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_7135207
_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         'C36 H28 Bi Fe O2 P W0.50'
_chemical_formula_sum            'C36 H28 Bi Fe O2 P W0.5'
_chemical_formula_weight         880.31
_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   geom
_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                98.928(2)
_cell_angle_beta                 97.552(2)
_cell_angle_gamma                92.666(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1002(4)
_cell_length_b                   10.1731(5)
_cell_length_c                   16.7783(8)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.9269
_cell_measurement_theta_min      2.4806
_cell_measurement_wavelength     0.71073
_cell_volume                     1517.60(12)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'BIS 8.5.5.6/2024-10-24'
_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      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            PhotonIII_C14
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'flat graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0075
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            90325
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_min         2.031
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.6
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.236
_exptl_absorpt_correction_T_max  0.528
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_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    1.926
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.529
_refine_diff_density_min         -3.336
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0358
_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^)+17.6518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5339
_reflns_number_total             5354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05762k3.cif
_cod_data_source_block           17
_cod_original_formula_sum        'C36 H28 Bi Fe O2 P W0.50'
_cod_database_code               7135207
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.414
_shelx_estimated_absorpt_t_max   0.528
_bruker_diffrn_measurement_temperature_device Cryostream
_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              38058
_shelx_hkl_checksum              82530