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_7716601
_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         'C46 H59 Al Fe N2 O3, 2(C6 H6)'
_chemical_formula_sum            'C58 H71 Al Fe N2 O3'
_chemical_formula_weight         926.99
_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             2024-06-02
_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                80.7550(10)
_cell_angle_beta                 77.6870(10)
_cell_angle_gamma                77.1070(10)
_cell_formula_units_Z            2
_cell_length_a                   10.71570(10)
_cell_length_b                   13.6963(2)
_cell_length_c                   18.2912(2)
_cell_measurement_reflns_used    19631
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.8820
_cell_measurement_theta_min      2.4860
_cell_volume                     2538.56(5)
_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      150.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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    -46.00  21.00   0.50    2.00    --  -46.70  99.00  96.00  134
  2  \w     -2.00  80.00   0.50    2.00    --   46.70 -99.00  -8.00  164
  3  \w     52.00 107.00   0.50    8.00    --  107.75 -99.00  -8.00  110
  4  \w    122.00 150.00   0.50    8.00    --  107.75  99.00  96.00   56
  5  \w    -36.00  27.00   0.50    2.00    --  -46.70  57.00-150.00  126
  6  \w    -86.00 -28.00   0.50    2.00    --  -46.70 125.00 120.00  116
  7  \w    -20.00   6.00   0.50    2.00    --  -46.70  57.00 -90.00   52
  8  \w     -8.00  28.00   0.50    2.00    --  -46.70  19.00   0.00   72
  9  \w   -117.00 -39.00   0.50    2.00    --  -46.70 -57.00   0.00  156
 10  \w     -4.00  29.00   0.50    2.00    --  -46.70  19.00 -90.00   66
 11  \w    -28.00  48.00   0.50    2.00    --   46.70 -19.00  30.00  152
 12  \w     65.00  91.00   0.50    2.00    --   46.70-125.00 -60.00   52
 13  \w     33.00  59.00   0.50    8.00    --  107.75 -30.00-120.00   52
 14  \w     32.00  58.00   0.50    8.00    --  107.75 -30.00  90.00   52
 15  \w     58.00 104.00   0.50    8.00    --  107.75 -95.00-150.00   92
 16  \w     34.00  59.00   0.50    8.00    --  107.75 -30.00 -60.00   50
 17  \w     35.00  66.00   0.50    8.00    --  107.75 -45.00-150.00   62
 18  \w    102.00 127.00   0.50    8.00    --  107.75-145.00-101.45   50
 19  \w     32.00  57.00   0.50    8.00    --  107.75 -30.00   0.00   50
 20  \w     87.00 112.00   0.50    8.00    --  107.75-125.00 120.00   50
 21  \w    136.00 175.00   0.50    8.00    --  107.75  30.00  90.00   78
 22  \w     32.00  59.00   0.50    8.00    --  107.75 -30.00  60.00   54
 23  \w     32.00  58.00   0.50    8.00    --  107.75 -30.00  30.00   52
 24  \w     32.00  59.00   0.50    8.00    --  107.75 -30.00 -30.00   54
 25  \w     36.00  93.00   0.50    8.00    --  107.75 -61.00  30.00  114
 26  \w    105.00 178.00   0.50    8.00    --  107.75  30.00 150.00  146
 27  \w     84.00 110.00   0.50    8.00    --  107.75-125.00   0.00   52
 28  \w     40.00  76.00   0.50    8.00    --  107.75 -77.00-150.00   72
 29  \w     83.00 119.00   0.50    8.00    --  107.75 -77.00-150.00   72
 30  \w     48.00  87.00   0.50    8.00    --  107.75 -77.00  30.00   78
 31  \w     91.00 117.00   0.50    8.00    --  107.75 -77.00  30.00   52
 32  \w     95.00 120.00   0.50    8.00    --  107.75  45.00-150.00   50
 33  \w     37.00  70.00   0.50    8.00    --  107.75-125.00   0.00   66
 34  \w     38.00  63.00   0.50    8.00    --  107.75 -45.00 -60.00   50
 35  \w     32.00  59.00   0.50    8.00    --  107.75 -30.00 150.00   54
 36  \w     72.00 106.00   0.50    8.00    --  107.75 -95.00 120.00   68
 37  \w     35.00  60.00   0.50    8.00    --  107.75 -45.00-120.00   50
 38  \w     33.00  59.00   0.50    8.00    --  107.75 -30.00 120.00   52
 39  \w     32.00  57.00   0.50    8.00    --  107.75 -30.00-150.00   50
 40  \w    138.00 166.00   0.50    8.00    --  107.75  45.00-150.00   56
 41  \w     36.00  92.00   0.50    8.00    --  107.75 -61.00  90.00  112
 42  \w     53.00 107.00   0.50    8.00    --  107.75-100.00 -46.50  108
 43  \w     34.00  88.00   0.50    8.00    --  107.75 -95.00-180.00  108
 44  \w     99.00 137.00   0.50    8.00    --  107.75 125.00-150.00   76
 45  \w     84.00 165.00   0.50    8.00    --  107.75  77.00   0.00  162
;
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.007
_diffrn_reflns_theta_min         2.490
_exptl_absorpt_coefficient_mu    2.894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84672
_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_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         10571
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0492P)^2^+0.8140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9984
_reflns_number_total             10571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (tBuDippNON)AlFp
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_database_code               7716601
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.869
_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. Uiso/Uaniso restraints and constraints
C53B \\sim C54B \\sim C55B \\sim C56B \\sim C57B \\sim C58B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C47A \\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C47B \\sim C48B \\sim C49B \\sim C50B \\sim C51B \\sim C52B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C58B)=Sof(H58B)=Sof(C53B)=Sof(H53B)=Sof(C54B)=Sof(H54B)=Sof(C55B)=
 Sof(H55B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=Sof(H57B)=1-FVAR(1)
 Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=
 Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C53A)=Sof(H53A)=FVAR(1)
 Sof(C51B)=Sof(H51B)=Sof(C52B)=Sof(H52B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=
 Sof(H48B)=Sof(C49B)=Sof(H49B)=Sof(C50B)=Sof(H50B)=1-FVAR(2)
 Sof(C52A)=Sof(H52A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=
 Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C26(H26), C27(H27), C28(H28), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C52A(H52A), C47A(H47A), C48A(H48A),
 C49A(H49A), C50A(H50A), C51A(H51A), C51B(H51B), C52B(H52B), C47B(H47B),
 C48B(H48B), C49B(H49B), C50B(H50B), C54A(H54A), C55A(H55A), C56A(H56A),
 C57A(H57A), C58A(H58A), C53A(H53A), C58B(H58B), C53B(H53B), C54B(H54B),
 C55B(H55B), C56B(H56B), C57B(H57B)
4.c Fitted hexagon refined as free rotating group:
 C52A(C47A,C48A,C49A,C50A,C51A), C51B(C52B,C47B,C48B,C49B,C50B), C54A(C55A,
 C56A,C57A,C58A,C53A), C58B(C53B,C54B,C55B,C56B,C57B)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), 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), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C)
;
_shelx_res_checksum              57168
_shelx_hkl_checksum              75602
_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
;