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_7135254
_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         'C46 H70 Al Fe N3 O P2 Si, 1[C5H12]'
_chemical_formula_sum            'C51 H82 Al Fe N3 O P2 Si'
_chemical_formula_weight         926.05
_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.cc2p9znn
_audit_creation_date             2024-11-18
_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                 94.4545(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.59351(6)
_cell_length_b                   10.02490(6)
_cell_length_c                   35.96271(15)
_cell_measurement_reflns_used    35298
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      73.4420
_cell_measurement_theta_min      4.5660
_cell_volume                     5245.40(4)
_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      173.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -80.00  33.00   1.00   11.90    --  -41.98  19.00 -30.00  113
  2  \w      9.00 118.00   1.00   11.90    --   41.98  77.00 150.00  109
  3  \w     66.00 105.00   1.00   11.90    --   41.98 147.00-175.00   39
  4  \w     10.00  69.00   1.00   11.90    --   41.98  77.00  60.00   59
  5  \w     20.00  95.00   1.00   11.90    --   41.98-125.00  30.00   75
  6  \w      3.00  83.00   1.00   11.90    --   41.98-125.00-150.00   80
  7  \w      9.00 109.00   1.00   11.90    --   41.98  77.00 -30.00  100
  8  \w      9.00 118.00   1.00   11.90    --   41.98  77.00-120.00  109
  9  \w     73.00 177.00   1.00   61.41    --  105.13  77.00   0.00  104
 10  \w     73.00  98.00   1.00   61.41    --  105.13  77.00-180.00   25
 11  \w     35.00 121.00   1.00   61.41    --  105.13-125.00-180.00   86
 12  \w     76.00 174.00   1.00   61.41    --  105.13  61.00-150.00   98
 13  \w     39.00 109.00   1.00   61.41    --  105.13 -95.00 -30.00   70
 14  \w     73.00  98.00   1.00   61.41    --  105.13  77.00  30.00   25
 15  \w     76.00 168.00   1.00   61.41    --  105.13  61.00 -30.00   92
 16  \w     73.00  98.00   1.00   61.41    --  105.13  77.00 150.00   25
 17  \w     73.00  99.00   1.00   61.41    --  105.13  77.00  60.00   26
 18  \w     30.00 137.00   1.00   61.41    --  105.13 -77.00-180.00  107
 19  \w     73.00 100.00   1.00   61.41    --  105.13  77.00-150.00   27
 20  \w    120.00 152.00   1.00   61.41    --  105.13  77.00 150.00   32
 21  \w     76.00 170.00   1.00   61.41    --  105.13  61.00 -90.00   94
 22  \w     76.00 101.00   1.00   61.41    --  105.13  61.00   0.00   25
 23  \w     73.00  98.00   1.00   61.41    --  105.13  77.00-120.00   25
 24  \w     73.00  99.00   1.00   61.41    --  105.13  77.00  90.00   26
 25  \w     76.00 171.00   1.00   61.41    --  105.13  61.00  60.00   95
 26  \w     76.00 161.00   1.00   61.41    --  105.13  61.00-120.00   85
 27  \w     76.00 173.00   1.00   61.41    --  105.13  61.00  90.00   97
 28  \w     73.00  98.00   1.00   61.41    --  105.13  77.00 -60.00   25
 29  \w    106.00 160.00   1.00   61.41    --  105.13  77.00 -60.00   54
 30  \w     76.00 169.00   1.00   61.41    --  105.13  61.00-180.00   93
 31  \w     76.00 102.00   1.00   61.41    --  105.13  61.00  30.00   26
 32  \w    117.00 168.00   1.00   61.41    --  105.13  77.00  30.00   51
 33  \w     76.00 102.00   1.00   61.41    --  105.13  61.00 120.00   26
 34  \w     73.00  99.00   1.00   61.41    --  105.13  77.00 -90.00   26
 35  \w     73.00  99.00   1.00   61.41    --  105.13  77.00 -30.00   26
 36  \w     76.00 102.00   1.00   61.41    --  105.13  61.00 150.00   26
 37  \w     73.00 178.00   1.00   61.41    --  105.13  77.00 120.00  105
 38  \w     76.00 102.00   1.00   61.41    --  105.13  61.00 -60.00   26
 39  \w     33.00 129.00   1.00   61.41    --  105.13 -61.00   0.00   96
;
_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      -0.0448720000
_diffrn_orient_matrix_UB_12      0.0070863000
_diffrn_orient_matrix_UB_13      -0.0401669000
_diffrn_orient_matrix_UB_21      -0.0956517000
_diffrn_orient_matrix_UB_22      -0.0150124000
_diffrn_orient_matrix_UB_23      0.0148826000
_diffrn_orient_matrix_UB_31      -0.0071751000
_diffrn_orient_matrix_UB_32      0.1527837000
_diffrn_orient_matrix_UB_33      0.0032871000
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            79867
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.638
_diffrn_reflns_theta_min         3.761
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.539
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.606
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       'blocky needle'
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         10511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.4883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9805
_reflns_number_total             10511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06456b3.cif
_cod_data_source_block           3b
_cod_database_code               7135254
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H82 Al1 Fe1 N3 O1 P2 Si1'
_chemical_oxdiff_usercomment     BS224-A
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C13(H13), C7(H7), C1(H1), C11(H11), C27(H27), C17(H17), C10(H10),
 C9(H9), C16(H16), C25(H25), C8(H8), C14(H14), C36(H36), C15(H15), C34(H34)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C42(H42A,H42B,H42C), C22(H22A,H22B,
 H22C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C),
 C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C41(H41A,H41B,
 H41C), C46(H46A,H46B,H46C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C30(H30A,
 H30B,H30C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              10699
_shelx_hkl_checksum              75616
_shelx_fab_checksum              2112
_platon_squeeze_special_details
;
A solvent mask was calculated and 172 electrons were 
found in a volume of 844\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C5H12] per formula unit 
which account for 168 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.886