Cleavage of Polarized P−P Bonds in N-Heterocyclic Diphosphines in Reactions with Metal Olefin Complexes
Burck, Sebastian; Gudat, Dietrich; Nieger, Martin; Organometallics 28 (2009) 1447–; doi:10.1021/om801008s

data_4068656
_publ_section_title
;
 Cleavage of Polarized P&#x2212;P Bonds in N-Heterocyclic Diphosphines in
 Reactions with Metal Olefin Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1447
_journal_paper_doi               10.1021/om801008s
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C34 H46 N2 O2 P2 W'
_chemical_formula_sum            'C34 H46 N2 O2 P2 W'
_chemical_formula_weight         760.52
_chemical_name_systematic
; 
 Dicarbonyl-2-(1,3-dimesityl-tetrahydro-1,3,2-diazaohospholyl)-(eta^5-
 2',3',4',5'-tetraethylphospholyl)-tungsten(0) 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.180(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   23.8525(5)
_cell_length_b                   18.1101(4)
_cell_length_c                   34.0334(6)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     14551.9(5)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 0.5 deg.'
_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  0.1009
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29175
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    3.292
_exptl_absorpt_correction_T_max  0.46380
_exptl_absorpt_correction_T_min  0.30445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Platon, cf. Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             6144
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.579
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         12438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+645.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2167
_reflns_number_gt                8365
_reflns_number_total             12438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801008s_si_001.cif
_cod_data_source_block           gud116_m_compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_sg_symbol_H-M      'C 2/c'
_cod_database_code               4068656