Synthesis, reactivity and coordination behaviour of a ferrocene phosphinostibine and intramolecular interactions in its P(v) and Sb(v) derivatives
Antala, Jakub; Schulz, Jiří; Císařová, Ivana; Štěpnička, Petr; New Journal of Chemistry 48 (2024) 5107–5119; doi:10.1039/D4NJ00349G

data_7063020
_publ_section_title
;
 Synthesis, reactivity and coordination behaviour of a ferrocene
 phosphinostibine and intramolecular interactions in its P(v) and Sb(v)
 derivatives
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5107
_journal_page_last               5119
_journal_paper_doi               10.1039/D4NJ00349G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C34 H40 Cl2 Fe P S Sb'
_chemical_formula_sum            'C34 H40 Cl2 Fe P S Sb'
_chemical_formula_weight         760.19
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                85.141(2)
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_cell_angle_gamma                77.2340(10)
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_cell_length_b                   12.1508(5)
_cell_length_c                   12.4622(5)
_cell_measurement_reflns_used    9268
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.46
_cell_volume                     1616.28(12)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
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_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
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_computing_publication_material  'PLATON (Spek, 2017)'
_computing_structure_refinement  'SHELXL-2017 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_max       15
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42500
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.460
_exptl_absorpt_coefficient_mu    1.587
_exptl_absorpt_correction_T_max  0.79
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0208P)^2^+1.5141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7210
_reflns_number_total             7415
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7063018--7063034.cif.'
_cod_database_code               7063020
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.785
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