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_7135252
_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         'C33 H62 Al Fe N2 O P3'
_chemical_formula_sum            'C33 H62 Al Fe N2 O P3'
_chemical_formula_weight         678.58
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2p9ztt
_audit_creation_date             2025-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-08-22 deposited with the CCDC.	2025-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.26490(10)
_cell_length_b                   14.44850(10)
_cell_length_c                   17.29140(10)
_cell_measurement_reflns_used    18637
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.4670
_cell_measurement_theta_min      3.8060
_cell_volume                     3812.78(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      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    -67.00  32.00   1.00    1.00    --  -42.36  38.00-150.00   99
  2  \w     18.00 117.00   1.00    1.00    --   42.36  38.00-150.00   99
  3  \w     18.00 117.00   1.00    1.00    --   42.36  38.00 150.00   99
  4  \w     14.00 116.00   1.00    1.00    --   42.36  57.00 -60.00  102
  5  \w     77.00 178.00   1.00    3.38    --  105.75  61.00-120.00  101
  6  \w     23.00 109.00   1.00    3.38    --  105.75 -95.00-120.00   86
  7  \w     73.00 178.00   1.00    3.38    --  105.75  77.00  90.00  105
  8  \w     73.00 178.00   1.00    3.38    --  105.75  77.00  60.00  105
  9  \w     77.00 178.00   1.00    3.38    --  105.75  30.00   0.00  101
 10  \w     33.00 132.00   1.00    3.38    --  105.75 -45.00  90.00   99
 11  \w     80.00 178.00   1.00    3.38    --  105.75  45.00 150.00   98
 12  \w     53.00 178.00   1.00    3.38    --  105.75  15.00  90.00  125
 13  \w    -98.00  -2.00   1.00    1.00    --  -42.36 125.00-120.00   96
 14  \w     10.00 119.00   1.00    1.00    --   42.36  77.00  30.00  109
 15  \w     10.00 119.00   1.00    1.00    --   42.36  77.00-180.00  109
 16  \w      2.00  98.00   1.00    1.00    --   42.36-125.00  90.00   96
 17  \w     73.00 161.00   1.00    3.38    --  105.75  77.00-180.00   88
 18  \w     23.00 109.00   1.00    3.38    --  105.75 -95.00  60.00   86
;
_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      -0.0674450000
_diffrn_orient_matrix_UB_12      -0.0354324000
_diffrn_orient_matrix_UB_13      0.0579980000
_diffrn_orient_matrix_UB_21      0.0383557000
_diffrn_orient_matrix_UB_22      0.0658068000
_diffrn_orient_matrix_UB_23      0.0621560000
_diffrn_orient_matrix_UB_31      -0.0645743000
_diffrn_orient_matrix_UB_32      0.0760451000
_diffrn_orient_matrix_UB_33      -0.0267335000
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41433
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.812
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.775
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.310
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00096(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0413P)^2^+1.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6799
_reflns_number_total             7594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06456b3.cif
_cod_data_source_block           S4
_cod_database_code               7135252
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C33 H62 Al Fe N2 O P3'
_chemical_oxdiff_usercomment     BS006
_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:
 C3(H00H), C9(H00Z), C11(H00I), C18(H00G), C20(H00V)
2.b Idealised Me refined as rotating group:
 C1(H00W,H00X,H00Y), C5(H00M,H00N,H00O), C6(H00J,H00K,H00L), C13(H00P,H00Q,
 H00R), C14(H,HA,H00), C15(H00A,H00B,H00C), C22(H00D,H00E,H00F), C23(HF,HG,H7),
 C24(H00S,H00T,H00U), C25(H01J,H01K,H01L), C26(HC,HB,H5), C27(H01M,H01N,H01O),
 C28(H01D,H01E,H01F), C29(H01G,H01H,H01I), C30(HH,HI,H4), C31(H01P,H01Q,H01R),
 C32(HE,HD,H6), C33(H01A,H01B,H01C)
;
_shelx_res_checksum              25006
_shelx_hkl_checksum              1767
_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 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.905