New Superhindered Polydentate Polyphosphine Ligands P(CH2CH2PtBu2)3, PhP(CH2CH2PtBu2)2, P(CH2CH2CH2PtBu2)3, and their Ruthenium(II) Chloride Complexes
Ryan Gilbert-Wilson; Leslie D. Field; Mohan M. Bhadbhade; Inorganic Chemistry 51 (2012) 3239–3246; doi:10.1021/ic2027169

data_4328580
_publ_section_title
;
 New Superhindered Polydentate Polyphosphine Ligands P(CH2CH2PtBu2)3,
 PhP(CH2CH2PtBu2)2, P(CH2CH2CH2PtBu2)3, and their Ruthenium(II) Chloride
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3239
_journal_page_last               3246
_journal_paper_doi               10.1021/ic2027169
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C33 H72 Cl2 P4 Ru'
_chemical_formula_weight         764.76
_chemical_name_systematic
; 
 ? 
;
_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                   12.462(2)
_cell_length_b                   14.307(3)
_cell_length_c                   21.914(4)
_cell_measurement_reflns_used    490
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      14.260
_cell_measurement_theta_min      2.475
_cell_volume                     3907.1(13)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2007)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2007)'
_computing_data_reduction        '<i>SAINT</i>  '
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.1778
_diffrn_reflns_av_sigmaI/netI    0.2943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15684
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.9221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2001)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       'Square plates'
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.15(11)
_refine_ls_extinction_coef       0.0040(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.1939
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.2326
_reflns_number_gt                3325
_reflns_number_total             6760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027169_si_001_2.cif
_cod_data_source_block           ryan6_reporcess
_cod_original_cell_volume        3907.1(12)
_cod_database_code               4328580