Synthesis, mechanism of formation, and catalytic activity of Xantphos nickel pi-complexes
Nicholas D. Staudaher; Ryan M. Stolley; Janis Louie; Chem.Commun. 50 (2014) 15577–; doi:10.1039/C4cc07590K

data_7116076
_publ_section_title
;
 Synthesis, mechanism of formation, and catalytic activity of Xantphos
 nickel pi-complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              15577
_journal_paper_doi               10.1039/C4cc07590K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C45 H42 Ni O P2'
_chemical_formula_sum            'C45 H42 Ni O P2'
_chemical_formula_weight         719.44
_chemical_name_systematic        'Xantphos Ni 3-Hexyne'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.2001(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6794(3)
_cell_length_b                   15.0260(3)
_cell_length_c                   17.7954(4)
_cell_measurement_reflns_used    6971
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      1.018
_cell_volume                     3652.08(14)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scan'
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29344
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.9083
_exptl_absorpt_correction_T_min  0.8642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0131P)^2^+4.9015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                5629
_reflns_number_total             7946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07590k3.cif
_cod_data_source_block           jl054
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7116076