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_7716134
_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         '2(I), C48 H38 Fe3 O4 P2'
_chemical_formula_sum            'C48 H38 Fe3 I2 O4 P2'
_chemical_formula_weight         1162.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4111(2)
_cell_length_b                   21.4111(2)
_cell_length_c                   19.0714(3)
_cell_measurement_reflns_used    21178
_cell_measurement_temperature    100.1(9)
_cell_measurement_theta_max      75.6550
_cell_measurement_theta_min      3.0900
_cell_volume                     8743.00(18)
_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 0.994
_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     -5.00  38.00   1.00   24.20    --  -41.84  19.00  60.00   43
  2  \w      7.00  33.00   1.00   24.20    --   41.84  84.00  76.40   26
  3  \w      9.00  42.00   1.00   24.20    --   41.84  76.00 126.69   33
  4  \w      9.00  42.00   1.00   24.20    --   41.84  80.00 -96.20   33
  5  \w     14.00 115.00   1.00   24.20    --   41.84  57.00-180.00  101
  6  \w      6.00  83.00   1.00   24.20    --   41.84 -99.00 -30.00   77
  7  \w     30.00 106.00   1.00   96.81    --  112.00 -95.00 -30.00   76
  8  \w     86.00 178.00   1.00   96.81    --  112.00  45.00-180.00   92
  9  \w     39.00  72.00   1.00   96.81    --  112.00 -45.00  90.00   33
 10  \w     36.00 109.00   1.00   96.81    --  112.00-111.00 -90.00   73
 11  \w     39.00  72.00   1.00   96.81    --  112.00 -45.00  30.00   33
 12  \w     30.00 106.00   1.00   96.81    --  112.00 -95.00  60.00   76
 13  \w    103.00 178.00   1.00   96.81    --  112.00  77.00  90.00   75
 14  \w    104.00 178.00   1.00   96.81    --  112.00 111.00  90.00   74
 15  \w     36.00 109.00   1.00   96.81    --  112.00-111.00  30.00   73
 16  \w     36.00 109.00   1.00   96.81    --  112.00-111.00 -30.00   73
 17  \w     39.00  72.00   1.00   96.81    --  112.00 -45.00  60.00   33
 18  \w     86.00 178.00   1.00   96.81    --  112.00  45.00-150.00   92
 19  \w     40.00  93.00   1.00   96.81    --  112.00 -61.00-150.00   53
 20  \w    104.00 178.00   1.00   96.81    --  112.00 111.00 150.00   74
 21  \w     40.00  93.00   1.00   96.81    --  112.00 -61.00-120.00   53
 22  \w     60.00  86.00   1.00   96.81    --  112.00 -61.00  30.00   26
 23  \w     50.00  76.00   1.00   96.81    --  112.00-111.00 150.00   26
 24  \w     64.00 121.00   1.00   96.81    --  112.00 178.00 -60.00   57
;
_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      -0.0051657000
_diffrn_orient_matrix_UB_12      0.0492381000
_diffrn_orient_matrix_UB_13      -0.0586345000
_diffrn_orient_matrix_UB_21      0.0091736000
_diffrn_orient_matrix_UB_22      -0.0514771000
_diffrn_orient_matrix_UB_23      -0.0554872000
_diffrn_orient_matrix_UB_31      -0.0711634000
_diffrn_orient_matrix_UB_32      -0.0102310000
_diffrn_orient_matrix_UB_33      -0.0028498000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37237
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.610
_diffrn_reflns_theta_min         4.130
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.013
_exptl_absorpt_correction_T_max  0.317
_exptl_absorpt_correction_T_min  0.088
_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    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.625
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 1908 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+24.7645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                4427
_reflns_number_total             4570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00416g2.cif
_cod_data_source_block           ak-705-f5
_cod_depositor_comments
'Adding full bibliography for 7716132--7716134.cif.'
_cod_original_cell_volume        8743.0(2)
_cod_database_code               7716134
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H38 Fe2 I2 O4 P2'
_shelx_estimated_absorpt_t_max   0.460
_shelx_estimated_absorpt_t_min   0.192
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: I2(0.33) I2A(0.17)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C12(H12), C4(H4), C24(H24), C3(H3), C23(H23), C9(H9),
 C11(H11), C16(H16), C5(H5), C1(H1), C20(H20), C15(H15), C21(H21), C22(H22),
 C18(H18), C2(H2), C17(H17)
;
_shelx_res_checksum              96711
_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 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.612