Iron-catalysed Alkene and Heteroarene H/D Exchange by Reversible Protonation of Iron-hydride Intermediates
Britton, Luke; Docherty, Jamie; Sklyaruk, Jan; Cooney, Jessica; Nichol, Gary Stephen; Dominey, Andrew; Thomas, Stephen P.; Chemical Science  (2022) –; doi:10.1039/D2SC03802A

data_1567463
_publ_section_title
;
 Iron-catalysed Alkene and Heteroarene H/D Exchange by Reversible
 Protonation of Iron-hydride Intermediates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03802A
_journal_year                    2022
_chemical_formula_moiety         'C17 H38 Fe O P4'
_chemical_formula_sum            'C17 H38 Fe O P4'
_chemical_formula_weight         438.20
_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   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-07-06
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.181(2)
_cell_angle_beta                 106.444(3)
_cell_angle_gamma                106.680(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9533(2)
_cell_length_b                   10.1488(3)
_cell_length_c                   13.3681(4)
_cell_measurement_reflns_used    11006
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      32.5210
_cell_measurement_theta_min      3.9410
_cell_volume                     1111.27(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-beta (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.920
_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    -52.00   8.00   1.00   15.00    --  -17.52  88.00  27.00   60
  2  \w    -30.00  17.00   1.00   15.00    --  -17.52 -88.00 -89.00   47
  3  \w    -30.00  54.00   1.00   15.00    --   18.93 -88.00 -89.00   84
  4  \w    -49.00  21.00   1.00   15.00    --  -17.52  77.00 -90.00   70
  5  \w    -49.00  21.00   1.00   15.00    --  -17.52  77.00 -30.00   70
  6  \w    -42.00  14.00   1.00   15.00    --  -17.52 -77.00 150.00   56
  7  \w     -4.00  92.00   1.00   15.00    --   18.93  38.00 150.00   96
  8  \w     -4.00  92.00   1.00   15.00    --   18.93  38.00  60.00   96
  9  \w     39.00 106.00   1.00   15.00    --   18.93 178.00-120.00   67
 10  \w    -54.00  37.00   1.00   15.00    --   18.93 -38.00 -30.00   91
 11  \w     -4.00  92.00   1.00   15.00    --   18.93  38.00 -60.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0266015000
_diffrn_orient_matrix_UB_12      0.0142523000
_diffrn_orient_matrix_UB_13      0.0428989000
_diffrn_orient_matrix_UB_21      -0.0269329000
_diffrn_orient_matrix_UB_22      0.0536134000
_diffrn_orient_matrix_UB_23      -0.0258720000
_diffrn_orient_matrix_UB_31      -0.0778821000
_diffrn_orient_matrix_UB_32      -0.0478637000
_diffrn_orient_matrix_UB_33      -0.0240186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.850
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
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            'pale yellow'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             468
_exptl_crystal_recrystallization_method
'The material was recrystallised from pentane by slow cooling'
_exptl_crystal_size_max          0.617
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0236P)^2^+0.4413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6581
_reflns_number_total             7639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03802a2.cif
_cod_data_source_block           se20003
_cod_database_code               1567463
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H76 Fe2 O2 P8 '
_chemical_oxdiff_usercomment     '@ 120 K JD12.020'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
;
_shelx_res_checksum              12957
_shelx_hkl_checksum              93158
_olex2_date_sample_data_collection 2020-07-01
_olex2_date_sample_submission    2020-07-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id JD12.020
_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 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.815