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_7716600
_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         'C39 H54 Al I N2 O'
_chemical_formula_sum            'C39 H54 Al I N2 O'
_chemical_formula_weight         720.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 105.1050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4074(2)
_cell_length_b                   17.6989(2)
_cell_length_c                   19.0286(2)
_cell_measurement_reflns_used    11977
_cell_measurement_temperature    150
_cell_measurement_theta_max      77.3700
_cell_measurement_theta_min      3.4540
_cell_volume                     3709.11(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -81.00 -41.00   0.50    1.00    --  -46.70 107.00  73.00   80
  2  \w     27.00  52.00   0.50    1.00    --   46.70-107.00 -24.00   50
  3  \w    105.00 177.00   0.50    3.50    --  107.75 107.00  73.00  144
  4  \w     73.00  98.00   0.50    3.50    --  107.75-107.00 -24.00   50
  5  \w   -116.00 -61.00   0.50    1.00    --  -46.70 -57.00 -90.00  110
  6  \w    -79.00 -13.00   0.50    1.00    --  -46.70 125.00 120.00  132
  7  \w   -116.00 -24.00   0.50    1.00    --  -46.70 -77.00   0.00  184
  8  \w     37.00  63.00   0.50    3.50    --  107.75 -45.00   0.00   52
  9  \w    102.00 127.00   0.50    3.50    --  107.75  45.00 -60.00   50
 10  \w     65.00 109.00   0.50    3.50    --  107.75 -45.00   0.00   88
 11  \w     96.00 139.00   0.50    3.50    --  107.75  30.00   0.00   86
 12  \w     50.00  76.00   0.50    3.50    --  107.75-125.00  30.00   52
 13  \w     62.00 111.00   0.50    3.50    --  107.75-125.00 150.00   98
 14  \w     96.00 177.00   0.50    3.50    --  107.75 125.00 120.00  162
 15  \w    152.00 177.00   0.50    3.50    --  107.75 125.00-180.00   50
 16  \w    130.00 156.00   0.50    3.50    --  107.75  45.00 -60.00   52
 17  \w     35.00 104.00   0.50    3.50    --  107.75 -95.00  30.00  138
 18  \w     99.00 140.00   0.50    3.50    --  107.75 125.00-180.00   82
 19  \w     91.00 176.00   0.50    3.50    --  107.75  61.00-120.00  170
 20  \w     96.00 125.00   0.50    3.50    --  107.75 125.00 -30.00   58
 21  \w     35.00 119.00   0.50    3.50    --  107.75 -61.00 120.00  168
;
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27076
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.002
_diffrn_reflns_theta_min         3.468
_exptl_absorpt_coefficient_mu    7.237
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.74a (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    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0223P)^2^+2.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6493
_reflns_number_total             7750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01774a2.cif
_cod_data_source_block           (tBuDippNON)AlI
_cod_depositor_comments
'Adding full bibliography for 7716596--7716604.cif.'
_cod_database_code               7716600
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.595
_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:
 C30(H30), C33(H33)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C26(H26), C27(H27), C28(H28)
2.c 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              87804
_shelx_hkl_checksum              13333
_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
;