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_4312165
_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            'C91 H69 F18 O7 P3 Pt2 S'
_chemical_formula_weight         2131.61
_chemical_name_common            ana235
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 94.44
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.66040(10)
_cell_length_b                   23.0236(2)
_cell_length_c                   23.3432(2)
_cell_measurement_reflns_used    207698
_cell_measurement_temperature    173.0(10)
_cell_volume                     8391.34(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      -0.0314177
_diffrn_orient_matrix_UB_12      0.0376609
_diffrn_orient_matrix_UB_13      0.0020861
_diffrn_orient_matrix_UB_21      -0.0357932
_diffrn_orient_matrix_UB_22      -0.0169137
_diffrn_orient_matrix_UB_23      0.029507
_diffrn_orient_matrix_UB_31      0.0428231
_diffrn_orient_matrix_UB_32      0.0134933
_diffrn_orient_matrix_UB_33      0.0311642
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103763
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    3.509
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.596
_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    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slide
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.075
_refine_diff_density_max         4.79
_refine_diff_density_min         -2.304
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         17095
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0512P)^2^+43.0491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                13984
_reflns_number_total             17095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048987jsi20040727_111735_4.cif
_cod_data_source_block           for_complex_8.3THF
_cod_original_cell_volume        8391.38(12)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4312165