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_7716604
_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         'C106 H134 Al2 Fe2 N4 O4, 5(C6 H6)'
_chemical_formula_sum            'C136 H164 Al2 Fe2 N4 O4'
_chemical_formula_weight         2084.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-02
_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                90
_cell_angle_beta                 94.0477(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.70547(11)
_cell_length_b                   19.02701(8)
_cell_length_c                   25.22918(9)
_cell_measurement_reflns_used    60759
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.8740
_cell_measurement_theta_min      2.9150
_cell_volume                     11829.93(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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     -8.00  17.00   0.50    1.00    --  -46.45  25.00  38.00   50
  2  \w   -119.00 -35.00   0.50    1.00    --  -46.45 -25.00-124.00  168
  3  \w     25.00  52.00   0.50    1.00    --   46.45 -25.00-124.00   54
  4  \w     36.00 121.00   0.50    1.00    --   46.45  25.00  38.00  170
  5  \w    124.00 150.00   0.50    4.00    --  107.75  25.00  38.00   52
  6  \w     -3.00  28.00   0.50    1.00    --  -46.45  19.00-120.00   62
  7  \w     -1.00  25.00   0.50    1.00    --  -46.45  19.00 -30.00   52
  8  \w    -23.00  25.00   0.50    1.00    --  -46.45  57.00-180.00   96
  9  \w     -8.00  29.00   0.50    1.00    --  -46.45  19.00 -60.00   74
 10  \w     -8.00  26.00   0.50    1.00    --  -46.45  19.00-180.00   68
 11  \w     38.00  90.00   0.50    1.00    --   46.45-125.00 -60.00  104
 12  \w     41.00  83.00   0.50    1.00    --   46.45-125.00-150.00   84
 13  \w     33.00  87.00   0.50    1.00    --   46.45-125.00 150.00  108
 14  \w    139.00 178.00   0.50    4.00    --  107.75  15.00 -60.00   78
 15  \w     93.00 119.00   0.50    4.00    --  107.75 -77.00-150.00   52
 16  \w    101.00 127.00   0.50    4.00    --  107.75  15.00 -60.00   52
 17  \w     39.00  65.00   0.50    4.00    --  107.75-125.00 120.00   52
 18  \w     77.00 112.00   0.50    4.00    --  107.75-125.00 120.00   70
 19  \w     32.00  59.00   0.50    4.00    --  107.75 -30.00 150.00   54
 20  \w     35.00  85.00   0.50    4.00    --  107.75 -61.00 -90.00  100
 21  \w     35.00  73.00   0.50    4.00    --  107.75 -77.00-150.00   76
 22  \w     86.00 138.00   0.50    4.00    --  107.75  77.00 -90.00  104
 23  \w     94.00 140.00   0.50    4.00    --  107.75  15.00-150.00   92
 24  \w     37.00  72.00   0.50    4.00    --  107.75 -45.00-150.00   70
 25  \w    146.00 173.00   0.50    4.00    --  107.75  15.00-150.00   54
 26  \w     32.00  58.00   0.50    4.00    --  107.75 -30.00 -30.00   52
 27  \w     75.00 103.00   0.50    4.00    --  107.75 -95.00 -60.00   56
 28  \w     66.00 104.00   0.50    4.00    --  107.75 -95.00  60.00   76
 29  \w     43.00  69.00   0.50    4.00    --  107.75 -45.00  30.00   52
 30  \w     34.00  83.00   0.50    4.00    --  107.75 -61.00-150.00   98
 31  \w     45.00  77.00   0.50    4.00    --  107.75 -95.00-180.00   64
 32  \w     61.00 107.00   0.50    4.00    --  107.75-103.00-102.97   92
 33  \w     36.00  62.00   0.50    4.00    --  107.75 -95.00-120.00   52
 34  \w     94.00 142.00   0.50    4.00    --  107.75 125.00-180.00   96
 35  \w     37.00  65.00   0.50    4.00    --  107.75-125.00 150.00   56
 36  \w     35.00  60.00   0.50    4.00    --  107.75 -45.00   0.00   50
 37  \w    105.00 165.00   0.50    4.00    --  107.75  15.00  90.00  120
 38  \w     36.00 106.00   0.50    4.00    --  107.75 -95.00 -30.00  140
 39  \w     71.00 106.00   0.50    4.00    --  107.75 -95.00   0.00   70
 40  \w     58.00  84.00   0.50    4.00    --  107.75 -61.00 150.00   52
 41  \w     57.00  83.00   0.50    4.00    --  107.75-125.00  30.00   52
 42  \w     37.00  67.00   0.50    4.00    --  107.75-125.00-150.00   60
 43  \w     82.00 112.00   0.50    4.00    --  107.75-125.00-150.00   60
 44  \w    105.00 133.00   0.50    4.00    --  107.75  30.00 150.00   56
 45  \w    149.00 178.00   0.50    4.00    --  107.75  77.00 -90.00   58
 46  \w     56.00 109.00   0.50    4.00    --  107.75 -85.00   0.64  106
 47  \w     71.00 112.00   0.50    4.00    --  107.75-125.00-180.00   82
 48  \w    127.00 152.00   0.50    4.00    --  107.75  30.00   0.00   50
 49  \w    126.00 178.00   0.50    4.00    --  107.75 125.00 -30.00  104
 50  \w    131.00 156.00   0.50    4.00    --  107.75 125.00  90.00   50
 51  \w    131.00 157.00   0.50    4.00    --  107.75  15.00  30.00   52
 52  \w    120.00 145.00   0.50    4.00    --  107.75  45.00-150.00   50
 53  \w     35.00  67.00   0.50    4.00    --  107.75 -45.00 -30.00   64
 54  \w     94.00 119.00   0.50    4.00    --  107.75-133.00 -80.73   50
 55  \w     35.00  60.00   0.50    4.00    --  107.75 -45.00 120.00   50
 56  \w    102.00 153.00   0.50    4.00    --  107.75  15.00   0.00  102
 57  \w    132.00 158.00   0.50    4.00    --  107.75  15.00  60.00   52
 58  \w     36.00  61.00   0.50    4.00    --  107.75 -77.00 -60.00   50
 59  \w     87.00 113.00   0.50    4.00    --  107.75 -77.00 -60.00   52
 60  \w     55.00 106.00   0.50    4.00    --  107.75 -81.00  15.18  102
 61  \w     34.00  68.00   0.50    4.00    --  107.75 -61.00  30.00   68
 62  \w     83.00 111.00   0.50    4.00    --  107.75-125.00 150.00   56
 63  \w     81.00 106.00   0.50    4.00    --  107.75 -95.00 -90.00   50
 64  \w     79.00 104.00   0.50    4.00    --  107.75 -95.00  90.00   50
 65  \w     76.00 109.00   0.50    4.00    --  107.75-109.00 -10.62   66
 66  \w     78.00 112.00   0.50    4.00    --  107.75-125.00-120.00   68
 67  \w     41.00  81.00   0.50    4.00    --  107.75 -73.00-167.85   80
 68  \w     32.00  58.00   0.50    4.00    --  107.75 -30.00 120.00   52
 69  \w     38.00  64.00   0.50    4.00    --  107.75 -95.00   0.00   52
 70  \w    114.00 161.00   0.50    4.00    --  107.75  45.00 -90.00   94
 71  \w     99.00 125.00   0.50    4.00    --  107.75  45.00  60.00   52
 72  \w    105.00 130.00   0.50    4.00    --  107.75  88.00 -65.94   50
 73  \w     79.00 105.00   0.50    4.00    --  107.75 -95.00 120.00   52
 74  \w     44.00  69.00   0.50    4.00    --  107.75 -77.00  60.00   50
 75  \w     40.00  66.00   0.50    4.00    --  107.75 -77.00  90.00   52
 76  \w     84.00 119.00   0.50    4.00    --  107.75 -77.00  90.00   70
 77  \w    100.00 129.00   0.50    4.00    --  107.75  77.00  60.00   58
 78  \w    136.00 162.00   0.50    4.00    --  107.75  77.00  60.00   52
 79  \w     79.00 104.00   0.50    4.00    --  107.75   0.00-180.00   50
 80  \w    131.00 157.00   0.50    4.00    --  107.75   0.00-180.00   52
 81  \w     37.00  71.00   0.50    4.00    --  107.75 -95.00 120.00   68
;
_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  0.0625
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            120135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.023
_diffrn_reflns_theta_min         2.934
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67291
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         12597
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.909
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+11.9060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11977
_reflns_number_total             12597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           '[(DippNON)AlOCFeCp]2'
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_original_cell_volume        11829.92(9)
_cod_database_code               7716604
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.917
_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
 C16-C14 = C16A-C14 = C17-C14 = C17A-C14 = C15-C14 = C15A-C14
 1.53 with sigma of 0.008
 C69-C66 = C70-C69 = C70_$2-C70
 1.4 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C15A \\sim C16 \\sim C16A \\sim C17 \\sim C17A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71: 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)
 Fixed Sof: C66(0.5) H66(0.5) C71(0.5) H71(0.5) C70(0.5) H70(0.5) C69(0.5)
 H69(0.5) C68(0.5) H68(0.5) C67(0.5) H67(0.5)
5.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C42(H42), C45(H45)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C26(H26), C27(H27), C28(H28), C38(H38),
 C39(H39), C40(H40), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C65(H65),
 C64(H64), C63(H63), C62(H62), C61(H61), C66(H66), C71(H71), C70(H70), C69(H69),
  C68(H68), C67(H67)
5.c Fitted hexagon refined as free rotating group:
 C54(C55,C56,C57,C58,C59), C60(C65,C64,C63,C62,C61), C66(C71,C70,C69,C68,C67)
5.d 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), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C)
;
_shelx_res_checksum              28314
_shelx_hkl_checksum              40759
_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
;