Synthesis and structural characterization of the racemic and meso forms of 2,2′′-dibromo-1,1′′-biferrocenes and their mixed-valence salts
Horikoshi, Ryo; Inoue, Ryota; Sumitani, Ryo; Takahashi, Kazuyuki; Mochida, Tomoyuki; CrystEngComm 27 (2025) 2371–2381; doi:10.1039/D5CE00076A

data_7250090
_publ_section_title
;
 Synthesis and structural characterization of the racemic and meso forms
 of 2,2&#x2032;&#x2032;-dibromo-1,1&#x2032;&#x2032;-biferrocenes and their
 mixed-valence salts
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2371
_journal_page_last               2381
_journal_paper_doi               10.1039/D5CE00076A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C11 H8 Br Fe N'
_chemical_formula_sum            'C11 H8 Br Fe N'
_chemical_formula_weight         289.94
_chemical_name_common            FcBrCN
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-03-21 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.018(8)
_cell_length_b                   10.319(9)
_cell_length_c                   10.748(10)
_cell_measurement_reflns_used    4565
_cell_measurement_temperature    90.(2)
_cell_measurement_theta_max      27.4979
_cell_measurement_theta_min      2.7500
_cell_volume                     1000.2(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  'Generate Report (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5561
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         2.74
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    5.455
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.532
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.445
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.024(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2209
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0090P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                2102
_reflns_number_total             2209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00076a2.cif
_cod_data_source_block           TDBBF
_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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7250089--7250092.cif.
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_cod_database_code               7250090
_shelx_res_checksum              6755