Novel route to carbodiphosphoranes producing a new P,C,P pincer carbene ligand.
Stallinger, Silvia; Reitsamer, Christian; Schuh, Walter; Kopacka, Holger; Wurst, Klaus; Peringer, Paul; Chemical communications (Cambridge, England)  (2007) 510–512; doi:10.1039/b609723e

data_7101667
_publ_section_title
;
 Novel route to carbodiphosphoranes producing a new P,C,P pincer
 carbene ligand.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              510
_journal_page_last               512
_journal_paper_doi               10.1039/b609723e
_journal_year                    2007
_chemical_formula_sum            'C69.5 H68 Cl2 O P4 Pd'
_chemical_formula_weight         1220.42
_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                84.068(1)
_cell_angle_beta                 82.649(1)
_cell_angle_gamma                89.914(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2001(2)
_cell_length_b                   12.4004(2)
_cell_length_c                   24.4161(4)
_cell_measurement_reflns_used    31104
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      1.0
_cell_volume                     3046.28(9)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17938
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    'mixed; refined with bond reastraint at O1'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         12411
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+2.6218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                10607
_reflns_number_total             12411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609723e.txt
_cod_data_source_block           p143
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C69.50 H68 Cl2 O P4 Pd'
_cod_database_code               7101667