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_4312166
_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            'C75 H48 Cl4 F13 O3 P3 Pt S'
_chemical_formula_weight         1705.99
_chemical_name_common            ana269
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.3490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1780(3)
_cell_length_b                   15.3627(2)
_cell_length_c                   23.0999(3)
_cell_measurement_reflns_used    83306
_cell_measurement_temperature    173.0(10)
_cell_volume                     6937.32(17)
_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      173.0(10)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      -0.0150163
_diffrn_orient_matrix_UB_12      -0.0116986
_diffrn_orient_matrix_UB_13      -0.0438958
_diffrn_orient_matrix_UB_21      -0.0151906
_diffrn_orient_matrix_UB_22      0.0618851
_diffrn_orient_matrix_UB_23      -0.0071474
_diffrn_orient_matrix_UB_31      0.0464817
_diffrn_orient_matrix_UB_32      0.0164452
_diffrn_orient_matrix_UB_33      -0.0043298
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55199
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    2.36
_exptl_absorpt_correction_T_max  0.7554
_exptl_absorpt_correction_T_min  0.3524
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.444
_refine_diff_density_min         -3.358
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         12146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.052
_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^)+(0.1216P)^2^+6.6278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.149
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                9270
_reflns_number_total             12146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048987jsi20040727_111735_5.cif
_cod_data_source_block           for_complex_9.2CH2Cl2
_cod_original_cell_volume        6937.32(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4312166
_exptl_absorpt_factor_mur        0.59
_exptl_absorpt_correction_t_ave  0.5835