Chiral heterobimetallic complexes of carbodiphosphoranes and phosphinidene_carbene adducts
Manuel Alcarazo; Karin Radkowski; Gerlinde Mehler; Richard Goddard; Alois Furstner; Chem.Commun. 49 (2013) 3140–; doi:10.1039/c3cc40382c

data_7109052
_publ_section_title
;
 Chiral heterobimetallic complexes of carbodiphosphoranes and
 phosphinidene_carbene adducts
;
_journal_name_full               Chem.Commun.
_journal_page_first              3140
_journal_paper_doi               10.1039/c3cc40382c
_journal_volume                  49
_journal_year                    2013
_chemical_compound_source        toluene
_chemical_formula_moiety         '2(C36 H29 N P2), C7 H8'
_chemical_formula_sum            'C79 H66 N2 P4'
_chemical_formula_weight         1167.22
_chemical_name_systematic
;
P-triphenyl-P'-2-pyridyl-diphenyl-carbodiphorphorane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                RKI-RF-151-01_6912
_audit_creation_date             2012-12-06
_cell_angle_alpha                73.849(2)
_cell_angle_beta                 73.626(2)
_cell_angle_gamma                78.953(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5881(12)
_cell_length_b                   11.7546(14)
_cell_length_c                   13.4581(16)
_cell_measurement_reflns_used    9641
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.7733
_cell_measurement_theta_min      2.8830
_cell_volume                     1531.9(3)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47413
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.04
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.99724
_exptl_absorpt_correction_T_min  0.99209
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       needle
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         10542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0746P)^2^+0.7848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                7527
_reflns_number_total             10542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40382c.txt
_cod_data_source_block           3
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7109052