2-Pyridylmetallocenes, part IV. Cycloplatination of 2-pyridyl-ferrocene, -ruthenocene and -cymantrene. Molecular structures of sigma-Pt{CpM[C5H3(2-C5H4N)]}Cl (DMSO) (M = Fe, Ru) and sigma-Pt{CpFe[C5H3(2-C5H4N)]}(acac)
Karlheinz Sunkel; Ramona Branzan; Stefan Weigand; Inorganica Chimica Acta 399 (2013) 193–199; doi:

data_1516898
_publ_section_title
;
 2-Pyridylmetallocenes, part IV. Cycloplatination of 2-pyridyl-ferrocene,
 -ruthenocene and -cymantrene. Molecular structures of
 sigma-Pt{CpM[C5H3(2-C5H4N)]}Cl (DMSO) (M = Fe, Ru) and
 sigma-Pt{CpFe[C5H3(2-C5H4N)]}(acac)
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              193
_journal_page_last               199
_journal_volume                  399
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C19 H22 Cl3 Fe1 N1 O1 Pt1 S1'
_chemical_formula_sum            'C19 H22 Cl3 Fe N O Pt S'
_chemical_formula_weight         669.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 116.795(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3079(5)
_cell_length_b                   26.2435(11)
_cell_length_c                   9.7687(5)
_cell_measurement_reflns_used    4394
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2499
_cell_measurement_theta_min      4.1369
_cell_measurement_wavelength     0.71073
_cell_volume                     2130.0(2)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0040998095
_diffrn_orient_matrix_UB_12      0.0228955615
_diffrn_orient_matrix_UB_13      0.0366576373
_diffrn_orient_matrix_UB_21      0.0326467622
_diffrn_orient_matrix_UB_22      -0.0128069815
_diffrn_orient_matrix_UB_23      0.0717153238
_diffrn_orient_matrix_UB_31      0.078888455
_diffrn_orient_matrix_UB_32      0.0064875806
_diffrn_orient_matrix_UB_33      0.0119842556
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8652
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    7.726
_exptl_absorpt_correction_T_max  0.3390
_exptl_absorpt_correction_T_min  0.2462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.065
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3289
_reflns_number_total             4322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-399-193-199-1.cif
_cod_data_source_block           publication_text-1
_cod_original_cell_volume        2130.00(18)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               1516898