Transition-metal complexes of group 12 with 1,1'-bis(phosphanyl)ferrocene ligands
Chaudhary, Karan; Trivedi, Manoj; Masram, Dhanraj T.; Rath, Nigam P.; Acta Crystallographica Section C 77 (2021) 240–248; doi:10.1107/S2053229621004162

data_2022365
_publ_section_title
;
 Transition-metal complexes of group 12 with 1,1'-bis(phosphanyl)ferrocene
 ligands
;
_journal_coeditor_code           YD3016
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              240
_journal_page_last               248
_journal_paper_doi               10.1107/S2053229621004162
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Fe (C13 H22 P S)2]'
_chemical_formula_moiety         'C26 H44 Fe P2 S2'
_chemical_formula_sum            'C26 H44 Fe P2 S2'
_chemical_formula_weight         538.52
_chemical_name_systematic
;
1,1'-Bis(di-<i>tert</i>-butylthiophosphinoyl)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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 116.9816(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7589(7)
_cell_length_b                   14.0445(5)
_cell_length_c                   14.7141(6)
_cell_measurement_reflns_used    5962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.77
_cell_volume                     2718.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2013)
;
_computing_publication_material
;
SHELXTL (Bruker, 2013)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26174
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         2.175
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.8878
_exptl_absorpt_correction_T_min  0.7680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.447
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0171P)^2^+1.5394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                4652
_reflns_number_total             6228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yd3016sup1.cif
_cod_data_source_block           Complex-3
_cod_depositor_comments
'Adding full bibliography for 2022363--2022366.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022365
_cod_database_fobs_code          2022365
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.958
_shelx_hkl_checksum              78844
_shelx_res_checksum              51268