The crystal structure of a new ferrocenyl P,N ligand: 1-[(2,2-dimethylhydrazin-1-ylidene)methyl]-1'-(diphenylphosphorothioyl)ferrocene
Mouas, Toma Nardjes; Daran, Jean-Claude; Merazig, Hocine; Manoury, Eric; Acta Crystallographica Section E 74 (2018) 133–136; doi:10.1107/S2056989018000440

data_2242321
_publ_section_title
;
 The crystal structure of a new ferrocenyl P,N ligand:
 1-[(2,2-dimethylhydrazin-1-ylidene)methyl]-1'-(diphenylphosphorothioyl)ferrocene
;
_journal_coeditor_code           SU5416
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              133
_journal_page_last               136
_journal_paper_doi               10.1107/S2056989018000440
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Fe (C8 H11 N2) (C17 H14 P S)]'
_chemical_formula_moiety         'C25 H25 Fe N2 P S'
_chemical_formula_sum            'C25 H25 Fe N2 P S'
_chemical_formula_weight         472.35
_chemical_name_systematic
;
1-[(2,2-Dimethylhydrazin-1-ylidene)methyl]-1'-(diphenylphosphorothioyl)ferrocene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.682(3)
_cell_angle_beta                 86.600(3)
_cell_angle_gamma                88.884(3)
_cell_formula_units_Z            4
_cell_length_a                   12.0684(5)
_cell_length_b                   13.9953(4)
_cell_length_c                   14.0634(5)
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.90
_cell_volume                     2275.61(14)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), PLATON (Spek, 2009) and
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49518
_diffrn_reflns_theta_full        27.482
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         10325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.9815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                8270
_reflns_number_total             10325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5416sup1.cif
_cod_data_source_block           I
_cod_database_code               2242321
_cod_database_fobs_code 2242321