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_7716603
_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         'C54 H67 Al Fe N2 O3'
_chemical_formula_sum            'C54 H67 Al Fe N2 O3'
_chemical_formula_weight         874.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 92.6500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.10740(10)
_cell_length_b                   18.5869(2)
_cell_length_c                   23.6162(2)
_cell_measurement_reflns_used    16687
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.6960
_cell_measurement_theta_min      3.0310
_cell_volume                     4870.40(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 0.998
_diffrn_measured_fraction_theta_max 0.978
_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   -105.00 -71.00   0.50    3.00    --  -46.57-136.00 -59.00   68
  2  \w   -113.00 -78.00   0.50    3.00    --  -46.57-134.00 119.00   70
  3  \w    -92.00 -50.00   0.50    3.00    --  -46.57 136.00   5.00   84
  4  \w     47.00  89.00   0.50    3.00    --   46.57-136.00 -59.00   84
  5  \w     44.00  69.00   0.50    3.00    --   46.57-134.00 119.00   50
  6  \w     99.00 141.00   0.50    9.00    --  107.75 134.00-173.00   84
  7  \w     92.00 118.00   0.50    9.00    --  107.75-134.00 119.00   52
  8  \w     81.00 117.00   0.50    9.00    --  107.75-136.00 -59.00   72
  9  \w    130.00 155.00   0.50    9.00    --  107.75 136.00   5.00   50
 10  \w     -4.00  23.00   0.50    3.00    --  -46.57  19.00 -60.00   54
 11  \w     -7.00  29.00   0.50    3.00    --  -46.57  19.00  90.00   72
 12  \w     -8.00  30.00   0.50    3.00    --  -46.57  19.00 -30.00   76
 13  \w     -2.00  27.00   0.50    3.00    --  -46.57  19.00   0.00   58
 14  \w     -8.00  30.00   0.50    3.00    --  -46.57  19.00  30.00   76
 15  \w     91.00 123.00   0.50    9.00    --  107.75  61.00  90.00   64
 16  \w     73.00 102.00   0.50    9.00    --  107.75-100.00 152.82   58
 17  \w     35.00  71.00   0.50    9.00    --  107.75 -45.00-120.00   72
 18  \w     90.00 123.00   0.50    9.00    --  107.75 -77.00 -60.00   66
 19  \w     35.00  71.00   0.50    9.00    --  107.75 -77.00 -60.00   72
 20  \w     32.00  57.00   0.50    9.00    --  107.75 -30.00-180.00   50
 21  \w     45.00  70.00   0.50    9.00    --  107.75-100.00 152.82   50
 22  \w     50.00  75.00   0.50    9.00    --  107.75 -95.00 120.00   50
 23  \w     96.00 165.00   0.50    9.00    --  107.75  30.00 120.00  138
 24  \w    109.00 172.00   0.50    9.00    --  107.75 125.00  30.00  126
 25  \w    130.00 157.00   0.50    9.00    --  107.75  61.00  90.00   54
 26  \w     40.00  71.00   0.50    9.00    --  107.75 -45.00 -60.00   62
 27  \w     42.00  68.00   0.50    9.00    --  107.75 -45.00 120.00   52
 28  \w     94.00 176.00   0.50    9.00    --  107.75 125.00 -60.00  164
 29  \w    102.00 176.00   0.50    9.00    --  107.75  45.00-120.00  148
 30  \w     75.00 109.00   0.50    9.00    --  107.75-109.00-165.33   68
 31  \w     52.00  93.00   0.50    9.00    --  107.75 -61.00  30.00   82
 32  \w     44.00 109.00   0.50    9.00    --  107.75-112.00 159.18  130
 33  \w     32.00  57.00   0.50    9.00    --  107.75 -30.00 120.00   50
;
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43061
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.019
_diffrn_reflns_theta_min         3.027
_exptl_absorpt_coefficient_mu    2.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82151
_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    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10185
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0405P)^2^+1.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9027
_reflns_number_total             10185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (DippNON)AlFp
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_database_code               7716603
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.841
_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
 C14-C17 \\sim C14-C17A
 with sigma of 0.02
 C14-C15 \\sim C14-C15A
 with sigma of 0.02
 C14-C16 \\sim C14-C16A
 with sigma of 0.02
3. 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)
4.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C42(H42), C45(H45)
4.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), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
4.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), 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              13127
_shelx_hkl_checksum              17665
_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
;