Multinuclear and Dynamic NMR Study of trans-[Pt(Cl)(PHCy2)2(PCy2)], [Pt(Cl)(PHCy2)3][BF4], [Pt(Cl)(PHCy2)3][Cl], trans-[Pt(Cl)(PHCy2)2{P(S)Cy2}], and trans-[Pt(Cl)(PHCy2)2{P(O)Cy2}]. Influence of Intramolecular PO...H-P and Cl...H-P Interactions on Restricted Rotation about Pt-P Bond. X-ray Structure of trans-[Pt(Cl)(PHCy2)2{P(O)Cy2}]
Piero Mastrorilli; Cosimo F. Nobile; Mario Latronico; Vito Gallo; Ulli Englert; Francesco P. Fanizzi; Oronzo Sciacovelli; Inorganic Chemistry 44 (2005) 9097–9104; doi:10.1021/ic051198x

data_4310109
_publ_contact_author_address
;
       Institut fuer Anorganische Chemie
       RWTH Aachen
       Prof.-Pirlet-Str.1
       52074 Aachen
       Germany
;
_publ_contact_author_email       ullrich.englert@ac.rwth-aachen.de
_publ_contact_author_fax         0049-241-8092288
_publ_contact_author_name        'Ulli Englert'
_publ_contact_author_phone       0049-241-8094666
_publ_section_title
;
Multinuclear and Dynamic NMR Study of trans-[Pt(Cl)(PHCy2)2(PCy2)],
[Pt(Cl)(PHCy2)3][BF4],
[Pt(Cl)(PHCy2)3][Cl], trans-[Pt(Cl)(PHCy2)2{P(S)Cy2}],
and trans-[Pt(Cl)(PHCy2)2{P(O)Cy2}]. Influence of Intramolecular
PO...H-P and Cl...H-P Interactions on Restricted Rotation about
Pt-P Bond. X-ray Structure of trans-[Pt(Cl)(PHCy2)2{P(O)Cy2}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9097
_journal_page_last               9104
_journal_paper_doi               10.1021/ic051198x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H68 Cl O P3 Pt, H2 O'
_chemical_formula_sum            'C36 H70 Cl O2 P3 Pt'
_chemical_formula_weight         858.37
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.035(2)
_cell_angle_beta                 111.432(2)
_cell_angle_gamma                94.637(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9262(8)
_cell_length_b                   13.3376(10)
_cell_length_c                   13.4580(9)
_cell_measurement_reflns_used    5535
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.46
_cell_volume                     1929.0(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full .984
_diffrn_measured_fraction_theta_max .984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38861
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    3.860
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_correction_T_min  0.5599
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.753
_refine_diff_density_min         -2.692
_refine_diff_density_rms         .152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         10259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                8980
_reflns_number_total             10259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051198xsi20050718_102012.cif
_cod_data_source_block           pm13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.2000P] 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^)+(0.0400P)^2^+1.2000P] 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      'P -1 '
_cod_database_code               4310109