Synthesis of a η2-2,3-diphosphabutadiene complex of zerovalent platinum from the corresponding η2-phosphaalkyne complex
Araujo, Maria Helena; Hitchcock, Peter B.; Nixon, John F.; Kuehner, Uwe; Stelzer, Othmar; Chemical Communications (Cambridge, United Kingdom)  (2003) 1092–1093; doi:10.1039/b301335a

data_7104099
_publ_section_title
;
 Synthesis of a \h2-2,3-diphosphabutadiene complex of zerovalent platinum
 from the corresponding \h2-phosphaalkyne complex
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   9
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1092
_journal_page_last               1093
_journal_paper_doi               10.1039/b301335a
_journal_year                    2003
_chemical_formula_moiety         '(C38 H54 O1 P4 Pt1 Si2).3.5(C4 H8 O1)'
_chemical_formula_sum            'C52 H82 O4.5 P4 Pt Si2'
_chemical_formula_weight         1154.33
_chemical_name_common            '[(Ph2PCH2CH2PPH2)Pt{tBuCH2PH(O)C(SiMe3)2}]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.94(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.187(5)
_cell_length_b                   19.897(8)
_cell_length_c                   20.892(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     11286.4(60)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7980
_diffrn_reflns_theta_max         22.95
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.078
_refine_diff_density_min         -2.400
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       0.00001(2)
_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_all   1.059
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_obs          0.0609
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+57.4535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1681
_refine_ls_wR_factor_obs         0.1468
_reflns_number_observed          5652
_reflns_number_total             7801
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b301335a.txt
_cod_data_source_block           feb798
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+57.4535P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+57.4535P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C52 H82 O4.50 P4 Pt Si2'
_cod_database_code               7104099