Alkynyldiphenylphosphine d8 (Pt, Rh, Ir) Complexes: Contrasting Behavior toward cis-[Pt(C6F5)2(THF)2]
Jesús R. Berenguer; María Bernechea; Juan Forniés; Ana García; Elena Lalinde; M. Teresa Moreno; Inorganic Chemistry 43 (2004) 8185–8198; doi:10.1021/ic048987j

data_4312168
_publ_section_title
;
 Alkynyldiphenylphosphine d8 (Pt, Rh, Ir) Complexes: Contrasting Behavior
 toward cis-[Pt(C6F5)2(THF)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8185
_journal_page_last               8198
_journal_paper_doi               10.1021/ic048987j
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C70 H34 F20 P2 Pt3 S2'
_chemical_formula_weight         1966.3
_chemical_name_common            ana279
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                107.1250(10)
_cell_angle_beta                 93.3460(10)
_cell_angle_gamma                109.9680(10)
_cell_formula_units_Z            2
_cell_length_a                   15.3996(3)
_cell_length_b                   15.7509(2)
_cell_length_c                   18.5369(4)
_cell_measurement_reflns_used    120532
_cell_measurement_temperature    223.0(10)
_cell_volume                     3974.89(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223.0(10)
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0676147
_diffrn_orient_matrix_UB_12      0.0225952
_diffrn_orient_matrix_UB_13      -0.0053078
_diffrn_orient_matrix_UB_21      -0.0056834
_diffrn_orient_matrix_UB_22      -0.0680287
_diffrn_orient_matrix_UB_23      -0.0229663
_diffrn_orient_matrix_UB_31      -0.0179912
_diffrn_orient_matrix_UB_32      0.0012372
_diffrn_orient_matrix_UB_33      -0.0522861
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42871
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    5.441
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.719
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00054(15)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         14635
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+7.1711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                11803
_reflns_number_total             14635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048987jsi20040727_111735_7.cif
_cod_data_source_block           for_complex_14
_cod_database_code               4312168