Synthesis and crystallographic studies of 2-(diphenylphosphinothioyl)-2-(3-oxobut-1-en-yl)ferrocene
Bandyopadhyay, Uchchhal; Sundararaju, Basker; Poli, Rinaldo; Manoury, Eric; Daran, Jean-Claude; Acta Crystallographica Section E 77 (2021) 853–856; doi:10.1107/S205698902100760X

data_2243882
_publ_section_title
;
 Synthesis and crystallographic studies of
 2-(diphenylphosphinothioyl)-2-(3-oxobut-1-en-yl)ferrocene
;
_journal_coeditor_code           ZL5019
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              853
_journal_page_last               856
_journal_paper_doi               10.1107/S205698902100760X
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Fe (C5 H5) (C21 H18 O P S)]'
_chemical_formula_moiety         'C26 H23 Fe O P S'
_chemical_formula_sum            'C26 H23 Fe O P S'
_chemical_formula_weight         470.32
_chemical_name_systematic
;
2-(Diphenylphosphinothioyl)-2-(3-oxobut-1-en-yl)ferrocene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.230(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3643(9)
_cell_length_b                   17.909(2)
_cell_length_c                   16.710(2)
_cell_measurement_reflns_used    4518
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.19
_cell_measurement_theta_min      2.70
_cell_volume                     2194.7(4)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia,
2012)
and Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43009
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.274
_diffrn_reflns_theta_min         3.712
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.7300
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       platelet
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.496
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0664P)^2^+1.8414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                3907
_reflns_number_total             5657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5019sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2194.8(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243882
_shelx_hkl_checksum              95895
_shelx_res_checksum              20836
_cod_database_fobs_code 2243882