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_7135250
_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         'C42 H71 Al Fe N4 P2 Si, 0.25(C5 H12)'
_chemical_formula_sum            'C43.25 H74 Al Fe N4 P2 Si'
_chemical_formula_weight         822.92
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2p9zpp
_audit_creation_date             2024-10-10
_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                85.197(3)
_cell_angle_beta                 81.930(4)
_cell_angle_gamma                61.139(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9256(5)
_cell_length_b                   12.2370(4)
_cell_length_c                   18.8626(8)
_cell_measurement_reflns_used    5500
_cell_measurement_temperature    173(3)
_cell_measurement_theta_max      72.0850
_cell_measurement_theta_min      4.0970
_cell_volume                     2386.51(19)
_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)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.966
_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     57.00  89.00   1.00    1.24    --   41.86-125.00 -30.00   32
  2  \w     18.00 109.00   1.00    1.24    --   41.86  57.00-180.00   91
  3  \w    -31.00  62.00   1.00    1.24    --   41.86 -38.00-120.00   93
  4  \w    -30.00  65.00   1.00    1.24    --   41.86 -57.00  30.00   95
  5  \w    129.00 174.00   1.00   27.79    --  105.13  30.00 -30.00   45
  6  \w     84.00 119.00   1.00   27.79    --  105.13-125.00 -60.00   35
  7  \w     79.00 177.00   1.00   27.79    --  105.13  30.00-120.00   98
  8  \w     33.00 130.00   1.00   27.79    --  105.13 -61.00 150.00   97
  9  \w     78.00 113.00   1.00   27.79    --  105.13  30.00 -30.00   35
 10  \w     29.00 133.00   1.00   27.79    --  105.13 -30.00 -90.00  104
 11  \w     30.00  91.00   1.00   27.79    --  105.13 -30.00  60.00   61
 12  \w     42.00  69.00   1.00   27.79    --  105.13-125.00 -60.00   27
 13  \w     39.00 116.00   1.00   27.79    --  105.13-125.00 120.00   77
 14  \w     41.00 107.00   1.00   27.79    --  105.13 -95.00 150.00   66
 15  \w     29.00 137.00   1.00   27.79    --  105.13 -77.00 -90.00  108
;
_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      -0.0951741000
_diffrn_orient_matrix_UB_12      0.0212640000
_diffrn_orient_matrix_UB_13      -0.0536504000
_diffrn_orient_matrix_UB_21      0.1135620000
_diffrn_orient_matrix_UB_22      -0.0610843000
_diffrn_orient_matrix_UB_23      -0.0590821000
_diffrn_orient_matrix_UB_31      0.0095684000
_diffrn_orient_matrix_UB_32      -0.1284019000
_diffrn_orient_matrix_UB_33      0.0209236000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16046
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.368
_diffrn_reflns_theta_min         4.126
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.820
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.583
_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    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             889
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9274
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0439P)^2^+0.0937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7246
_reflns_number_total             9274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06456b3.cif
_cod_data_source_block           3c
_cod_original_cell_volume        2386.51(18)
_cod_database_code               7135250
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43.25 H74 Al1 Fe1 N4 P2 Si1'
_chemical_oxdiff_usercomment     BS194-A
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C45 = C45-C44 = C44-C43 = C43-C42
 1.52 with sigma of 0.02
 C46-C44 = C45-C43 = C44-C42
 2.54 with sigma of 0.04
 C46-C45 \\sim C45-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.02
 C46-C44 \\sim C44-C42 \\sim C45-C43
 with sigma of 0.04
3. Rigid bond restraints
 C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C42(0.25) H42A(0.25) H42B(0.25) H42C(0.25) C43(0.25) H43A(0.25)
 H43B(0.25) C44(0.25) H44A(0.25) H44B(0.25) C45(0.25) H45A(0.25) H45B(0.25)
 C46(0.25) H46A(0.25) H46B(0.25) H46C(0.25)
7.a Ternary CH refined with riding coordinates:
 C2(H6), C5(H5)
7.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C21(H21),
 C23(H23), C29(H29), C31(H31)
7.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              58810
_shelx_hkl_checksum              72301
_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 1.193
_oxdiff_exptl_absorpt_empirical_full_min 0.858