Successive Formation of Hydrido(germyl)platinum, Germaplatinacycle, and Germylene-Bridged Dinuclear Platinum Complexes from the Reaction of a Zerovalent Platinum Complex with α,ω-Dihydrodigermanes
Usui, Yoko; Hosotani, Sayaka; Ogawa, Aki; Nanjo, Masato; Mochida, Kunio; Organometallics 24 (2005) 4337–; doi:10.1021/om0503287

data_4075947
_publ_section_title
;
 Successive Formation of Hydrido(germyl)platinum, Germaplatinacycle, and
 Germylene-Bridged Dinuclear Platinum Complexes from the Reaction of a
 Zerovalent Platinum Complex with \a,\w-Dihydrodigermanes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4337
_journal_paper_doi               10.1021/om0503287
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         Pt(GePh2SiMe2SiMe2GePh2)(PPh3)2
_chemical_formula_sum            'C70 H67 Ge2 P2 Pt Si2'
_chemical_formula_weight         1366.63
_chemical_name_common
;
(2,2,3,3-tetramethyl-1,1,4,4-tetraphenyl-
2,3-disilatetragerman-1,4-diyl)bis
(triphenylphosphine)platinum 
;
_chemical_name_systematic
; 
(2,2,3,3-tetramethyl-1,1,4,4-tetraphenyl-
2,3-disilatetragerman-1,4-diyl)bis
(triphenylphosphine)platinum 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 111.360(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.344(2)
_cell_length_b                   12.8430(14)
_cell_length_c                   22.869(2)
_cell_measurement_reflns_used    4370
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.91
_cell_volume                     6111.8(10)
_computing_cell_refinement       SCALEPACK
_computing_data_collection       XPRESS
_computing_data_reduction        DENZO
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'MacScience DIP2030 imaging plate'
_diffrn_measurement_method       /w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4370
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2748
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.097(9)
_refine_ls_extinction_coef       0.00041(13)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         4370
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.251
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                4199
_reflns_number_total             4370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0503287si20050713_102814.cif
_cod_data_source_block           publication
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6111.8(11)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4075947