Monomeric tri-coordinated bis(ferrocenyl)haloalumanes.
Anzai, Togo; Sugamata, Koh; Sasamori, Takahiro; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1360–1364; doi:10.1039/d4dt03233k

data_7718228
_publ_section_title
;
 Monomeric tri-coordinated bis(ferrocenyl)haloalumanes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1360
_journal_page_last               1364
_journal_paper_doi               10.1039/d4dt03233k
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C76 H98 Al Br Fe2, 0.5(C6 H14)'
_chemical_formula_sum            'C79 H105 Al Br Fe2'
_chemical_formula_weight         1273.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2lm4m0
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2024-11-11 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.980(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.2977(8)
_cell_length_b                   11.2247(2)
_cell_length_c                   24.8238(6)
_cell_measurement_reflns_used    49280
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.7710
_cell_measurement_theta_min      1.9560
_cell_volume                     7081.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material  'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Incoatec ImS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61376
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.702
_diffrn_reflns_theta_min         1.602
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       prism
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 6413 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         17050
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0356P)^2^+5.6977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                15314
_reflns_number_total             17050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03233k3.cif
_cod_data_source_block           4b
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7718228
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              4366