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_1567420
_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         'C96 H136 Al2 Fe2 N4'
_chemical_formula_sum            'C96 H136 Al2 Fe2 N4'
_chemical_formula_weight         1511.74
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2x (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                 91.562(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.996(8)
_cell_length_b                   29.021(14)
_cell_length_c                   19.433(10)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.21
_cell_volume                     9018(8)
_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 4.166
_diffrn_detector_type            Apex2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1216
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            111641
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.382
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_min         1.261
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Nonius FR-591'
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.6565
_exptl_absorpt_correction_T_min  0.5802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         16515
_refine_ls_number_restraints     1141
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0479P)^2^+14.0878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12605
_reflns_number_total             16515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02783f2.cif
_cod_data_source_block           test1
_cod_depositor_comments
'Adding full bibliography for 1567415--1567421.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1567420
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              28720