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_1567417
_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         'C104 H146 Al2 Fe2 I2 N4'
_chemical_formula_sum            'C104 H146 Al2 Fe2 I2 N4'
_chemical_formula_weight         1871.70
_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   difm
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-17 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.357(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.797(3)
_cell_length_b                   16.275(4)
_cell_length_c                   19.697(6)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      2.56
_cell_volume                     4980(2)
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8-Quest with Photon2'
_diffrn_measurement.method       '\w and \f scans'
_diffrn_radiation.monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62023
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.831
_diffrn_reflns_theta_min         2.461
_diffrn_source                   'microfocus sealed X--ray tube'
_diffrn_source.type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       Block
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.950
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         14170
_refine_ls_number_restraints     1003
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0720P)^2^+20.3213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9525
_reflns_number_total             14170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02783f2.cif
_cod_data_source_block           test_1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1567415--1567421.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1567417
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              72793