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_7133959
_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
'C29 H54 Fe N6 P2, F6 P, 2(C H2 Cl2), C24 H20 B'
_chemical_formula_sum            'C55 H78 B Cl4 F6 Fe N6 P3'
_chemical_formula_weight         1238.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-13
_audit_creation_method
;FinalCif V139 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-10-27 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                76.017(3)
_cell_angle_beta                 74.960(3)
_cell_angle_gamma                70.874(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7534(4)
_cell_length_b                   13.1143(5)
_cell_length_c                   20.0807(6)
_cell_measurement_reflns_used    29073
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.1200
_cell_measurement_theta_min      2.3120
_cell_volume                     3018.97(19)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9743
_diffrn_measured_fraction_theta_max 0.9590
_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    1.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    1.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    1.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    1.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    1.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    1.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    1.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    1.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    1.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    1.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    1.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    1.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    1.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    1.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    1.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    1.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    1.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    1.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    1.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    1.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    1.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    1.00    --  -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      -0.1273088000
_diffrn_orient_matrix_UB_12      0.0088267000
_diffrn_orient_matrix_UB_13      0.0175586000
_diffrn_orient_matrix_UB_21      0.0140929000
_diffrn_orient_matrix_UB_22      -0.0752377000
_diffrn_orient_matrix_UB_23      0.0709563000
_diffrn_orient_matrix_UB_31      -0.0244587000
_diffrn_orient_matrix_UB_32      0.1009455000
_diffrn_orient_matrix_UB_33      0.0340456000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.9719
_diffrn_reflns_Laue_measured_fraction_max 0.9583
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46024
_diffrn_reflns_point_group_measured_fraction_full 0.9719
_diffrn_reflns_point_group_measured_fraction_max 0.9583
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         69.4127
_diffrn_reflns_theta_min         2.3126
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67743
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       cube
_exptl_crystal_F_000             1146.455
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.135
_refine_diff_density_max         1.2861
_refine_diff_density_min         -1.2763
_refine_diff_density_rms         0.1320
_refine_ls_d_res_high            0.8235
_refine_ls_d_res_low             19.1050
_refine_ls_goodness_of_fit_ref   1.0280
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    125
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0280
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+1.6927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10628
_reflns_number_total             10857
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc05463f2.cif
_cod_data_source_block           CA1321
_cod_depositor_comments
'Adding full bibliography for 7133957--7133959.cif.'
_cod_original_cell_volume        3018.97(17)
_cod_database_code               7133959
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_completeness 97.43
_cell_oxdiff_measurement_reflns_used 29073
_cell_oxdiff_volume              3018.97(17)
_cell_oxdiff_angle_gamma         70.874(3)
_cell_oxdiff_angle_beta          74.960(3)
_cell_oxdiff_angle_alpha         76.017(3)
_cell_oxdiff_length_c            20.0807(6)
_cell_oxdiff_length_b            13.1143(5)
_cell_oxdiff_length_a            12.7534(4)
_chemical_oxdiff_formula         C77H94B2FeN6P2
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C00N(H00a,H00b), C00O(H00c,H00d), C00T(H00e,H00f), C00Z(H00g,H00h), C016(H01a,
 H01b), C01D(H01f,H01g), C01E(H01h,H01i), C01H(H01j,H01k), C01I(H01l,H01m),
 C01J(H01n,H01o), C01N(H01q,H01r), C01T(H01w,H01x), C01W(H01z,Hb), C021(H02g,
 H02h), C024(H02i,H02j)
2.b Aromatic/amide H refined with riding coordinates:
 C017(H017), C01Q(H10), C01G(H6), C01A(H3), C00L(H00L), C01F(H5), C01P(H9),
 C01K(H7), C01L(H8), C01C(H4), C015(H015), C00R(H00R), C013(H013), C01S(H11),
 C010(H010), C018(H018), C019(H019), C01V(H12), C014(H014), C00W(H00W),
 C00X(H00X), C011(H011), C01M(H01p), C01R(H01v)
2.c Idealised Me refined as rotating group:
 C01B(H01c,H01d,H01e), C01O(H01s,H01t,H01u), C01U(H01y,H,Ha), C01X(H01,Hc,Hd),
 C01Y(H1,He,Hf), C01Z(H2,Hg,Hh), C020(H02a,H02b,H02c), C022(H02d,H02e,H02f)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.207
_oxdiff_exptl_absorpt_empirical_full_min 0.692