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_7135249
_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         'C35 H57 Al Fe N2 P2 Si'
_chemical_formula_sum            'C35 H57 Al Fe N2 P2 Si'
_chemical_formula_weight         678.68
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2p9zmm
_audit_creation_date             2024-10-11
_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                75.091(5)
_cell_angle_beta                 80.271(5)
_cell_angle_gamma                71.666(6)
_cell_formula_units_Z            2
_cell_length_a                   10.8871(7)
_cell_length_b                   11.7522(7)
_cell_length_c                   16.8494(9)
_cell_measurement_reflns_used    4970
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      73.1950
_cell_measurement_theta_min      4.0570
_cell_volume                     1968.4(2)
_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      172.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.942
_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     17.00 116.00   1.00    1.02    --   41.98  38.00  60.00   99
  2  \w     78.00 112.00   1.00    3.06    --  105.13  30.00  90.00   34
  3  \w    141.00 174.00   1.00    3.06    --  105.13  30.00  90.00   33
  4  \w     89.00 159.00   1.00    3.06    --  105.13  30.00   0.00   70
  5  \w     35.00 109.00   1.00    3.06    --  105.13 -95.00  60.00   74
  6  \w     36.00 109.00   1.00    3.06    --  105.13 -95.00 -60.00   73
  7  \w     37.00 130.00   1.00    3.06    --  105.13 -45.00 -90.00   93
  8  \w     34.00 109.00   1.00    3.06    --  105.13 -95.00-180.00   75
  9  \w     29.00 122.00   1.00    3.06    --  105.13 -30.00  30.00   93
 10  \w     29.00 122.00   1.00    3.06    --  105.13 -30.00 150.00   93
 11  \w    -24.00  67.00   1.00    1.02    --   41.98 -38.00-120.00   91
 12  \w    -98.00  -2.00   1.00    1.02    --  -41.98 125.00 120.00   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      -0.0676312000
_diffrn_orient_matrix_UB_12      0.1259260000
_diffrn_orient_matrix_UB_13      -0.0523836000
_diffrn_orient_matrix_UB_21      -0.1080246000
_diffrn_orient_matrix_UB_22      0.0213445000
_diffrn_orient_matrix_UB_23      0.0710783000
_diffrn_orient_matrix_UB_31      0.0786461000
_diffrn_orient_matrix_UB_32      0.0609170000
_diffrn_orient_matrix_UB_33      0.0352052000
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11702
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.789
_diffrn_reflns_theta_min         4.061
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.519
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.416
_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             728
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7517
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.3929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6001
_reflns_number_total             7517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06456b3.cif
_cod_data_source_block           2a
_cod_database_code               7135249
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35 H57 Al1 Fe1 N2 P2 Si1'
_chemical_oxdiff_usercomment     BS171-B
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-H1A \\sim Si1-H1B
 with sigma of 0.02
 Fe1-P1 \\sim Fe1-P1A
 with sigma of 0.02
 P1-C30 \\sim P1A-C30A
 with sigma of 0.02
 P1-C32 \\sim P1A-C32A
 with sigma of 0.02
 P1-C31 \\sim P1A-C31A
 with sigma of 0.02
 Fe1-C30 \\sim Fe1-C30A
 with sigma of 0.04
 Fe1-C32 \\sim Fe1-C32A
 with sigma of 0.04
 Fe1-C31 \\sim Fe1-C31A
 with sigma of 0.04
 C30-C32 \\sim C30A-C32A
 with sigma of 0.04
 C30-C31 \\sim C30A-C31A
 with sigma of 0.04
 C32-C31 \\sim C32A-C31A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P1 \\sim H1A \\sim C30 \\sim C32 \\sim C31 \\sim P1A \\sim C30A \\sim C32A
\\sim C31A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
4. Rigid body (RIGU) restrains
 P1, C30, C32, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1A, C30A, C32A, C31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, C30, C32, C31, P1A, C30A, C32A, C31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P1A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C32A)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=Sof(C31A)=Sof(H31E)=Sof(H31F)=Sof(H31D)=1-FVAR(1)
 Sof(P1)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C8(H8), C16(H16), C14(H14), C25(H25), C2(H2), C3(H3), C6(H6),
 C5(H5), C4(H4)
6.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C33(H33A,H33B,
 H33C), C18(H18A,H18B,H18C), C35(H35A,H35B,H35C), C28(H28A,H28B,H28C), C10(H10A,
 H10B,H10C), C29(H29A,H29B,H29C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C),
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C30A(H30D,H30E,
 H30F), C32A(H32D,H32E,H32F), C31A(H31E,H31F,H31D)
;
_shelx_res_checksum              59140
_shelx_hkl_checksum              62865
_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 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.836