Mechanochemical synthesis of iron aluminyl complexes.
Kallmeier, Fabian; Matthews, Aidan J. R.; Nelmes, Gareth R.; Lawson, Nina R.; Hicks, Jamie; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12450–12454; doi:10.1039/d4dt01774a

data_7716596
_publ_section_title
;
 Mechanochemical synthesis of iron aluminyl complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12450
_journal_page_last               12454
_journal_paper_doi               10.1039/d4dt01774a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C41 H70 Al I N2 O Si2, C6 H6'
_chemical_formula_sum            'C47 H76 Al I N2 O Si2'
_chemical_formula_weight         895.15
_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   geom
_audit_creation_date             2024-06-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                86.848(3)
_cell_angle_beta                 83.768(3)
_cell_angle_gamma                72.693(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4360(4)
_cell_length_b                   13.9695(5)
_cell_length_c                   14.6880(6)
_cell_measurement_reflns_used    16701
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.2490
_cell_measurement_theta_min      3.2960
_cell_volume                     2421.05(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_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    -68.00  -9.00   0.50    2.00    --  -46.57 120.00-177.00  118
  2  \w    -94.00 -68.00   0.50    2.00    --  -46.57-155.00 -58.00   52
  3  \w    -99.00 -73.00   0.50    2.00    --  -46.57 155.00 -20.00   52
  4  \w     89.00 115.00   0.50    2.00    --   46.57 155.00 -20.00   52
  5  \w     76.00 101.00   0.50    2.00    --   46.57-155.00 -58.00   50
  6  \w     30.00  86.00   0.50    2.00    --   46.57-120.00  98.00  112
  7  \w    113.00 138.00   0.50    7.50    --  107.75 120.00-177.00   50
  8  \w     51.00 105.00   0.50    7.50    --  107.75-120.00  98.00  108
  9  \w     91.00 128.00   0.50    7.50    --  107.75-155.00 -58.00   74
 10  \w     94.00 119.00   0.50    7.50    --  107.75 155.00 -20.00   50
 11  \w    -52.00 -26.00   0.50    2.00    --  -46.57 -77.00 -60.00   52
 12  \w     -8.00  30.00   0.50    2.00    --  -46.57  19.00 -60.00   76
 13  \w     -6.00  29.00   0.50    2.00    --  -46.57  19.00 -90.00   70
 14  \w    -22.00  25.00   0.50    2.00    --  -46.57  38.00 -30.00   94
 15  \w     -3.00  30.00   0.50    2.00    --  -46.57  19.00 150.00   66
 16  \w      2.00  28.00   0.50    2.00    --  -46.57  19.00  90.00   52
 17  \w    -92.00 -66.00   0.50    2.00    --  -46.57 -77.00 -60.00   52
 18  \w     -1.00  29.00   0.50    2.00    --  -46.57  19.00   0.00   60
 19  \w     -5.00  28.00   0.50    2.00    --  -46.57  19.00-150.00   66
 20  \w    -18.00  22.00   0.50    2.00    --  -46.57  38.00  60.00   80
 21  \w     32.00  57.00   0.50    7.50    --  107.75 -30.00 -30.00   50
 22  \w     95.00 163.00   0.50    7.50    --  107.75  45.00-180.00  136
 23  \w     42.00 108.00   0.50    7.50    --  107.75-102.00  89.81  132
 24  \w     32.00  59.00   0.50    7.50    --  107.75 -30.00 -90.00   54
 25  \w     44.00  69.00   0.50    7.50    --  107.75 -77.00  60.00   50
 26  \w     32.00  57.00   0.50    7.50    --  107.75 -30.00-150.00   50
 27  \w     37.00  72.00   0.50    7.50    --  107.75 -45.00-120.00   70
 28  \w     42.00  94.00   0.50    7.50    --  107.75-125.00 -30.00  104
 29  \w     66.00  98.00   0.50    7.50    --  107.75 -95.00   0.00   64
 30  \w     58.00  98.00   0.50    7.50    --  107.75-100.00 176.39   80
 31  \w     40.00 109.00   0.50    7.50    --  107.75-111.00-136.17  138
 32  \w    105.00 131.00   0.50    7.50    --  107.75  30.00  90.00   52
 33  \w    143.00 175.00   0.50    7.50    --  107.75  30.00  90.00   64
 34  \w     33.00  58.00   0.50    7.50    --  107.75 -30.00  90.00   50
 35  \w     44.00  75.00   0.50    7.50    --  107.75 -61.00-150.00   62
 36  \w     94.00 178.00   0.50    7.50    --  107.75  45.00  30.00  168
 37  \w     32.00  57.00   0.50    7.50    --  107.75 -30.00 120.00   50
 38  \w     97.00 178.00   0.50    7.50    --  107.75  45.00  60.00  162
 39  \w     58.00 100.00   0.50    7.50    --  107.75 -95.00-120.00   84
 40  \w     35.00 106.00   0.50    7.50    --  107.75 -95.00 120.00  142
 41  \w     35.00  66.00   0.50    7.50    --  107.75 -45.00-180.00   62
 42  \w     34.00  59.00   0.50    7.50    --  107.75 -30.00-180.00   50
 43  \w     59.00 124.00   0.50    7.50    --  107.75-141.00  10.24  130
 44  \w     34.00  65.00   0.50    7.50    --  107.75 -95.00-180.00   62
 45  \w    143.00 169.00   0.50    7.50    --  107.75 125.00 -60.00   52
 46  \w     35.00  69.00   0.50    7.50    --  107.75 -45.00  60.00   68
 47  \w     98.00 124.00   0.50    7.50    --  107.75 125.00 -60.00   52
 48  \w     75.00 106.00   0.50    7.50    --  107.75-103.00  40.55   62
 49  \w     49.00  93.00   0.50    7.50    --  107.75 -61.00 -30.00   88
 50  \w     34.00  67.00   0.50    7.50    --  107.75 -61.00 -60.00   66
 51  \w     40.00  73.00   0.50    7.50    --  107.75 -45.00 -60.00   66
 52  \w     54.00  90.00   0.50    7.50    --  107.75 -61.00-120.00   72
 53  \w     36.00  73.00   0.50    7.50    --  107.75 -45.00  90.00   74
 54  \w     33.00  59.00   0.50    7.50    --  107.75 -30.00 -60.00   52
 55  \w     62.00 107.00   0.50    7.50    --  107.75-108.00 114.03   90
 56  \w     84.00 109.00   0.50    7.50    --  107.75-112.00 -75.19   50
 57  \w     76.00 106.00   0.50    7.50    --  107.75 -95.00 -30.00   60
 58  \w    125.00 177.00   0.50    7.50    --  107.75  30.00 120.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.123
_diffrn_reflns_theta_min         3.315
_exptl_absorpt_coefficient_mu    6.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
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    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.796
_refine_diff_density_min         -1.890
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         10093
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0849P)^2^+1.7028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8548
_reflns_number_total             10093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (TIPSNON)AlI
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_database_code               7716596
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.262
_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. Restrained distances
 Si2-C39 = Si2A-C39A = Si2-C33 = Si2A-C36 = Si2-C36
 1.9 with sigma of 0.008
 Si2A-C33A
 1.9 with sigma of 0.008
 Si2-C36 = Si2A-C36A = Si2-C39 = Si2A-C39A = Si2-C33 = Si2A-C33A
 1.9 with sigma of 0.008
 C34-C33 = C35-C33 = C37-C36 = C38-C36 = C40-C39 = C41-C39 = C34A-C33A = C35A-
 C33A = C41A-C39A = C40A-C39A
 1.53 with sigma of 0.008
 Si1A-C24A = Si1-C24 = Si1-C27 = Si1A-C27A = Si1-C30 = Si1A-C30A
 1.9 with sigma of 0.008
 C29-C27 = C29A-C27A = C28-C27 = C28A-C27A = C32-C30 = C32A-C30A = C31-C30 =
 C31A-C30A = C25A-C24A = C25-C24 = C26-C24 = C26A-C24A
 1.53 with sigma of 0.008
 C37A-C36A = C38A-C36A
 1.53 with sigma of 0.008
 C43-C42 = C44-C43 = C44-C42_$1
 1.4 with sigma of 0.008
 C34-C35 = C37-C38 = C40-C41
 2.5 with sigma of 0.008
 C34A-C35A = C40A-C41A
 2.5 with sigma of 0.008
 C25-C26 = C28-C29 = C31-C32 = C25A-C26A = C28A-C29A = C31A-C32A
 2.5 with sigma of 0.008
 C37A-C38A
 2.5 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C21A \\sim C22 \\sim C22A \\sim C23 \\sim C23A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Si2 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40 \\sim C41: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Si2A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C39A \\sim C40A \\sim
C41A: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
Si1 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim
C31 \\sim C32: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Si1A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim
C30A \\sim C31A \\sim C32A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
4. Others
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
 Sof(Si2A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36A)=Sof(C37A)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=
 Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(3)
 Sof(Si2)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(3)
 Sof(Si1A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27A)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(4)
 Sof(Si1)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C24A(H24A), C27(H27), C27A(H27A), C30(H30), C30A(H30A), C33(H33),
 C33A(H33A), C36(H36), C36A(H36A), C39(H39), C39A(H39A)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,
 H16E,H16F), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C22(H22A,H22B,
 H22C), C22A(H22D,H22E,H22F), C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F),
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C26(H26A,H26B,H26C), C26A(H26D,H26E,
 H26F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C29(H29A,H29B,H29C),
 C29A(H29D,H29E,H29F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F), C32(H32A,H32B,
 H32C), C32A(H32D,H32E,H32F), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F),
 C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F), C37(H37A,H37B,H37C), C37A(H37D,H37E,
 H37F), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C40(H40A,H40B,H40C),
 C40A(H40D,H40E,H40F), C41(H41A,H41B,H41C), C41A(H41D,H41E,H41F)
;
_shelx_res_checksum              96629
_shelx_hkl_checksum              27069
_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
;