Lewis Acid Platinum Complexes of Conformationally Flexible NUPHOS Diphosphines: Highly Efficient Catalysts for the Carbonyl−Ene Reaction
Doherty, Simon; Goodrich, Peter; Hardacre, Christopher; Luo, He−Kuan; Nieuwenhuyzen, Mark; Rath, Rakesh K.; Organometallics 24 (2005) 5945–; doi:10.1021/om0505716

data_4076081
_publ_section_title
;
 Lewis Acid Platinum Complexes of Conformationally Flexible NUPHOS
 Diphosphines:&#x00A0; Highly Efficient Catalysts for the
 Carbonyl&#x2212;Ene Reaction
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5945
_journal_paper_doi               10.1021/om0505716
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C48 H52 Cl6 N2 O8 P2 Pt'
_chemical_formula_weight         1254.65
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 102.196(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.647(3)
_cell_length_b                   23.066(5)
_cell_length_c                   19.835(4)
_cell_measurement_reflns_used    981
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.85
_cell_measurement_theta_min      2.26
_cell_volume                     5208(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43828
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    3.116
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1215
_refine_ls_number_reflns         14838
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                12403
_reflns_number_total             14838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0505716si20050708_093506.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

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        5208.3(19)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4076081