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_7716599
_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         'C38 H51 Al Fe N2 O3, C6 H14'
_chemical_formula_sum            'C44 H65 Al Fe N2 O3'
_chemical_formula_weight         752.81
_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
_atom_sites_solution_primary     dual
_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                85.068(3)
_cell_angle_beta                 76.654(4)
_cell_angle_gamma                71.928(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4105(4)
_cell_length_b                   11.6341(5)
_cell_length_c                   18.7132(7)
_cell_measurement_reflns_used    6094
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.2980
_cell_measurement_theta_min      11.5250
_cell_volume                     2096.23(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -40.00  26.00   0.50    6.00    --  -46.45  61.00  15.00  132
  2  \w    -21.00  13.00   0.50    6.00    --   46.45 -61.00-123.00   68
  3  \w     34.00 119.00   0.50    6.00    --   46.45  61.00  15.00  170
  4  \w     18.00  62.00   0.50    6.00    --   46.45 -61.00-123.00   88
  5  \w     36.00  79.00   0.50   24.00    --  107.75 -61.00-123.00   86
  6  \w     95.00 177.00   0.50   24.00    --  107.75  61.00  15.00  164
  7  \w    -19.00  21.00   0.50    6.00    --  -46.45  38.00 150.00   80
  8  \w     -6.00  30.00   0.50    6.00    --  -46.45  19.00   0.00   72
  9  \w     -7.00  26.00   0.50    6.00    --  -46.45  19.00 -60.00   66
 10  \w    -18.00  19.00   0.50    6.00    --  -46.45  38.00 -30.00   74
 11  \w   -114.00 -31.00   0.50    6.00    --  -46.45 -61.00-123.00  166
 12  \w     47.00  79.00   0.50    6.00    --   46.45-125.00-180.00   64
 13  \w     44.00  93.00   0.50    6.00    --   46.45-125.00  90.00   98
 14  \w     37.00  87.00   0.50    6.00    --   46.45-125.00 150.00  100
 15  \w     32.00  58.00   0.50   24.00    --  107.75 -30.00  60.00   52
 16  \w     72.00 100.00   0.50   24.00    --  107.75 -77.00-150.00   56
 17  \w     52.00 107.00   0.50   24.00    --  107.75 -97.00-158.69  110
 18  \w     45.00  74.00   0.50   24.00    --  107.75 -95.00-120.00   58
 19  \w     32.00  59.00   0.50   24.00    --  107.75 -30.00 150.00   54
 20  \w    101.00 129.00   0.50   24.00    --  107.75  30.00   0.00   56
 21  \w    100.00 177.00   0.50   24.00    --  107.75  77.00 -60.00  154
 22  \w     33.00  59.00   0.50   24.00    --  107.75 -30.00 -60.00   52
 23  \w     80.00 109.00   0.50   24.00    --  107.75-111.00  59.61   58
 24  \w     36.00  70.00   0.50   24.00    --  107.75-104.00 -38.61   68
 25  \w     32.00  59.00   0.50   24.00    --  107.75 -30.00  30.00   54
 26  \w     72.00 108.00   0.50   24.00    --  107.75-104.00 -38.61   72
 27  \w     76.00 101.00   0.50   24.00    --  107.75 -95.00 150.00   50
 28  \w    145.00 178.00   0.50   24.00    --  107.75  30.00-120.00   66
 29  \w     36.00  65.00   0.50   24.00    --  107.75 -45.00 120.00   58
 30  \w    140.00 172.00   0.50   24.00    --  107.75  45.00 -90.00   64
 31  \w    150.00 177.00   0.50   24.00    --  107.75  30.00 150.00   54
 32  \w     81.00 106.00   0.50   24.00    --  107.75 -95.00-120.00   50
 33  \w     38.00  69.00   0.50   24.00    --  107.75 -95.00  60.00   62
 34  \w     71.00 105.00   0.50   24.00    --  107.75 -95.00  60.00   68
 35  \w     32.00  58.00   0.50   24.00    --  107.75 -30.00-120.00   52
 36  \w     34.00 103.00   0.50   24.00    --  107.75 -95.00 -30.00  138
 37  \w    104.00 132.00   0.50   24.00    --  107.75  30.00-120.00   56
 38  \w    100.00 144.00   0.50   24.00    --  107.75  30.00 150.00   88
 39  \w    133.00 178.00   0.50   24.00    --  107.75  30.00   0.00   90
 40  \w     32.00  59.00   0.50   24.00    --  107.75 -30.00 -30.00   54
 41  \w     95.00 129.00   0.50   24.00    --  107.75  45.00 -90.00   68
 42  \w     34.00  83.00   0.50   24.00    --  107.75 -95.00-150.00   98
 43  \w     41.00 107.00   0.50   24.00    --  107.75-103.00 150.14  132
 44  \w     40.00  74.00   0.50   24.00    --  107.75-111.00  59.61   68
 45  \w     53.00 103.00   0.50   24.00    --  107.75 -95.00   0.00  100
 46  \w    102.00 132.00   0.50   24.00    --  107.75 125.00-180.00   60
 47  \w     66.00 122.00   0.50   24.00    --  107.75 -88.00  66.80  112
 48  \w     37.00  87.00   0.50   24.00    --  107.75 -61.00  60.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0017576000
_diffrn_orient_matrix_UB_12      0.1246852000
_diffrn_orient_matrix_UB_13      -0.0356946000
_diffrn_orient_matrix_UB_21      -0.1438775000
_diffrn_orient_matrix_UB_22      0.0567571000
_diffrn_orient_matrix_UB_23      0.0488546000
_diffrn_orient_matrix_UB_31      0.0686083000
_diffrn_orient_matrix_UB_32      0.0252671000
_diffrn_orient_matrix_UB_33      0.0591580000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10687
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.089
_diffrn_reflns_theta_max         67.089
_diffrn_reflns_theta_min         2.427
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0953
_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^)+(0.0236P)^2^+17.8279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.2424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9022
_reflns_number_total             10687
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 1.5096\% 
around [-0.76 -0.32 -0.56] (reciprocal) or [-0.99 -0.06 -0.11] (direct)
;
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (tBuNON)AlFp
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_database_code               7716599
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C44 H65 Al1 Fe1 N2 O3'
_chemical_oxdiff_usercomment     'tol - hex'
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.540(5)
 0.460(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C40-C39 = C41-C40 = C42-C41 = C43-C42 = C44-C43
 1.53 with sigma of 0.008
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C36) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C11(H11), C9(H9), C37(H37), C38(H38), C34(H34), C36(H36),
 C35(H35)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,H27B,
 H27C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C25(H25A,
 H25B,H25C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C),
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C39(H39A,H39B,
 H39C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              40295
_shelx_hkl_checksum              37021
_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 1.992
_oxdiff_exptl_absorpt_empirical_full_min 0.227
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2