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_7716598
_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         'C48 H75 Al Fe N2 O3 Si2, C6 H6'
_chemical_formula_sum            'C54 H81 Al Fe N2 O3 Si2'
_chemical_formula_weight         945.21
_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                96.1280(10)
_cell_angle_beta                 97.6050(10)
_cell_angle_gamma                113.366(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9890(2)
_cell_length_b                   15.0157(2)
_cell_length_c                   16.5211(3)
_cell_measurement_reflns_used    12249
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      77.2640
_cell_measurement_theta_min      2.7350
_cell_volume                     2664.49(9)
_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_environment      N~2~
_diffrn_ambient_temperature      150.01(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 0.957
_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    -83.00 -38.00   0.50    7.00    --  -46.57 108.00-131.00   90
  2  \w    -30.00   1.00   0.50    7.00    --  -46.57 108.00-131.00   62
  3  \w     25.00  53.00   0.50    7.00    --   46.57-108.00 132.00   56
  4  \w    -42.00  13.00   0.50    7.00    --  -46.57  57.00  60.00  110
  5  \w     -7.00  30.00   0.50    7.00    --  -46.57  19.00 -60.00   74
  6  \w    -22.00  27.00   0.50    7.00    --  -46.57  38.00-180.00   98
  7  \w     -2.00  24.00   0.50    7.00    --  -46.57  19.00 -30.00   52
  8  \w    -22.00  16.00   0.50    7.00    --  -46.57  38.00-150.00   76
  9  \w    -92.00 -42.00   0.50    7.00    --  -46.57 -38.00 -30.00  100
 10  \w     -6.00  23.00   0.50    7.00    --  -46.57  19.00 150.00   58
 11  \w     -7.00  26.00   0.50    7.00    --  -46.57  19.00 -90.00   66
 12  \w     33.00  93.00   0.50    7.00    --   46.57-125.00  60.00  120
 13  \w    127.00 154.00   0.50   28.00    --  107.75 108.00-131.00   54
 14  \w     37.00  73.00   0.50   28.00    --  107.75 -45.00   0.00   72
 15  \w     32.00  57.00   0.50   28.00    --  107.75 -30.00-150.00   50
 16  \w     40.00  74.00   0.50   28.00    --  107.75-125.00   0.00   68
 17  \w     72.00 104.00   0.50   28.00    --  107.75-125.00 -90.00   64
 18  \w     94.00 168.00   0.50   28.00    --  107.75  45.00 120.00  148
 19  \w     39.00  69.00   0.50   28.00    --  107.75 -45.00 150.00   60
 20  \w    136.00 162.00   0.50   28.00    --  107.75  45.00 150.00   52
 21  \w    152.00 178.00   0.50   28.00    --  107.75  30.00  30.00   52
 22  \w    102.00 145.00   0.50   28.00    --  107.75  30.00  30.00   86
 23  \w     57.00 105.00   0.50   28.00    --  107.75 -95.00 150.00   96
 24  \w     47.00 111.00   0.50   28.00    --  107.75-125.00  30.00  128
 25  \w     33.00  58.00   0.50   28.00    --  107.75 -30.00-180.00   50
 26  \w     40.00  72.00   0.50   28.00    --  107.75 -45.00 120.00   64
 27  \w     42.00  68.00   0.50   28.00    --  107.75 -45.00-120.00   52
 28  \w     85.00 112.00   0.50   28.00    --  107.75-125.00   0.00   54
 29  \w     40.00  73.00   0.50   28.00    --  107.75 -45.00  60.00   66
 30  \w     33.00  58.00   0.50   28.00    --  107.75 -30.00 -30.00   50
 31  \w     55.00 104.00   0.50   28.00    --  107.75 -95.00  30.00   98
 32  \w     94.00 178.00   0.50   28.00    --  107.75  45.00  90.00  168
 33  \w     32.00  57.00   0.50   28.00    --  107.75 -30.00 120.00   50
 34  \w     34.00  92.00   0.50   28.00    --  107.75 -61.00  60.00  116
 35  \w     97.00 131.00   0.50   28.00    --  107.75 125.00   0.00   68
 36  \w     36.00  92.00   0.50   28.00    --  107.75 -61.00-120.00  112
 37  \w     39.00  66.00   0.50   28.00    --  107.75 -45.00-180.00   54
 38  \w     32.00  57.00   0.50   28.00    --  107.75 -30.00 -60.00   50
 39  \w     32.00  57.00   0.50   28.00    --  107.75 -30.00 150.00   50
 40  \w     67.00  92.00   0.50   28.00    --  107.75 -95.00  60.00   50
 41  \w     97.00 124.00   0.50   28.00    --  107.75  45.00 150.00   54
 42  \w     70.00 107.00   0.50   28.00    --  107.75-101.00-124.89   74
 43  \w     71.00 108.00   0.50   28.00    --  107.75-108.00 132.00   74
;
_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      0.0570626000
_diffrn_orient_matrix_UB_12      0.0208869000
_diffrn_orient_matrix_UB_13      0.0929469000
_diffrn_orient_matrix_UB_21      0.0413402000
_diffrn_orient_matrix_UB_22      0.1113108000
_diffrn_orient_matrix_UB_23      0.0011395000
_diffrn_orient_matrix_UB_31      -0.1239890000
_diffrn_orient_matrix_UB_32      -0.0076872000
_diffrn_orient_matrix_UB_33      0.0221224000
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29255
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.067
_diffrn_reflns_theta_min         2.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63216
_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    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0651P)^2^+2.1907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9167
_reflns_number_total             10909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (TIPSNON)AlFp
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_original_cell_volume        2664.49(8)
_cod_database_code               7716598
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H O N Al Fe Si'
_chemical_oxdiff_usercomment     'from benzene-d6'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.542
_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 Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C30(H30), C33(H33), C36(H36), C39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
2.c Fitted hexagon refined as free rotating group:
 C49(C50,C51,C52,C53,C54)
2.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), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              67843
_shelx_hkl_checksum              75496
_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 2.321
_oxdiff_exptl_absorpt_empirical_full_min 0.502