A Heterometallic σ-Silane Adduct from Cooperative Reactivity of an Iron–Aluminium Complex
Crimmin, Mark Richard; Stadler, Benedek; Chemical Communications  (2025) –; doi:10.1039/D5CC06456B

data_7135251
_publ_section_title
;
 A Heterometallic \s-Silane Adduct from Cooperative Reactivity of an
 Iron--Aluminium Complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC06456B
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37 H59 Al Fe N4 O P2'
_chemical_formula_sum            'C37 H59 Al Fe N4 O P2'
_chemical_formula_weight         720.65
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2p9zss
_audit_creation_date             2025-06-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-08-22 deposited with the CCDC.	2025-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.455(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.7184(3)
_cell_length_b                   17.9691(3)
_cell_length_c                   17.6796(4)
_cell_measurement_reflns_used    28139
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      27.9750
_cell_measurement_theta_min      2.6230
_cell_volume                     4040.34(15)
_computing_cell_refinement       'CrysAlisPro 1.171.44.85 (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 38.46 (release 23-01-2017))'
_computing_data_reduction        'CrysAlisPro 1.171.44.85 (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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.914
_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    -18.00  26.00   1.00   60.00    --  -13.18 -99.00 -90.00   44
  2  \w     -1.00  70.00   1.00   60.00    --   14.43  77.00  30.00   71
  3  \w    -81.00  -5.00   1.00   60.00    --  -13.18 -77.00-150.00   76
  4  \w    -32.00  56.00   1.00   60.00    --  -13.18  37.00 -90.00   88
  5  \w    -64.00   7.00   1.00   60.00    --  -13.18 120.00  10.56   71
  6  \w    -67.00 -31.00   1.00   60.00    --  -13.18 125.00-135.96   36
  7  \w    -40.00  51.00   1.00   60.00    --  -13.18  77.00 150.00   91
  8  \w     -5.00  76.00   1.00   60.00    --   14.43  37.00 -30.00   81
  9  \w      0.00  68.00   1.00   60.00    --   14.43  57.00 150.00   68
 10  \w    -52.00  31.00   1.00   60.00    --   14.43 -57.00 -30.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315471000
_diffrn_orient_matrix_UB_12      -0.0206102000
_diffrn_orient_matrix_UB_13      0.0254656000
_diffrn_orient_matrix_UB_21      0.0386938000
_diffrn_orient_matrix_UB_22      0.0046465000
_diffrn_orient_matrix_UB_23      0.0287083000
_diffrn_orient_matrix_UB_31      -0.0248227000
_diffrn_orient_matrix_UB_32      0.0333467000
_diffrn_orient_matrix_UB_33      0.0117362000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         2.543
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.85 (Rigaku Oxford Diffraction, 2024)
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            'pale yellow'
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.425
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 6321 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.251(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         17439
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0523P)^2^+0.5088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                15440
_reflns_number_total             17439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06456b3.cif
_cod_data_source_block           5b
_cod_original_cell_volume        4040.33(15)
_cod_database_code               7135251
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C47 H59 Al1 Fe1 N4 O1 P2'
_chemical_oxdiff_usercomment     BS232-C
_cell_oxdiff_angle_alpha         89.9961(15)
_cell_oxdiff_angle_beta          90.4133(17)
_cell_oxdiff_angle_gamma         90.0580(15)
_cell_oxdiff_length_a            12.7221(3)
_cell_oxdiff_length_b            17.9678(3)
_cell_oxdiff_length_c            17.6756(4)
_cell_oxdiff_measurement_reflns_used 28139
_cell_oxdiff_volume              4040.33(14)
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.798
_diffrn_oxdiff_digest_od_ed
;

;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7180(18)
 0.2820(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C25A(H00T), C18(H00L), C27A(H013), C18A(H20), C16(H00Q), C25(H21), C27(H22),
 C16A(H4), C4(H16), C3A(H6A), C3(H18), C10A(H026), C5(H023), C5A(H23), C10(H1B),
  C4A(H16A)
3.b Idealised Me refined as rotating group:
 C13(H00G,H00H,H00I), C12A(HHA,HIA,H4A), C31A(H15A,HFA,HGA), C20(H01W,H01X,
 H01Y), C29A(HLA,HMA,H7A), C22(H01Z,H,HA), C30A(H5A,HJA,HKA), C21(H01,HB,HC),
 C33(H14,HD,HE), C20A(H5,H6,H7), C31(H15,HF,HG), C13A(H8,H9,H10), C12(H11,HH,
 HI), C22A(H12,H13,HAA), C30(H17,HJ,HK), C21A(H01A,HBA,HCA), C36A(H10A,HVA,HWA),
  C29(H19,HL,HM), C34(H02W,H02X,H02Y), C32(H02Z,HN,HO), C8(H02,HP,HQ), C35A(HYA,
 H11A,HXA), C37A(H9A,HTA,HUA), C7A(H8A,HRA,HSA), C8A(H02A,HPA,HQA), C7(H1C,HR,
 HS), C32A(H1D,HNA,HOA), C37(H1E,HT,HU), C34A(H1F,H1G,H1H), C36(H1I,HV,HW),
 C33A(H14A,HDA,HEA), C35(H1J,HX,HY)
;
_shelx_res_checksum              38237
_shelx_hkl_checksum              82332
_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 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.935