Synthesis and Reactivity of New Ni, Pd, and Pt 2,6-Bis(di-tert-butylphosphinito)pyridine Pincer Complexes
Sabuj Kundu; William W. Brennessel; William D. Jones; Inorganic Chemistry 50 (2011) 9443–9453; doi:10.1021/ic201102v

data_4326332
_publ_contact_author_address
'Department of Chemistry, University of Rochester, Rochester, New York 14627'
_publ_contact_author_email       jones@chem.rochester.edu
_publ_contact_author_name        'William D. Jones'
_publ_section_title
;
 Synthesis and Reactivity of New Ni, Pd, and Pt
 2,6-Bis(di-tert-butylphosphinito)pyridine Pincer Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9443
_journal_page_last               9453
_journal_paper_doi               10.1021/ic201102v
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C21 H39 Cl N Ni O2 P2), Cl4 Ni, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H82 Cl10 N2 Ni3 O4 P4'
_chemical_formula_weight         1357.63
_chemical_name_common            jonsk05
_chemical_name_systematic
; 
 [(PONOP)NiCl]2 NiCl4 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.802(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0398(13)
_cell_length_b                   22.128(2)
_cell_length_c                   12.1003(13)
_cell_measurement_reflns_used    3874
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.53
_cell_volume                     3116.7(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            74719
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_correction_T_min  0.6203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dichroic yellow-green / orange'
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
'Flack H D (1983), 12032 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         24702
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                16353
_reflns_number_total             24702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201102v_si_002_01.cif
_cod_data_source_block           jonsk05_3aNiCl4
_cod_database_code               4326332