Synthesis of heteroleptic bis-phosphine bis-NHC iron (0) complexes: a strategy to enhance small molecule activation.
Andre, Christian M.; Szymczak, Nathaniel K.; Chemical communications (Cambridge, England) 60 (2024) 14037–14040; doi:10.1039/d4cc05463f

data_7133958
_publ_section_title
;
 Synthesis of heteroleptic bis-phosphine bis-NHC iron (0) complexes: a
 strategy to enhance small molecule activation.
;
_journal_issue                   95
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14037
_journal_page_last               14040
_journal_paper_doi               10.1039/d4cc05463f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C26 H48 Fe N4 O P2'
_chemical_formula_sum            'C26 H48 Fe N4 O P2'
_chemical_formula_weight         550.47
_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   geom
_audit_creation_date             2024-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-14 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                67.588(2)
_cell_angle_beta                 86.730(2)
_cell_angle_gamma                87.945(2)
_cell_formula_units_Z            4
_cell_length_a                   8.7819(3)
_cell_length_b                   18.2197(4)
_cell_length_c                   19.7713(4)
_cell_measurement_reflns_used    24984
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.2750
_cell_measurement_theta_min      2.3940
_cell_volume                     2919.43(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'DTREK_VERSION=d*TREK version 9.9.9.4 W9RSSI -- Aug 22 2012'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.960
_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   -110.00  70.00   1.00    1.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00    3.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    3.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    3.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    3.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    3.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    3.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    3.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    3.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    3.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    3.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    3.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    3.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    3.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    3.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    3.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    3.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    3.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    3.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    3.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    3.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    3.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    3.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1583268000
_diffrn_orient_matrix_UB_12      0.0408279000
_diffrn_orient_matrix_UB_13      -0.0129433000
_diffrn_orient_matrix_UB_21      0.0315884000
_diffrn_orient_matrix_UB_22      0.0273566000
_diffrn_orient_matrix_UB_23      -0.0833641000
_diffrn_orient_matrix_UB_31      -0.0693996000
_diffrn_orient_matrix_UB_32      -0.0771503000
_diffrn_orient_matrix_UB_33      0.0016146000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19454
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.580
_diffrn_reflns_theta_min         2.420
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         19454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0536
_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^)+(0.1152P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14723
_reflns_number_total             19454
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9690\% 
around [1.00 -0.00 -0.00] (reciprocal) or [1.00 -0.01 -0.02] (direct)
;
_cod_data_source_file            d4cc05463f2.cif
_cod_data_source_block           ca1368_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7133957--7133959.cif.'
_cod_database_code               7133958
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H51F12FeN5OP4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8490(5)
 0.1510(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C00K(H00N,H00O), C00M(H00A,H00B), C00N(H00P,H00Q), C00O(H00C,H00D), C00P(H00E,
 H00F), C00U(H00W,H00X), C00W(H00Z,H), C00X(H00G,H00H), C00Y(H00I,H00J),
 C00Z(H00K,H00L), C010(H01A,H01B), C011(H2,HA), C012(H01C,H01D), C014(H3,HB),
 C015(H4,HC), C017(H5,HD), C019(H01E,H01F), C01A(H01G,H01H), C01B(H6,HE),
 C01C(H7,HF), C01D(H8,HG), C01H(H9,HH), C01K(H11,HK), C01L(H01S,H01T),
 C01Q(H01X,H01Y), C01R(H01Z,HN)
3.b Aromatic/amide H refined with riding coordinates:
 C00I(H00M), C00Q(H00S), C00R(H00R), C00V(H00Y), C013(H013), C016(H016),
 C018(H018), C01E(H01I)
3.c Idealised Me refined as rotating group:
 C00T(H00T,H00U,H00V), C01F(H01J,H01K,H01L), C01G(H01M,H01N,H01O), C01I(H01P,
 H01Q,H01R), C01J(H10,HI,HJ), C01M(H01U,H01V,H01W), C01O(H12,HL,HM), C01S(H01,
 HO,HP), C01T(H1,HQ,HR), C01U(H13,HS,HT), C01V(H14,HU,HV), C01W(H15,HW,HX)
;
_shelx_res_checksum              11542
_shelx_hkl_checksum              99072
_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 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.622
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2