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_1567421
_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 N4'
_chemical_formula_sum            'C90 H122 Al2 Fe2 N4'
_chemical_formula_weight         1425.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 105.079(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.856(8)
_cell_length_b                   14.800(4)
_cell_length_c                   29.131(10)
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.43
_cell_volume                     8266(5)
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX3 ver. 2019.1 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (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      100(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_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  0.0813
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            221609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         32.534
_diffrn_reflns_theta_min         1.998
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         28967
_refine_ls_number_restraints     1692
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+3.5778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18589
_reflns_number_total             28967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02783f2.cif
_cod_data_source_block           Test_1_a
_cod_depositor_comments
'Adding full bibliography for 1567415--1567421.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567421
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              80458