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_1567418
_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         'C90 H122 Al2 Fe2 I2 N4, C6 H14'
_chemical_formula_sum            'C96 H136 Al2 Fe2 I2 N4'
_chemical_formula_weight         1765.54
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-24
_audit_creation_method           'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_audit_update_record
;
2022-04-17 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                112.0886(13)
_cell_angle_beta                 93.6385(11)
_cell_angle_gamma                100.4721(13)
_cell_formula_units_Z            2
_cell_length_a                   15.8692(2)
_cell_length_b                   16.9522(3)
_cell_length_c                   18.67859(19)
_cell_measurement_reflns_used    28144
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.4100
_cell_measurement_theta_min      2.5930
_cell_volume                     4530.35(12)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9596
_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   -117.00 -44.00   0.50    0.88    --  -47.20 -44.00  20.00  146
  2  \w    -46.00  24.00   0.50    0.88    --  -47.20  44.00 171.00  140
  3  \w    -25.00  50.00   0.50    0.88    --   47.20 -44.00  20.00  150
  4  \w     47.00  73.00   0.50    0.88    --   47.20  44.00 171.00   52
  5  \w   -157.00-100.00   0.50    3.51    --  -86.25 -44.00  20.00  114
  6  \w    -47.00 -14.00   0.50    3.51    --  -86.25  44.00 171.00   66
  7  \w     95.00 177.00   0.50    3.51    --  107.11  44.00 171.00  164
  8  \w   -108.00 -82.00   0.50    0.88    --  -47.20-125.00 120.00   52
  9  \w    -84.00 -17.00   0.50    0.88    --  -47.20 125.00-150.00  134
 10  \w   -120.00 -82.00   0.50    0.88    --  -47.20-125.00 -30.00   76
 11  \w    -19.00   7.00   0.50    0.88    --  -47.20  19.00-150.00   52
 12  \w    -21.00  22.00   0.50    0.88    --   47.20 -77.00-180.00   86
 13  \w     37.00  70.00   0.50    0.88    --   47.20 -77.00-180.00   66
 14  \w    -21.00  19.00   0.50    0.88    --   47.20 -19.00-120.00   80
 15  \w   -136.00 -98.00   0.50    3.51    --  -86.25 -94.00 120.00   76
 16  \w    -56.00 -14.00   0.50    3.51    --  -86.25 125.00-120.00   84
 17  \w    -55.00 -28.00   0.50    3.51    --  -86.25 125.00   0.00   54
 18  \w     37.00  74.00   0.50    3.51    --  107.11 -77.00 -60.00   74
 19  \w     53.00 112.00   0.50    3.51    --  107.11-125.00 -30.00  118
 20  \w    102.00 177.00   0.50    3.51    --  107.11  45.00-150.00  150
 21  \w     41.00  67.00   0.50    3.51    --  107.11 -61.00-120.00   52
 22  \w     37.00 112.00   0.50    3.51    --  107.11-125.00  60.00  150
 23  \w     79.00 105.00   0.50    3.51    --  107.11 -94.00 150.00   52
 24  \w     38.00  97.00   0.50    3.51    --  107.11-125.00 120.00  118
 25  \w     39.00  71.00   0.50    3.51    --  107.11 -61.00 150.00   64
 26  \w     77.00 103.00   0.50    3.51    --  107.11-115.00 -82.98   52
 27  \w    126.00 164.00   0.50    3.51    --  107.11 125.00 120.00   76
 28  \w    101.00 137.00   0.50    3.51    --  107.11  15.00 120.00   72
 29  \w    152.00 177.00   0.50    3.51    --  107.11  15.00 120.00   50
 30  \w     41.00  68.00   0.50    3.51    --  107.11-130.00  18.87   54
 31  \w     76.00 115.00   0.50    3.51    --  107.11-130.00  18.87   78
 32  \w     35.00  72.00   0.50    3.51    --  107.11-115.00 -82.98   74
 33  \w     96.00 177.00   0.50    3.51    --  107.11  15.00 -60.00  162
 34  \w     35.00  80.00   0.50    3.51    --  107.11-125.00-150.00   90
 35  \w     87.00 112.00   0.50    3.51    --  107.11-125.00-150.00   50
 36  \w     96.00 172.00   0.50    3.51    --  107.11  77.00 120.00  152
 37  \w     55.00 112.00   0.50    3.51    --  107.11-125.00  90.00  114
 38  \w    106.00 142.00   0.50    3.51    --  107.11  30.00  60.00   72
 39  \w     42.00  67.00   0.50    3.51    --  107.11 -61.00  30.00   50
 40  \w    137.00 163.00   0.50    3.51    --  107.11 125.00 -30.00   52
 41  \w     37.00 107.00   0.50    3.51    --  107.11-110.00 127.39  140
 42  \w     44.00 121.00   0.50    3.51    --  107.11-137.00 -77.37  154
 43  \w     63.00 111.00   0.50    3.51    --  107.11-125.00-180.00   96
 44  \w    102.00 154.00   0.50    3.51    --  107.11 125.00-120.00  104
 45  \w     98.00 124.00   0.50    3.51    --  107.11 125.00 120.00   52
 46  \w     42.00  71.00   0.50    3.51    --  107.11 -61.00 -60.00   58
 47  \w     77.00 102.00   0.50    3.51    --  107.11 -77.00-150.00   50
 48  \w     43.00  68.00   0.50    3.51    --  107.11 -61.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0223769000
_diffrn_orient_matrix_UB_12      0.0896549000
_diffrn_orient_matrix_UB_13      -0.0055331000
_diffrn_orient_matrix_UB_21      0.0890214000
_diffrn_orient_matrix_UB_22      0.0204454000
_diffrn_orient_matrix_UB_23      0.0490182000
_diffrn_orient_matrix_UB_31      0.0391029000
_diffrn_orient_matrix_UB_32      -0.0407797000
_diffrn_orient_matrix_UB_33      -0.0752250000
_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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61135
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         77.4246
_diffrn_reflns_theta_min         2.5801
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.408
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53386
_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    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.702
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         18481
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+13.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15048
_reflns_number_total             18481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02783f2.cif
_cod_data_source_block           MaHa048_DeDh_a
_cod_depositor_comments
'Adding full bibliography for 1567415--1567421.cif.'
_cod_original_cell_volume        4530.36(11)
_cod_database_code               1567418
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.173
_shelx_estimated_absorpt_t_max   0.552
_shelx_res_checksum              73885
_cell_oxdiff_length_a            15.8692(2)
_cell_oxdiff_length_b            16.9522(3)
_cell_oxdiff_length_c            18.67859(19)
_cell_oxdiff_angle_alpha         112.0886(13)
_cell_oxdiff_angle_beta          93.6385(11)
_cell_oxdiff_angle_gamma         100.4721(13)
_cell_oxdiff_volume              4530.36(11)
_cell_oxdiff_measurement_reflns_used 28144
_oxdiff_exptl_absorpt_empirical_full_min 0.561
_oxdiff_exptl_absorpt_empirical_full_max 1.948
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
0181fcf989c718a49bf50b79c731ff790a0427208af
;
_diffrn_oxdiff_digest_hkl
;
0112154cc57ae6e0cef31b3a1b741d7ebb104f
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C96 H136 Al2 Fe2 I2 N4'