Structural, Spectroscopic, and Theoretical Elucidation of a Redox-Active Pincer-Type Ancillary Applied in Catalysis
Debashis Adhikari; Susanne Mossin; Falguni Basuli; John C. Huffman; Robert K. Szilagyi; Karsten Meyer; Daniel J. Mindiola; Journal of the American Chemical Society 130 (2008) 3676–3682; doi:10.1021/ja7108486

data_4107568
_publ_section_title
;
 Structural, Spectroscopic, and Theoretical Elucidation of a Redox-Active
 Pincer-Type Ancillary Applied in Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3676
_journal_page_last               3682
_journal_paper_doi               10.1021/ja7108486
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C26 H40 Cl N Ni P2, C F3 O3 S'
_chemical_formula_sum            'C27 H40 Cl F3 N Ni O3 P2 S'
_chemical_formula_weight         671.76
_chemical_name_systematic
; 
 ? 
;
_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                 92.510(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9057(9)
_cell_length_b                   18.8042(15)
_cell_length_c                   14.7900(11)
_cell_measurement_reflns_used    1001
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      3.14
_cell_volume                     3030.1(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      132(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'   0.30 degree frames measured for 20.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27480
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic green'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       'elongated prism'
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         8843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0180P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                5686
_reflns_number_total             8843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7108486-file004.cif
_cod_data_source_block           05276
_cod_original_sg_symbol_Hall     '-P 2yn  '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4107568