Autoionization of Homogeneous Nickel(II) Diphosphane Hydrogenation Catalysts. An NMR Study and Crystal Structures of [Ni(o-MeO-dppe)I2] and [Ni(o-MeO-dppe)2](PF6)2
Ingrid M. Angulo; Elisabeth Bouwman; Martin Lutz; Wilhelmus P. Mul; Anthony L. Spek; Inorganic Chemistry 40 (2001) 2073–2082; doi:10.1021/ic0006955

data_4319528
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Dep. Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@chem.uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Autoionization of Homogeneous Nickel(II) Diphosphane Hydrogenation
 Catalysts. An NMR Study and Crystal Structures of [Ni(o-MeO-dppe)I2] and
 [Ni(o-MeO-dppe)2](PF6)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2073
_journal_page_last               2082
_journal_paper_doi               10.1021/ic0006955
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C60 H64 Ni O8 P4, 2(P F6)'
_chemical_formula_sum            'C60 H64 F12 Ni O8 P6'
_chemical_formula_weight         1385.64
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1745(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5326(3)
_cell_length_b                   13.6794(2)
_cell_length_c                   21.7134(3)
_cell_measurement_temperature    150(2)
_cell_volume                     6394.34(16)
_computing_cell_refinement       'DENZO 1.11.0'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'DENZO 1.11.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50044
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7304
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0530P)^2^+4.8452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                6275
_reflns_number_total             7304
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0006955_1.cif
_cod_data_source_block           s2135a
_cod_original_cell_volume        6394.34(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4319528