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_4326335
_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         'C21 H39 Cl N O2 P2 Pt, C24 H20 B, C6 H6'
_chemical_formula_sum            'C51 H65 B Cl N O2 P2 Pt'
_chemical_formula_weight         1027.33
_chemical_name_common            jonsk45
_chemical_name_systematic
; 
 [(PONOP)PtCl] BPh4.C6H6
;
_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                 95.038(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.635(3)
_cell_length_b                   23.104(6)
_cell_length_c                   17.868(4)
_cell_measurement_reflns_used    3934
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.35
_cell_volume                     4785(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1103
_diffrn_reflns_av_sigmaI/netI    0.1275
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            119232
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.8361
_exptl_absorpt_correction_T_min  0.4021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       needle
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
'Flack H D (1983), 18698 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         38201
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                27213
_reflns_number_total             38201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201102v_si_002_04.cif
_cod_data_source_block           jonsk45_3c
_cod_database_code               4326335