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_7716602
_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         '2(C43 H49 Al Fe N2 O2 Si), C6 H12'
_chemical_formula_sum            'C92 H110 Al2 Fe2 N4 O4 Si2'
_chemical_formula_weight         1557.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-01
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4527(2)
_cell_length_b                   19.4412(2)
_cell_length_c                   44.6082(6)
_cell_measurement_reflns_used    22592
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      77.5530
_cell_measurement_theta_min      3.0190
_cell_volume                     16870.1(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.967
_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    -96.00 -41.00   0.50    5.00    --  -46.57 -45.00  53.00  110
  2  \w     94.00 178.00   0.50   20.00    --  107.75  45.00-156.00  168
  3  \w     35.00  60.00   0.50   20.00    --  107.75 -45.00  53.00   50
  4  \w     46.00  81.00   0.50   20.00    --  107.75 -81.00-144.00   70
  5  \w    117.00 160.00   0.50   20.00    --  107.75 106.00  65.00   86
  6  \w    -22.00  18.00   0.50    5.00    --  -46.57  38.00-120.00   80
  7  \w     -8.00  27.00   0.50    5.00    --  -46.57  19.00 -30.00   70
  8  \w     -4.00  30.00   0.50    5.00    --  -46.57  19.00-150.00   68
  9  \w    -22.00   3.00   0.50    5.00    --  -46.57  38.00   0.00   50
 10  \w      4.00  29.00   0.50    5.00    --  -46.57  19.00-180.00   50
 11  \w     32.00  59.00   0.50   20.00    --  107.75 -30.00 -90.00   54
 12  \w     32.00  59.00   0.50   20.00    --  107.75 -30.00-180.00   54
 13  \w     40.00  87.00   0.50   20.00    --  107.75 -61.00   0.00   94
 14  \w     33.00  59.00   0.50   20.00    --  107.75 -30.00  60.00   52
 15  \w     34.00  59.00   0.50   20.00    --  107.75 -30.00  30.00   50
 16  \w     32.00  57.00   0.50   20.00    --  107.75 -30.00-150.00   50
 17  \w     32.00  58.00   0.50   20.00    --  107.75 -30.00-120.00   52
 18  \w     83.00 114.00   0.50   20.00    --  107.75 -81.00-144.00   62
;
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            72374
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.112
_diffrn_reflns_theta_min         3.014
_exptl_absorpt_coefficient_mu    3.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73923
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             6624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         17462
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+8.8226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14131
_reflns_number_total             17462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (DAS)AlFp
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_database_code               7716602
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.530
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C50-C46 = C47-C46 = C48-C47 = C48-C49 = C50-C49
 1.4 with sigma of 0.008
 C46A-C50A = C49A-C48A = C49A-C50A = C47A-C48A = C47A-C46A
 1.4 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=
 Sof(H49A)=Sof(C50A)=Sof(H50A)=1-FVAR(1)
 Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=
 Sof(C50)=Sof(H50)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29), C57(H57), C60(H60), C69(H69), C72(H72)
5.b Secondary CH2 refined with riding coordinates:
 C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,
 H91B), C92(H92A,H92B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C22(H22), C23(H23), C24(H24), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C46A(H46A),
 C47(H47), C47A(H47A), C48(H48), C48A(H48A), C49(H49), C49A(H49A), C50(H50),
 C50A(H50A), C53(H53), C54(H54), C55(H55), C65(H65), C66(H66), C67(H67),
 C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84),
  C85(H85), C86(H86)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,
 H73C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              34848
_shelx_hkl_checksum              38365
_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
;