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_7135253
_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_formula_moiety         'C39 H67 Al Fe N2 O P2 Si, 0.5(C5 H12)'
_chemical_formula_sum            'C41.5 H73 Al Fe N2 O P2 Si'
_chemical_formula_weight         788.87
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2p9zqq
_audit_creation_date             2024-10-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-22 deposited with the CCDC.	2025-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6664(2)
_cell_length_b                   11.47260(10)
_cell_length_c                   22.7577(2)
_cell_measurement_reflns_used    22471
_cell_measurement_temperature    173(3)
_cell_measurement_theta_max      73.0510
_cell_measurement_theta_min      3.9000
_cell_volume                     4587.57(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      173(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_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      9.00  63.00   1.00   14.34    --   41.86  77.00   0.00   54
  2  \w     17.00 114.00   1.00   14.34    --   41.86  38.00   0.00   97
  3  \w     59.00 108.00   1.00   14.34    --   41.86  57.00  90.00   49
  4  \w      9.00 115.00   1.00   14.34    --   41.86  77.00-180.00  106
  5  \w     14.00  52.00   1.00   14.34    --   41.86  57.00  90.00   38
  6  \w     88.00 114.00   1.00   14.34    --   41.86  77.00   0.00   26
  7  \w    -30.00  69.00   1.00   14.34    --   41.86 -57.00 -60.00   99
  8  \w      9.00  70.00   1.00   14.34    --   41.86  77.00 120.00   61
  9  \w      4.00  95.00   1.00   14.34    --   41.86-125.00 -90.00   91
 10  \w    -29.00  70.00   1.00   14.34    --   41.86 -57.00  60.00   99
 11  \w      9.00  77.00   1.00   14.34    --   41.86  77.00 -90.00   68
 12  \w    143.00 169.00   1.00   50.66    --  105.13  61.00-180.00   26
 13  \w     25.00  56.00   1.00   50.66    --  105.13 -95.00 150.00   31
 14  \w     73.00  99.00   1.00   50.66    --  105.13  77.00 -90.00   26
 15  \w     76.00 138.00   1.00   50.66    --  105.13  61.00-180.00   62
 16  \w    130.00 156.00   1.00   50.66    --  105.13  61.00   0.00   26
 17  \w    110.00 178.00   1.00   50.66    --  105.13  77.00  60.00   68
 18  \w     73.00 177.00   1.00   50.66    --  105.13  77.00-120.00  104
 19  \w     76.00 102.00   1.00   50.66    --  105.13  61.00 150.00   26
 20  \w     73.00  99.00   1.00   50.66    --  105.13  77.00  60.00   26
 21  \w     76.00 102.00   1.00   50.66    --  105.13  61.00  60.00   26
 22  \w     76.00 111.00   1.00   50.66    --  105.13  61.00   0.00   35
 23  \w     29.00 138.00   1.00   50.66    --  105.13 -77.00  60.00  109
 24  \w     73.00  99.00   1.00   50.66    --  105.13  77.00-180.00   26
 25  \w     76.00 102.00   1.00   50.66    --  105.13  61.00 -90.00   26
 26  \w     76.00 172.00   1.00   50.66    --  105.13  61.00 -60.00   96
 27  \w     73.00  99.00   1.00   50.66    --  105.13  73.00 -47.00   26
 28  \w     73.00  99.00   1.00   50.66    --  105.13  77.00   0.00   26
 29  \w     73.00 176.00   1.00   50.66    --  105.13  77.00  30.00  103
 30  \w     73.00  99.00   1.00   50.66    --  105.13  77.00 150.00   26
 31  \w     26.00 109.00   1.00   50.66    --  105.13 -95.00-120.00   83
 32  \w    109.00 178.00   1.00   50.66    --  105.13  77.00 -30.00   69
 33  \w     77.00 102.00   1.00   50.66    --  105.13  61.00-120.00   25
 34  \w     73.00  99.00   1.00   50.66    --  105.13  77.00  90.00   26
 35  \w     76.00 151.00   1.00   50.66    --  105.13  61.00 120.00   75
 36  \w     76.00 171.00   1.00   50.66    --  105.13  61.00-150.00   95
 37  \w     42.00  84.00   1.00   50.66    --  105.13 -77.00 -60.00   42
 38  \w    128.00 159.00   1.00   50.66    --  105.13  61.00  90.00   31
 39  \w     76.00 105.00   1.00   50.66    --  105.13  61.00  90.00   29
 40  \w     76.00 116.00   1.00   50.66    --  105.13  61.00  30.00   40
 41  \w     73.00 177.00   1.00   50.66    --  105.13  77.00 120.00  104
 42  \w     73.00  99.00   1.00   50.66    --  105.13  77.00-150.00   26
 43  \w    116.00 141.00   1.00   50.66    --  105.13  77.00 -90.00   25
 44  \w     81.00 108.00   1.00   50.66    --  105.13 -95.00 150.00   27
 45  \w     73.00  99.00   1.00   50.66    --  105.13  77.00 -30.00   26
 46  \w     32.00 121.00   1.00   50.66    --  105.13-125.00  60.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431796000
_diffrn_orient_matrix_UB_12      0.1068130000
_diffrn_orient_matrix_UB_13      0.0204828000
_diffrn_orient_matrix_UB_21      -0.0258911000
_diffrn_orient_matrix_UB_22      -0.0718048000
_diffrn_orient_matrix_UB_23      0.0514954000
_diffrn_orient_matrix_UB_31      0.0717822000
_diffrn_orient_matrix_UB_32      0.0383043000
_diffrn_orient_matrix_UB_33      0.0395039000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            70357
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.667
_diffrn_reflns_theta_min         3.906
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       'blocky needle'
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9215
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0492P)^2^+1.5279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8014
_reflns_number_total             9215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06456b3.cif
_cod_data_source_block           4a
_cod_original_formula_sum        'C41.50 H73 Al Fe N2 O P2 Si'
_cod_database_code               7135253
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C41.5 H73 Al1 Fe1 N2 O1 P2 Si1'
_chemical_oxdiff_usercomment     BS216-B
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.520
_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. Restrained distances
 C44-C43 = C43-C42 = C42-C41 = C41-C40
 1.52 with sigma of 0.02
 C44-C42 = C43-C41 = C42-C40
 2.54 with sigma of 0.04
 C44-C43 \\sim C43-C42 \\sim C42-C41 \\sim C41-C40
 with sigma of 0.02
 C44-C42 \\sim C42-C40 \\sim C43-C41
 with sigma of 0.04
 Si1-C1 \\sim Si1-C1A
 with sigma of 0.02
 C1-C2 \\sim C1A-C6A
 with sigma of 0.02
 C1-C6 \\sim C1A-C2A
 with sigma of 0.02
 C2-C3 \\sim C6A-C5A
 with sigma of 0.02
 C6-C5 \\sim C2A-C3A
 with sigma of 0.02
 C5-C4 \\sim C3A-C4A
 with sigma of 0.02
 C3-C4 \\sim C5A-C4A
 with sigma of 0.02
 Si1-C2 \\sim Si1-C6A
 with sigma of 0.04
 Si1-C6 \\sim Si1-C2A
 with sigma of 0.04
 C1-C5 \\sim C1A-C3A
 with sigma of 0.04
 C1-C3 \\sim C1A-C5A
 with sigma of 0.04
 C2-C6 \\sim C6A-C2A
 with sigma of 0.04
 C2-C4 \\sim C6A-C4A
 with sigma of 0.04
 C6-C4 \\sim C2A-C4A
 with sigma of 0.04
 C5-C3 \\sim C3A-C5A
 with sigma of 0.04
 C7-C8 \\sim C7-C8A
 with sigma of 0.02
 C7-C10 \\sim C7-C10A
 with sigma of 0.02
 C7-C9 \\sim C7-C9A
 with sigma of 0.02
3. Rigid bond restraints
 C40, C40, C41, C41, C42, C43, C43, C44, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C1A, C2, C2A, C3, C3A, C4, C4A, C5, C5A, C6, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C8A, C9, C9A, C10, C10A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C40 \\sim C40 \\sim C41 \\sim C41 \\sim C42 \\sim C43 \\sim C43 \\sim C44 \\sim
C44: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C3A \\sim C4 \\sim C4A \\sim C5
\\sim C5A \\sim C6 \\sim C6A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C8 \\sim C8A \\sim C9 \\sim C9A \\sim C10 \\sim C10A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C40, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(C2A)=Sof(H7)=Sof(C3A)=Sof(H8)=Sof(C4A)=Sof(H10)=Sof(C5A)=Sof(H9)=
 Sof(C6A)=Sof(H0)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H013)=Sof(C3)=Sof(H019)=Sof(C4)=Sof(H01P)=Sof(C5)=
 Sof(H018)=Sof(C6)=Sof(H017)=FVAR(1)
 Sof(C8A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C9A)=Sof(H01W)=Sof(H01X)=Sof(H01Y)=
 Sof(C10A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(2)
 Sof(C8)=Sof(H01M)=Sof(H01N)=Sof(H01O)=Sof(C9)=Sof(H01T)=Sof(H01U)=Sof(H01V)=
 Sof(C10)=Sof(H01Q)=Sof(H01R)=Sof(H01S)=FVAR(2)
 Fixed Sof: C40(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C41(0.5) H5A(0.5) H5B(0.5)
 C42(0.5) H4A(0.5) H4B(0.5) C43(0.5) H3A(0.5) H3B(0.5) C44(0.5) H2A(0.5)
 H2B(0.5) H2C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C41(H5A,H5B), C42(H4A,H4B), C43(H3A,H3B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H013), C2A(H7), C3(H019), C3A(H8), C4(H01P), C4A(H10), C5(H018), C5A(H9),
 C6(H017), C6A(H0), C12(H00G), C18(H00J), C20(H00F), C27(H00N), C29(H00T)
7.c Idealised Me refined as rotating group:
 C8(H01M,H01N,H01O), C8A(H11A,H11B,H11C), C9(H01T,H01U,H01V), C9A(H01W,H01X,
 H01Y), C10(H01Q,H01R,H01S), C10A(H12A,H12B,H12C), C14(H,H00X,H00Y), C15(H00I,
 H00K,H00L), C22(H00U,H00V,H00W), C23(HB,HA,H00Z), C24(H00D,H00E,H00H),
 C31(H00Q,H00R,H00S), C32(HF,HE,H11), C33(HH,HG,H12), C34(H01G,H01H,H01I),
 C35(H01D,H01E,H01F), C36(H00M,H00O,H00P), C37(H01A,H01B,H01C), C38(H01J,H01K,
 H01L), C39(HD,HC,H00), C40(H6A,H6B,H6C), C44(H2A,H2B,H2C)
;
_shelx_res_checksum              23373
_shelx_hkl_checksum              46074
_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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.747