A Mixed Phosphine−Iminophosphorane Tetradentate Ligand: Synthesis, Coordination to Group 10 Metal Centers, and Use as Catalyst in Suzuki−Miyaura Coupling
Buchard, Antoine; Komly, Bruno; Auffrant, Audrey; Le Goff, Xavier F.; Floch, Pascal Le; Organometallics 27 (2008) 4380–; doi:10.1021/om8002637

data_4071599
_publ_section_title
;
 A Mixed Phosphine&#x2212;Iminophosphorane Tetradentate Ligand: Synthesis,
 Coordination to Group 10 Metal Centers, and Use as Catalyst in
 Suzuki&#x2212;Miyaura Coupling
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4380
_journal_paper_doi               10.1021/om8002637
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C54 H52 Br2 Cl4 N2 Ni P4'
_chemical_formula_sum            'C54 H52 Br2 Cl4 N2 Ni P4'
_chemical_formula_weight         1213.19
_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                86.688(1)
_cell_angle_beta                 86.511(1)
_cell_angle_gamma                78.482(1)
_cell_formula_units_Z            2
_cell_length_a                   12.498(1)
_cell_length_b                   13.157(1)
_cell_length_c                   16.541(1)
_cell_measurement_reflns_used    28365
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2657.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  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     0.71069
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24716
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    2.229
_exptl_absorpt_correction_T_max  0.8779
_exptl_absorpt_correction_T_min  0.5009
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.737
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         11661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0835P)^2^+2.4835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                8576
_reflns_number_total             11661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8002637-file001.cif
_cod_data_source_block           ab416
_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_sg_symbol_H-M      'P-1     '
_cod_database_code               4071599