Synthesis and Reactivity of Nickel and Palladium Fluoride Complexes with PCP Pincer Ligands. NMR-Based Assessment of Electron-Donating Properties of Fluoride and Other Monoanionic Ligands
Mart\?ínez-Prieto, Luis Miguel; Melero, Cristóbal; del R\?ío, Diego; Palma, Pilar; Cámpora, Juan; Álvarez, Eleuterio; Organometallics 31 (2012) 1425–; doi:10.1021/om2009793

data_4067982
_publ_section_title
;
 Synthesis and Reactivity of Nickel and Palladium Fluoride Complexes with
 PCP Pincer Ligands. NMR-Based Assessment of Electron-Donating Properties
 of Fluoride and Other Monoanionic Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1425
_journal_paper_doi               10.1021/om2009793
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C21 H38 Ni P2'
_chemical_formula_sum            'C21 H38 Ni P2'
_chemical_formula_weight         411.16
_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                 96.038(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.998(9)
_cell_length_b                   13.794(9)
_cell_length_c                   28.90(3)
_cell_measurement_reflns_used    3776
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      49.7
_cell_measurement_theta_min      5.9
_cell_volume                     4360(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '135mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD2000
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_radiation_monochromator  'graded mirror'
_diffrn_radiation_source         'Enraf Nonius FR590'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36997
_diffrn_reflns_theta_full        63.34
_diffrn_reflns_theta_max         63.34
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.648
_exptl_absorpt_correction_T_max  0.7865
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Bruker (2001). APEX2, Bruker (2007)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                5401
_reflns_number_total             6775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2009793_si_001.cif
_cod_data_source_block           '[(iPrPCP)Ni-Me]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4067982