Practical synthesis of ferrocenyldiarylstibines and bismuthines.
Rezazgui, David; Schulz, Jiří; Štěpnička, Petr; Chemical communications (Cambridge, England) 61 (2025) 18705–18708; doi:10.1039/d5cc05762k

data_7135206
_publ_section_title
;
 Practical synthesis of ferrocenyldiarylstibines and bismuthines.
;
_journal_issue                   94
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              18705
_journal_page_last               18708
_journal_paper_doi               10.1039/d5cc05762k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C34 H31 B Fe P Sb'
_chemical_formula_sum            'C34 H31 B Fe P Sb'
_chemical_formula_weight         658.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'Intrinsic Phasing'
_audit_creation_method
;FinalCif 2024.9-1 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-09-25 deposited with the CCDC.	2025-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                82.755(2)
_cell_angle_beta                 82.306(2)
_cell_angle_gamma                86.952(2)
_cell_formula_units_Z            4
_cell_length_a                   8.9845(6)
_cell_length_b                   16.3617(8)
_cell_length_c                   20.0366(12)
_cell_measurement_reflns_used    1347
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      19.1623
_cell_measurement_theta_min      1.887
_cell_measurement_wavelength     0.71073
_cell_volume                     2893.6(3)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.1.2.Release'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66658
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.512
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'translucent pale yellow'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.063
_refine_diff_density_max         2.135
_refine_diff_density_min         -2.293
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         13118
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0309P)^2^+18.2443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11032
_reflns_number_total             13118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05762k3.cif
_cod_data_source_block           13BH3
_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/current/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 
;
_cod_database_code               7135206
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.911
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              95806
_shelx_hkl_checksum              11890