00  63.00   1.00   41.91    --  113.00-111.00  30.00   28
 47  \w    110.00 135.00   1.00   41.91    --  113.00  77.00 -90.00   25
 48  \w     56.00  82.00   1.00   41.91    --  113.00 -61.00  30.00   26
 49  \w    124.00 172.00   1.00   41.91    --  113.00  45.00 -90.00   48
 50  \w     62.00 104.00   1.00   41.91    --  113.00-111.00 120.00   42
 51  \w     46.00  81.00   1.00   41.91    --  113.00 -61.00-180.00   35
 52  \w     90.00 131.00   1.00   41.91    --  113.00  15.00 120.00   41
 53  \w     97.00 123.00   1.00   41.91    --  113.00  30.00-150.00   26
 54  \w    109.00 135.00   1.00   41.91    --  113.00 178.00  60.00   26
 55  \w    107.00 164.00   1.00   41.91    --  113.00  45.00 150.00   57
 56  \w     93.00 119.00   1.00   41.91    --  113.00 -77.00-150.00   26
 57  \w     32.00  58.00   1.00   41.91    --  113.00 -83.00  84.15   26
 58  \w     40.00  83.00   1.00   41.91    --  113.00 -61.00 -60.00   43
 59  \w    126.00 151.00   1.00   41.91    --  113.00 111.00-180.00   25
 60  \w    146.00 172.00   1.00   41.91    --  113.00 111.00   0.00   26
 61  \w     64.00 109.00   1.00   41.91    --  113.00-111.00-180.00   45
 62  \w     74.00 109.00   1.00   41.91    --  113.00-111.00 -60.00   35
 63  \w     53.00  79.00   1.00   41.91    --  113.00 -79.00-117.27   26
 64  \w     36.00  61.00   1.00   41.91    --  113.00 -95.00-150.00   25
 65  \w     94.00 119.00   1.00   41.91    --  113.00 178.00 120.00   25
 66  \w    119.00 145.00   1.00   41.91    --  113.00  45.00-150.00   26
 67  \w     37.00  62.00   1.00   41.91    --  113.00 -77.00 -60.00   25
 68  \w     91.00 116.00   1.00   41.91    --  113.00 -77.00  60.00   25
 69  \w    123.00 148.00   1.00   41.91    --  113.00 -87.00  73.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0867639000
_diffrn_orient_matrix_UB_12      -0.0943311000
_diffrn_orient_matrix_UB_13      0.0052794000
_diffrn_orient_matrix_UB_21      0.1579500000
_diffrn_orient_matrix_UB_22      0.0537727000
_diffrn_orient_matrix_UB_23      0.0301190000
_diffrn_orient_matrix_UB_31      0.0183439000
_diffrn_orient_matrix_UB_32      -0.0165061000
_diffrn_orient_matrix_UB_33      0.0672991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40468
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.482
_diffrn_reflns_theta_min         3.798
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.052
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+1.2647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5505
_reflns_number_total             5952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00416g2.cif
_cod_data_source_block           ak-684f2
_cod_depositor_comments
'Adding full bibliography for 7716132--7716134.cif.'
_cod_database_code               7716133
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C128  H116  Fe4  I4  O4  P8  '
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.315
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C14(H14), C3(H3), C2(H2), C13(H13), C5(H5), C26(H26),
 C10(H10), C28(H28), C32(H32), C19(H19), C20(H20), C12(H12), C22(H22), C11(H11),
  C18(H18), C24(H24), C29(H29), C25(H25), C31(H31), C17(H17), C30(H30),
 C23(H23), C16(H16)
;
_shelx_res_checksum              99690
_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 1.376
_oxdiff_exptl_absorpt_empirical_full_min 0.822