Asymmetric Synthesis of P-Stereogenic Homo- and Heterobimetallic Complexes via Selective Monoinsertion of Dialkynylphosphine into the Pd−C Bond of a Palladacycle
Chen, Shuli; Pullarkat, Sumod A.; Li, Yongxin; Leung, Pak-Hing; Organometallics 30 (2011) 1530–; doi:10.1021/om101078p

data_4064015
_publ_section_title
;
 Asymmetric Synthesis of P-Stereogenic Homo- and Heterobimetallic
 Complexes via Selective Monoinsertion of Dialkynylphosphine into the
 Pd&#x2212;C Bond of a Palladacycle
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1530
_journal_paper_doi               10.1021/om101078p
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C38.84 H46.34 Cl1.31 N3.34 O P Pd2'
_chemical_formula_weight         866.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                76.468(2)
_cell_angle_beta                 81.334(2)
_cell_angle_gamma                65.2880(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9213(3)
_cell_length_b                   11.8390(4)
_cell_length_c                   18.3636(6)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.99
_cell_measurement_theta_min      2.47
_cell_volume                     1901.61(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52822
_diffrn_reflns_theta_full        31.13
_diffrn_reflns_theta_max         31.13
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.8418
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         20408
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                19277
_reflns_number_total             20408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101078p_si_003.cif
_cod_data_source_block           leung508
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1901.62(11)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4064015