Synthesis, Structures, and Properties of the Phosphonium-1-indenylide (PHIN) Ligands 1-C9H6PPh3, 1-C9H6PMePh2, and 1-C9H6PMe2Ph and of the Corresponding Ruthenium(II) Complexes [Ru(η5-C5H5)(η5-PHIN)]PF6
Fowler, Kevin G.; Littlefield, Shalyn L.; Baird, Michael C.; Budzelaar, Peter H. M.; Organometallics 30 (2011) 6098–; doi:10.1021/om200545j

data_4065053
_publ_section_title
;
 Synthesis, Structures, and Properties of the Phosphonium-1-indenylide
 (PHIN) Ligands 1-C9H6PPh3, 1-C9H6PMePh2, and 1-C9H6PMe2Ph and of the
 Corresponding Ruthenium(II) Complexes [Ru(\h5-C5H5)(\h5-PHIN)]PF6
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6098
_journal_paper_doi               10.1021/om200545j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C27 H21 P'
_chemical_formula_weight         376.41
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7916(14)
_cell_length_b                   12.3946(16)
_cell_length_c                   14.957(2)
_cell_measurement_reflns_used    5676
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      2.50
_cell_volume                     2000.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19833
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9573
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.194
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.5316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                3515
_reflns_number_total             3933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200545j_si_008.cif
_cod_data_source_block           mb27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4065053
_refine_di                       '(b) CIF file of III'