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_7116078
_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         'C53 H42 Ni O P2, C6 H6'
_chemical_formula_sum            'C59 H48 Ni O P2'
_chemical_formula_weight         893.62
_chemical_name_systematic        'Xantphos Ni Diphenylacetylene'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 98.8516(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8793(3)
_cell_length_b                   18.2497(3)
_cell_length_c                   19.5980(5)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     4551.52(17)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60117
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.001
_diffrn_reflns_theta_min         2.096
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         9871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0039P)^2^+7.5454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6050
_reflns_number_total             9871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07590k3.cif
_cod_data_source_block           nanny
_cod_database_code               7116078
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.933
_shelxl_version_number           2014-3
_shelx_res_checksum              98767