Stepwise reduction of a base-stabilised ferrocenyl aluminium(iii) dihalide for the synthesis of structurally-diverse dialane species
Dhara, Debabrata; Fantuzzi, Felipe; Härterich, Marcel; Dewhurst, Rian D.; Krummenacher, Ivo; Arrowsmith, Merle; Pranckevicius, Conor; Braunschweig, Holger; Chemical Science 13 (2022) 9693–9700; doi:10.1039/D2SC02783F

data_1567419
_publ_section_title
;
 Stepwise reduction of a base-stabilised ferrocenyl aluminium(iii)
 dihalide for the synthesis of structurally-diverse dialane species
;
_journal_issue                   33
_journal_name_full               'Chemical Science'
_journal_page_first              9693
_journal_page_last               9700
_journal_paper_doi               10.1039/D2SC02783F
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C97 H130 Al2 Fe2 I2 N4'
_chemical_formula_sum            'C97 H130 Al2 Fe2 I2 N4'
_chemical_formula_weight         1771.50
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2n (K.Radacki 2005-21)'
_audit_update_record
;
2022-04-17 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.1360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1651(2)
_cell_length_b                   19.7884(2)
_cell_length_c                   23.3393(2)
_cell_measurement_reflns_used    44871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.2850
_cell_measurement_theta_min      2.3990
_cell_volume                     9413.59(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(7)
_diffrn_detector                 'HPAD area detector (HyPix 6000)'
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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   -118.00 -56.00   0.50    3.00    --  -47.45-147.00  21.00  124
   2  \w    -84.00 -58.00   0.50    3.00    --  -47.45 124.00 -93.00   52
   3  \w   -116.00 -72.00   0.50    3.00    --  -47.45-124.00-173.00   88
   4  \w     54.00  93.00   0.50    3.00    --   47.45-124.00-173.00   78
   5  \w     53.00  86.00   0.50    3.00    --   47.45-147.00  21.00   66
   6  \w   -139.00-114.00   0.50   10.00    --  -86.25-124.00-173.00   50
   7  \w   -106.00 -81.00   0.50   10.00    --  -86.25-147.00  21.00   50
   8  \w     48.00  76.00   0.50   10.00    --  107.75-124.00-173.00   56
   9  \w    101.00 126.00   0.50   10.00    --  107.75 147.00  71.00   50
  10  \w    111.00 136.00   0.50   10.00    --  107.75 124.00 -93.00   50
  11  \w     87.00 112.00   0.50   10.00    --  107.75-147.00  21.00   50
  12  \w    -26.00  28.00   0.50    3.00    --  -47.45  19.00 -60.00  108
  13  \w   -119.00 -71.00   0.50    3.00    --  -47.45-125.00 120.00   96
  14  \w    -26.00  28.00   0.50    3.00    --  -47.45  19.00-180.00  108
  15  \w     -4.00  27.00   0.50    3.00    --  -47.45  19.00-150.00   62
  16  \w    101.00 127.00   0.50   10.00    --  107.75  77.00 -30.00   52
  17  \w    141.00 167.00   0.50   10.00    --  107.75  77.00 -30.00   52
  18  \w     42.00  67.00   0.50   10.00    --  107.75 -77.00-180.00   50
  19  \w     81.00 106.00   0.50   10.00    --  107.75 -94.00-180.00   50
  20  \w     43.00  71.00   0.50   10.00    --  107.75 -61.00-120.00   56
  21  \w     37.00 114.00   0.50   10.00    --  107.75-125.00-180.00  154
  22  \w     51.00  93.00   0.50   10.00    --  107.75 -77.00-120.00   84
  23  \w    142.00 176.00   0.50   10.00    --  107.75  15.00 -90.00   68
  24  \w     99.00 169.00   0.50   10.00    --  107.75  45.00 -60.00  140
  25  \w     91.00 117.00   0.50   10.00    --  107.75-125.00 -90.00   52
  26  \w     91.00 153.00   0.50   10.00    --  107.75  61.00-150.00  124
  27  \w     39.00  65.00   0.50   10.00    --  107.75 -94.00-180.00   52
  28  \w    100.00 159.00   0.50   10.00    --  107.75 125.00-120.00  118
  29  \w     38.00  68.00   0.50   10.00    --  107.75 -77.00-150.00   60
  30  \w     38.00 117.00   0.50   10.00    --  107.75-125.00 150.00  158
  31  \w     45.00  99.00   0.50   10.00    --  107.75 -77.00 -30.00  108
  32  \w     77.00 117.00   0.50   10.00    --  107.75-125.00 -30.00   80
  33  \w     49.00  75.00   0.50   10.00    --  107.75-125.00 -60.00   52
  34  \w     82.00 116.00   0.50   10.00    --  107.75-125.00 -60.00   68
  35  \w     40.00  66.00   0.50   10.00    --  107.75 -61.00  60.00   52
  36  \w     41.00  66.00   0.50   10.00    --  107.75-125.00   0.00   50
  37  \w     87.00 117.00   0.50   10.00    --  107.75-125.00-120.00   60
  38  \w     83.00 108.00   0.50   10.00    --  107.75 -94.00 150.00   50
  39  \w     38.00  63.00   0.50   10.00    --  107.75 -61.00-150.00   50
  40  \w     96.00 128.00   0.50   10.00    --  107.75  15.00-120.00   64
  41  \w    132.00 177.00   0.50   10.00    --  107.75  15.00-120.00   90
  42  \w     42.00  67.00   0.50   10.00    --  107.75 -61.00 -30.00   50
  43  \w    111.00 170.00   0.50   10.00    --  107.75  15.00-150.00  118
  44  \w     72.00 106.00   0.50   10.00    --  107.75 -77.00-180.00   68
  45  \w     38.00  67.00   0.50   10.00    --  107.75 -77.00 -90.00   58
  46  \w     41.00  66.00   0.50   10.00    --  107.75 -77.00  30.00   50
  47  \w     77.00 102.00   0.50   10.00    --  107.75 -77.00  30.00   50
  48  \w     41.00  67.00   0.50   10.00    --  107.75 -61.00 -60.00   52
  49  \w    102.00 127.00   0.50   10.00    --  107.75  15.00 -30.00   50
  50  \w    153.00 178.00   0.50   10.00    --  107.75  15.00 -30.00   50
  51  \w    106.00 132.00   0.50   10.00    --  107.75 -80.00  27.29   52
  52  \w     59.00  85.00   0.50   10.00    --  107.75 -77.00 120.00   52
  53  \w     40.00  81.00   0.50   10.00    --  107.75 -94.00 -30.00   82
  54  \w    138.00 173.00   0.50   10.00    --  107.75  45.00-120.00   70
  55  \w     94.00 120.00   0.50   10.00    --  107.75  15.00 -60.00   52
  56  \w    104.00 129.00   0.50   10.00    --  107.75  45.00-120.00   50

;
_diffrn_measurement_device_type  'Rigaku OD XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            121360
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.762
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'microfocus sealed tube (PhotonJet)'
_exptl_absorpt_coefficient_mu    8.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.73a (Rigaku Oxford Diffraction, 2020) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK 
scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.073
_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     1182
_refine_ls_number_reflns         19848
_refine_ls_number_restraints     1191
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0486P)^2^+12.2770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16709
_reflns_number_total             19848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02783f2.cif
_cod_data_source_block           MaHa102_DeDh_a
_cod_depositor_comments
'Adding full bibliography for 1567415--1567421.cif.'
_cod_original_cell_volume        9413.59(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1567419
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.396
_shelx_estimated_absorpt_t_max   0.687
_shelx_res_checksum              99880